data_global

#==============================================================================
# PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic      2020-01-08
_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted     2020-07-08
_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?
_journal_coeditor_name            ?
_journal_coeditor_code      LO5070SUP1
_journal_coeditor_notes
; ?
;
_journal_paper_category      FA
_journal_techeditor_code      B200934
_iucr_compatibility_tag          ACTA95
_journal_techeditor_notes  
;
;
_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?
_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

#==============================================================================

_audit_creation_date               2019-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_requested_journal  'Acta Crystallographica Section B'
_publ_section_title  
; High-Pressure preference for the reduced water contents in porous 
zinc-aspartate hydrates
;
_publ_section_abstract
;
Zinc asparagine (ZnAsp2) complex, commonly used as dietary supplements, 
favorably crystallizes as dihydrate (ZnAsp2*2H2O) of aqueous solution. 
At normal conditions the dihydrate easily transforms into sesquihydrate 
ZnAsp2*1.5H2O. 
The dihydrate crystal is triclinic, space group P-1, and the sesquihydrate is 
monoclinic,
 space group C2/c. However, their structures are closely related and similarly 
consist 
of zinc-aspartate ribbons parallel to pores accommodating water molecules. 
These porous structures can breathe water molecules in and out depending 
on temperature and air humidity. High-pressure preference of the sesquihydrate 
has been evidenced by recrystallizations under pressure and compressibility
 measured by single-crystal X-ray diffraction up to 4 GPa. This preference
 has been expalined by reduced volume of the sesquihydrate and water compressed 
separately, compared to the dihydrate. The sesquhydrate undergoes an 
isostructural
 phase transition, when the voids collapse at 0.8 GPa, 
whereas the compression of 
dihydrate is monotonic owing to the pores being supported by the water contents.
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;

#=============================================================================

data_Zn-aspartate_sesquihydrate_0_001GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972145'

_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'  -1.5491   0.6778 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    16.2789(3) 
_cell_length_b                    10.7307(2) 
_cell_length_c                    14.5393(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.017(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2536.26(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     2468 
_cell_measurement_theta_min       5.44  
_cell_measurement_theta_max       76.24
 
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.868 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1464 
_exptl_absorpt_coefficient_mu     3.234 
_exptl_absorpt_correction_type    'integration' 
_exptl_absorpt_correction_T_min   0.712 
_exptl_absorpt_correction_T_max   0.937
_exptl_absorpt_process_details    'integration' 
_exptl_special_details 
; 
 ? 
; 
_diffrn_ambient_temperature       296(2) 
_diffrn_radiation_wavelength      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'multiwire proportional' 
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           62
_diffrn_standards_interval_count   24
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_source                     'sealed x-ray tube'
_diffrn_radiation_probe            x-ray
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             10199 
_diffrn_reflns_av_R_equivalents   0.0199 
_diffrn_reflns_av_sigmaI/netI     0.0155 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        20 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          5.44 
_diffrn_reflns_theta_max          76.24 
_reflns_number_total              2632 
_reflns_number_gt                 2468 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0487P)²+2.5290P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00025(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2632 
_refine_ls_number_parameters      196 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0315 
_refine_ls_R_factor_gt            0.0296 
_refine_ls_wR_factor_ref          0.0863 
_refine_ls_wR_factor_gt           0.0847 
_refine_ls_goodness_of_fit_ref    1.106 
_refine_ls_restrained_S_all       1.110 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
_diffrn_measured_fraction_theta_max    0.987 
_diffrn_reflns_theta_full              76.24 
_diffrn_measured_fraction_theta_full   0.987 
_refine_diff_density_max    0.600 
_refine_diff_density_min   -0.404 
_refine_diff_density_rms    0.063 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Zn1 Zn 0.730510(15) 0.50404(2) 0.449948(17) 0.02585(12) Uani 1 1 d . . . 
O4 O 0.67955(8) 0.87379(13) 0.55387(10) 0.0342(3) Uani 1 1 d . . . 
O2 O 0.54889(8) 0.76159(13) 0.39793(10) 0.0321(3) Uani 1 1 d . . . 
O1 O 0.63918(9) 0.60880(14) 0.40487(10) 0.0334(3) Uani 1 1 d . . . 
O14 O 0.76009(9) 0.04837(15) 0.41962(10) 0.0363(3) Uani 1 1 d . . . 
O11 O 0.75421(9) 0.37497(15) 0.36264(12) 0.0414(4) Uani 1 1 d . . . 
O13 O 0.87616(10) 0.14571(16) 0.45899(10) 0.0412(4) Uani 1 1 d . . . 
O12 O 0.62930(9) 0.33025(16) 0.30225(12) 0.0432(4) Uani 1 1 d D . . 
O3 O 0.57758(11) 1.00639(13) 0.58153(14) 0.0420(4) Uani 1 1 d . . . 
N13 N 0.89140(10) 0.25231(16) 0.29576(11) 0.0311(3) Uani 1 1 d . . . 
H13A H 0.9032 0.2616 0.2371 0.037 Uiso 1 1 calc R . . 
H13B H 0.9359 0.2261 0.3282 0.037 Uiso 1 1 calc R . . 
H13C H 0.8752 0.3250 0.3180 0.037 Uiso 1 1 calc R . . 
O1W O 0.60744(13) 0.98762(17) 0.33339(14) 0.0499(4) Uani 1 1 d G . . 
H1WA H 0.6562 0.9951 0.3567 0.075 Uiso 1 1 d G . . 
H1WB H 0.5871 0.9277 0.3629 0.075 Uiso 1 1 d G . . 
N3 N 0.46595(11) 0.82054(17) 0.56868(13) 0.0365(4) Uani 1 1 d . . . 
H3A H 0.4608 0.8449 0.5102 0.044 Uiso 1 1 calc R . . 
H3B H 0.4505 0.8821 0.6050 0.044 Uiso 1 1 calc R . . 
H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc R . . 
O2W O 0.5000 0.5206(3) 0.2500 0.0659(9) Uani 1 2 d SD . . 
H2W H 0.537(2) 0.466(3) 0.255(3) 0.075(11) Uiso 1 1 d D . . 
C1 C 0.59020(10) 0.68141(16) 0.44282(13) 0.0248(4) Uani 1 1 d . . . 
C4 C 0.60666(11) 0.90115(17) 0.57328(12) 0.0268(4) Uani 1 1 d . . . 
C11 C 0.70387(11) 0.31174(17) 0.31161(13) 0.0269(4) Uani 1 1 d . . . 
C14 C 0.82094(11) 0.11819(17) 0.40240(13) 0.0271(4) Uani 1 1 d . . . 
C12 C 0.74310(11) 0.20731(18) 0.25943(13) 0.0278(4) Uani 1 1 d . . . 
H12A H 0.7522 0.2363 0.1976 0.033 Uiso 1 1 calc R . . 
H12B H 0.7046 0.1383 0.2541 0.033 Uiso 1 1 calc R . . 
C13 C 0.82431(11) 0.15916(17) 0.30241(13) 0.0261(4) Uani 1 1 d . . . 
H13 H 0.8397 0.0860 0.2668 0.031 Uiso 1 1 calc R . . 
C3 C 0.55298(12) 0.78806(18) 0.59243(14) 0.0297(4) Uani 1 1 d . . . 
H3 H 0.5578 0.7727 0.6589 0.036 Uiso 1 1 calc R . . 
C2 C 0.57929(13) 0.66917(17) 0.54510(14) 0.0302(4) Uani 1 1 d . . . 
H2A H 0.6308 0.6411 0.5746 0.036 Uiso 1 1 calc R . . 
H2B H 0.5385 0.6052 0.5546 0.036 Uiso 1 1 calc R . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Zn1 O11 1.9313(15) . ? 
Zn1 O1 1.9496(14) . ? 
Zn1 O4 1.9682(14) 7_666 ? 
Zn1 O14 1.9762(15) 7_656 ? 
O4 C4 1.269(2) . ? 
O4 Zn1 1.9682(14) 7_666 ? 
O2 C1 1.254(2) . ? 
O1 C1 1.262(2) . ? 
O14 C14 1.277(2) . ? 
O14 Zn1 1.9762(15) 7_656 ? 
O11 C11 1.272(2) . ? 
O13 C14 1.223(2) . ? 
O12 C11 1.231(2) . ? 
O3 C4 1.233(2) . ? 
N13 C13 1.487(2) . ? 
N3 C3 1.482(3) . ? 
C1 C2 1.513(3) . ? 
C4 C3 1.530(3) . ? 
C11 C12 1.513(3) . ? 
C14 C13 1.523(3) . ? 
C12 C13 1.522(2) . ? 
C3 C2 1.522(3) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O11 Zn1 O1 111.58(6) . . ? 
O11 Zn1 O4 106.53(6) . 7_666 ? 
O1 Zn1 O4 99.31(6) . 7_666 ? 
O11 Zn1 O14 114.74(7) . 7_656 ? 
O1 Zn1 O14 120.39(6) . 7_656 ? 
O4 Zn1 O14 101.33(6) 7_666 7_656 ? 
C4 O4 Zn1 123.92(13) . 7_666 ? 
C1 O1 Zn1 134.19(13) . . ? 
C14 O14 Zn1 109.47(12) . 7_656 ? 
C11 O11 Zn1 128.38(13) . . ? 
O2 C1 O1 121.99(18) . . ? 
O2 C1 C2 118.94(16) . . ? 
O1 C1 C2 119.05(16) . . ? 
O3 C4 O4 127.02(18) . . ? 
O3 C4 C3 118.89(17) . . ? 
O4 C4 C3 114.01(16) . . ? 
O12 C11 O11 125.44(18) . . ? 
O12 C11 C12 120.26(17) . . ? 
O11 C11 C12 114.29(16) . . ? 
O13 C14 O14 124.07(18) . . ? 
O13 C14 C13 120.72(17) . . ? 
O14 C14 C13 115.08(16) . . ? 
C11 C12 C13 115.20(15) . . ? 
N13 C13 C12 111.71(15) . . ? 
N13 C13 C14 108.63(15) . . ? 
C12 C13 C14 114.57(15) . . ? 
N3 C3 C2 112.35(16) . . ? 
N3 C3 C4 108.62(16) . . ? 
C2 C3 C4 113.94(16) . . ? 
C1 C2 C3 114.97(16) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C1 C2 C3 N3 72.7(2) . . . . ? 
C1 C2 C3 C4 -51.4(2) . . . . ? 
N3 C3 C4 O3 30.6(2) . . . . ? 
O2 C1 C2 C3 -28.1(2) . . . . ? 
C11 C12 C13 N13 -69.7(2) . . . . ? 
C11 C12 C13 C14 54.4(2) . . . . ? 
N13 C13 C14 O13 -11.5(2) . . . . ? 
O12 C11 C12 C13 -156.33(19) . . . . ? 
Zn1 O1 C1 C2 -19.2(3) . . . . ? 
Zn1 O11 C11 C12 -173.08(14) . . . . ? 
Zn1 O4 C4 C3 167.31(12) . 7_666 7_666 7_666 ? 
Zn1 O14 C14 C13 -176.44(12) . 7_656 7_656 7_656 ? 
 

_olex2_submission_special_instructions  'No special instructions were received'

# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_0_05GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972146'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_0_05GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.160 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_0_05GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.031 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     16.210(4)
_cell_length_b                     10.6863(6)
_cell_length_c                     14.4936(9)
_cell_angle_alpha                  90
_cell_angle_beta                   92.95(3)
_cell_angle_gamma                  90
_cell_volume                       2507.3(7)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      351
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         50000 
_cell_measurement_theta_max        26.413
_cell_measurement_theta_min        3.813
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.013
_exptl_absorpt_correction_T_max    0.904
_exptl_absorpt_correction_T_min    0.675
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.05(2) GPa
 (50000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
; 
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.889
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0235
_diffrn_reflns_av_unetI/netI       0.0101
_diffrn_reflns_Laue_measured_fraction_full  0.160
_diffrn_reflns_Laue_measured_fraction_max  0.146
_diffrn_reflns_limit_h_max         2
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         13
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              4042
_diffrn_reflns_point_group_measured_fraction_full  0.160
_diffrn_reflns_point_group_measured_fraction_max  0.146
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.413
_diffrn_reflns_theta_min           3.813
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.160
_diffrn_measured_fraction_theta_max  0.146
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  351
_reflns_number_total               378
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max           0.113
_refine_diff_density_min           -0.115
_refine_diff_density_rms           0.023
_refine_ls_goodness_of_fit_ref     1.101
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       199
_refine_ls_number_reflns           378
_refine_ls_number_restraints       127
_refine_ls_R_factor_all            0.0231
_refine_ls_R_factor_gt             0.0210
_refine_ls_restrained_S_all        0.949
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0404P)²+5.4767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0519
_refine_ls_wR_factor_ref           0.0540
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H2W-O2W
 0.85 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
 O1W-H1WA
 0.85 with sigma of 0.05
 O1W-H1WB
 0.85 with sigma of 0.05
 O14_$5-H1WA
 2 with sigma of 0.1
 H1WA-H1WB
 1.34 with sigma of 0.05
 O2-H1WB
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2W)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O1W) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.004 and sigma
for terminal atoms of 0.008
4.a Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7318(4) 0.50459(6) 0.45038(5) 0.024(2) Uani 1 1 d . U . . .
 O4 O 0.681(3) 0.8726(9) 0.5540(5) 0.034(3) Uani 1 1 d . U . . .
 O2 O 0.5485(13) 0.7608(3) 0.3983(3) 0.030(5) Uani 1 1 d D U . . .
 O1 O 0.639(2) 0.6086(4) 0.4051(3) 0.030(3) Uani 1 1 d . U . . .
 O14 O 0.7580(15) 0.0475(5) 0.4184(3) 0.036(3) Uani 1 1 d D U . . .
 O11 O 0.7551(15) 0.3755(4) 0.3623(3) 0.044(3) Uani 1 1 d . U . . .
 O13 O 0.877(2) 0.1447(5) 0.4588(3) 0.035(5) Uani 1 1 d . U . . .
 O12 O 0.626(2) 0.3323(8) 0.3014(6) 0.049(6) Uani 1 1 d D U . . .
 O3 O 0.577(2) 1.0065(4) 0.5825(5) 0.039(5) Uani 1 1 d . U . . .
 N13 N 0.888(2) 0.2514(5) 0.2948(4) 0.030(5) Uani 1 1 d . U . . .
 H13A H 0.9032 0.2616 0.2371 0.037 Uiso 1 1 calc R . . . . 
 H13B H 0.9359 0.2261 0.3282 0.037 Uiso 1 1 calc R . . . . 
 H13C H 0.8752 0.3250 0.3180 0.037 Uiso 1 1 calc R . . . . 
 O1W O 0.6051(17) 0.9874(9) 0.3316(8) 0.052(5) Uani 1 1 d D U . . .
 H1WA H 0.657(4) 0.994(13) 0.338(10) 0.063 Uiso 1 1 d DR . . . .
 H1WB H 0.593(10) 0.928(6) 0.367(5) 0.063 Uiso 1 1 d DR . . . .
 N3 N 0.469(4) 0.8203(10) 0.5689(6) 0.037(6) Uani 1 1 d . U . . .
 H3A H 0.4608 0.8449 0.5102 0.044 Uiso 1 1 calc R . . .  .
 H3B H 0.4505 0.8821 0.6050 0.044 Uiso 1 1 calc R . . . .
 H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc R . . . .
 O2W O 0.500000 0.5205(9) 0.250000 0.072(6) Uani 1 2 d DS TU P . .
 H2W H 0.538(7) 0.472(6) 0.278(5) 0.06(4) Uiso 1 1 d D . . . .
 C1 C 0.590(4) 0.6807(6) 0.4423(5) 0.024(3) Uani 1 1 d . U . . .
 C4 C 0.607(4) 0.9019(9) 0.5728(7) 0.023(4) Uani 1 1 d . U . . .
 C11 C 0.706(4) 0.3138(13) 0.3099(8) 0.023(4) Uani 1 1 d . U . . .
 C14 C 0.820(3) 0.1175(6) 0.4020(5) 0.022(3) Uani 1 1 d . U . . .
 C12 C 0.743(3) 0.2076(6) 0.2584(4) 0.024(3) Uani 1 1 d . U . . .
 H12A H 0.703756 0.139443 0.254129 0.029 Uiso 1 1 calc R . . . .
 H12B H 0.752479 0.235219 0.196003 0.029 Uiso 1 1 calc R . . . .
 C13 C 0.823(2) 0.1588(6) 0.3011(4) 0.025(3) Uani 1 1 d . U . . .
 H13 H 0.839066 0.085722 0.265171 0.030 Uiso 1 1 calc R . . . .
 C3 C 0.554(3) 0.7880(10) 0.5930(8) 0.06(6) Uani 1 1 d . . . . .
 H3 H 0.558567 0.773291 0.659759 0.075 Uiso 1 1 calc R . . . .
 C2 C 0.5767(19) 0.6678(5) 0.5459(4) 0.024(3) Uani 1 1 d . U . . .
 H2A H 0.533177 0.607083 0.553838 0.029 Uiso 1 1 calc R . . . .
 H2B H 0.626809 0.635126 0.576370 0.029 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.94(4) 7_666 ?
 Zn1 O1 1.96(3) . ?
 Zn1 O14 1.980(4) 7_656 ?
 Zn1 O11 1.930(7) . ?
 O4 C4 1.28(8) . ?
 O2 C1 1.25(3) . ?
 O1 C1 1.24(5) . ?
 O14 C14 1.29(4) . ?
 O11 C11 1.26(4) . ?
 O13 C14 1.23(3) . ?
 O12 C11 1.32(8) . ?
 O3 C4 1.23(3) . ?
 N13 C13 1.45(3) . ?
 N3 C3 1.44(10) . ?
 C1 C2 1.535(17) . ?
 C4 C3 1.52(5) . ?
 C11 C12 1.50(3) . ?
 C14 C13 1.531(10) . ?
 C12 C13 1.50(5) . ?
 C3 C2 1.509(19) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 99.1(12) 7_666 . ?
 O4 Zn1 O14 101.3(7) 7_666 7_656 ?
 O1 Zn1 O14 120.4(8) . 7_656 ?
 O11 Zn1 O4 107.1(9) . 7_666 ?
 O11 Zn1 O1 110.9(5) . . ?
 O11 Zn1 O14 115.1(3) . 7_656 ?
 C4 O4 Zn1 122.5(13) . 7_666 ?
 C1 O1 Zn1 134.4(13) . . ?
 C14 O14 Zn1 108.2(11) . 7_656 ?
 C11 O11 Zn1 129(2) . . ?
 O2 C1 C2 117(3) . . ?
 O1 C1 O2 122.9(10) . . ?
 O1 C1 C2 120(2) . . ?
 O4 C4 C3 112.6(19) . . ?
 O3 C4 O4 129(4) . . ?
 O3 C4 C3 119(5) . . ?
 O11 C11 O12 125(2) . . ?
 O11 C11 C12 116(4) . . ?
 O12 C11 C12 119(3) . . ?
 O14 C14 C13 114(2) . . ?
 O13 C14 O14 125.2(11) . . ?
 O13 C14 C13 121(3) . . ?
 C13 C12 C11 114.7(19) . . ?
 N13 C13 C14 108.4(16) . . ?
 N13 C13 C12 110.5(13) . . ?
 C12 C13 C14 115(2) . . ?
 N3 C3 C4 107(2) . . ?
 N3 C3 C2 110(2) . . ?
 C2 C3 C4 116(3) . . ?
 C3 C2 C1 114.6(9) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O4 C4 C3 167.4(8) . 7_666 7_666 7_666 ?
 Zn1 O1 C1 C2 -22(6) . . . . ?
 Zn1 O14 C14 C13 -176.6(14) . 7_656 7_656 7_656 ?
 Zn1 O11 C11 C12 -172.1(9) . . . . ?
 O2 C1 C2 C3 -32(4) . . . . ?
 O12 C11 C12 C13 -154.5(19) . . . . ?
 N13 C13 C14 O13 -13(3) . . . . ?
 N3 C3 C4 O3 32(2) . . . . ?
 C1 C2 C3 N3 75(4) . . . . ?
 C1 C2 C3 C4 -47(4) . . . . ?
 C11 C12 C13 N13 -68(2) . . . . ?
 C11 C12 C13 C14 55(2) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_0_29GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972147'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_0_29GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.341 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 

_cell_length_a                     16.206(3)
_cell_length_b                     10.6965(4)
_cell_length_c                     14.4922(5)
_cell_angle_alpha                  90
_cell_angle_beta                   93.185(8)
_cell_angle_gamma                  90
_cell_volume                       2508.2(5)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      712
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         290000
_cell_measurement_theta_max        27.135
_cell_measurement_theta_min        4.569
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.012
_exptl_absorpt_correction_T_max    0.904
_exptl_absorpt_correction_T_min    0.747
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.29(2) GPa
 (290000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;
_exptl_crystal_colour             colourless
_exptl_crystal_density_diffrn     1.889 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_density_meas        ?
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.15
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0256
_diffrn_reflns_av_unetI/netI       0.0171
_diffrn_reflns_Laue_measured_fraction_full  0.341
_diffrn_reflns_Laue_measured_fraction_max  0.295
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -10
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              5096
_diffrn_reflns_point_group_measured_fraction_full  0.341
_diffrn_reflns_point_group_measured_fraction_max  0.295
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.135
_diffrn_reflns_theta_min           4.569
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.341
_diffrn_measured_fraction_theta_max  0.295
_diffrn_measurement_device_type    'multiwire proportional' 
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'

_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  712
_reflns_number_total               823
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.322
_refine_diff_density_min           -0.216
_refine_diff_density_rms           0.044
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.107
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       200
_refine_ls_number_reflns           823
_refine_ls_number_restraints       32
_refine_ls_R_factor_all            0.0378
_refine_ls_R_factor_gt             0.0300
_refine_ls_restrained_S_all        1.102
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0408P)²+7.4628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0756
_refine_ls_wR_factor_ref           0.0796
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2W-H2W
 1 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(H2W)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C11) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Zn1 Zn 0.73109(7) 0.50456(5) 0.45041(4) 0.0254(7) Uani 1 1 d . . . . . 
O4 O 0.6792(5) 0.8729(3) 0.5534(3) 0.040(4) Uani 1 1 d . . . . . 
O2 O 0.5483(4) 0.7615(3) 0.3981(3) 0.029(3) Uani 1 1 d . . . . .
O1 O 0.6395(4) 0.6085(3) 0.4050(3) 0.036(4) Uani 1 1 d . . . . .
O14 O 0.7582(5) 0.0480(4) 0.4182(3) 0.038(4) Uani 1 1 d . . . . .
O11 O 0.7552(5) 0.3760(4) 0.3625(3) 0.044(4) Uani 1 1 d . . . . .
O13 O 0.8751(5) 0.1447(4) 0.4585(3) 0.038(4) Uani 1 1 d . . . . .
O12 O 0.6301(6) 0.3312(4) 0.3012(4) 0.0492(16) Uani 1 1 d DU . . . .
O3 O 0.5767(5) 1.0067(3) 0.5819(3) 0.042(4) Uani 1 1 d . . . . . 
N13 N 0.8919(6) 0.2518(5) 0.2953(3) 0.035(5) Uani 1 1 d . . . . . 
H13A H 0.9032 0.2616 0.2371 0.037 Uiso 1 1 calc R . . . . 
H13B H 0.9359 0.2261 0.3282 0.037 Uiso 1 1 calc R . . . .
H13C H 0.8752 0.3250 0.3180 0.037 Uiso 1 1 calc R . . . .
O1W O 0.6063(7) 0.9871(4) 0.3309(4) 0.067(5) Uani 1 1 d G . . . .
H1WA H 0.6520 1.0165 0.3527 0.090 Uiso 1 1 d G . . . .
H1WB H 0.5985 0.9222 0.3631 0.090 Uiso 1 1 d G . . . .
N3 N 0.4665(9) 0.8202(6) 0.5686(5) 0.046(7) Uani 1 1 d . . . . .
H3A H 0.4608 0.8449 0.5102 0.044 Uiso 1 1 calc R . . . .
H3B H 0.4505 0.8821 0.6050 0.044 Uiso 1 1 calc R . . . .
H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc R . . . . 
O2W O 0.5000 0.5199(7) 0.2500 0.071(3) Uani 1 2 d SDU . . . .
H2W H 0.554(5) 0.475(7) 0.246(7) 0.14(4) Uani 1 1 d DU . . . . 
C1 C 0.5882(6) 0.6810(5) 0.4419(4) 0.029(5) Uani 1 1 d . . . . .
C4 C 0.6084(8) 0.9009(5) 0.5740(4) 0.029(6) Uani 1 1 d . . . . .
C11 C 0.7038(8) 0.3126(5) 0.3108(5) 0.028(2) Uani 1 1 d U . . . .
C14 C 0.8204(7) 0.1176(5) 0.4015(4) 0.0275(14) Uani 1 1 d U . . . . 
C12 C 0.7447(11) 0.2080(7) 0.2587(5) 0.033(7) Uani 1 1 d . . . . .
H12A H 0.7057 0.1394 0.2514 0.040 Uiso 1 1 calc R . . . . 
H12B H 0.7551 0.2383 0.1974 0.040 Uiso 1 1 calc R . . . . 
C13 C 0.8230(9) 0.1581(7) 0.3008(4) 0.026(7) Uani 1 1 d . . . . . 
H13 H 0.8378 0.0846 0.2649 0.031 Uiso 1 1 calc R . . . . 
C3 C 0.5521(11) 0.7874(7) 0.5924(5) 0.034(8) Uani 1 1 d . . . . . 
H3 H 0.5565 0.7719 0.6591 0.041 Uiso 1 1 calc R . . . . 
C2 C 0.5782(6) 0.6686(4) 0.5459(3) 0.027(5) Uani 1 1 d . . . . . 
H2A H 0.5374 0.6043 0.5560 0.032 Uiso 1 1 calc R . . . .
H2B H 0.6303 0.6409 0.5752 0.032 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.960(7) 7_666 ?
 Zn1 O1 1.940(6) . ?
 Zn1 O14 1.984(4) 7_656 ?
 Zn1 O11 1.930(4) . ?
 O4 C4 1.239(13) . ?
 O2 C1 1.232(9) . ?
 O1 C1 1.276(8) . ?
 O14 C14 1.288(10) . ?
 O11 C11 1.282(13) . ?
 O13 C14 1.212(12) . ?
 O12 C11 1.212(15) . ?
 O3 C4 1.251(8) . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.507(17) . ?
 O1W H1WA 0.8499 . ?
 O1W H1WB 0.8501 . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.45(2) . ?
 O2W H2W 1.01(5) . ?
 C1 C2 1.530(7) . ?
 C4 C3 1.551(16) . ?
 C11 C12 1.522(9) . ?
 C14 C13 1.525(8) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.48(2) . ?
 C13 H13 0.9800 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.510(8) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O14 101.0(2) 7_666 7_656 ?
 O1 Zn1 O4 99.3(2) . 7_666 ?
 O1 Zn1 O14 120.8(2) . 7_656 ?
 O11 Zn1 O4 106.3(3) . 7_666 ?
 O11 Zn1 O1 111.3(3) . . ?
 O11 Zn1 O14 115.0(2) . 7_656 ?
 C4 O4 Zn1 122.9(4) . 7_666 ?
 C1 O1 Zn1 135.2(4) . . ?
 C14 O14 Zn1 108.4(6) . 7_656 ?
 C11 O11 Zn1 127.9(7) . . ?
 H13A N13 H13B 111.0 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 109.5 . . ?
 H1WA O1W H1WB 104.5 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 109.5 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 109.5 . . ?
 O2 C1 O1 122.9(5) . . ?
 O2 C1 C2 119.2(6) . . ?
 O1 C1 C2 117.9(6) . . ?
 O4 C4 O3 129.2(8) . . ?
 O4 C4 C3 114.5(7) . . ?
 O3 C4 C3 116.3(10) . . ?
 O11 C11 C12 113.1(12) . . ?
 O12 C11 O11 125.7(7) . . ?
 O12 C11 C12 121.2(12) . . ?
 O14 C14 C13 114.0(10) . . ?
 O13 C14 O14 124.1(5) . . ?
 O13 C14 C13 121.8(9) . . ?
 C11 C12 H12A 108.1 . . ?
 C11 C12 H12B 108.1 . . ?
 H12A C12 H12B 107.3 . . ?
 C13 C12 C11 116.6(11) . . ?
 C13 C12 H12A 108.1 . . ?
 C13 C12 H12B 108.1 . . ?
 N13 C13 C14 107.4(10) . . ?
 N13 C13 H13 107.5 . . ?
 C14 C13 H13 107.5 . . ?
 C12 C13 N13 111.1(7) . . ?
 C12 C13 C14 115.5(10) . . ?
 C12 C13 H13 107.5 . . ?
 N3 C3 C4 109.5(7) . . ?
 N3 C3 H3 106.9 . . ?
 N3 C3 C2 112.6(12) . . ?
 C4 C3 H3 106.9 . . ?
 C2 C3 C4 113.6(9) . . ?
 C2 C3 H3 106.9 . . ?
 C1 C2 H2A 108.6 . . ?
 C1 C2 H2B 108.6 . . ?
 C3 C2 C1 114.5(5) . . ?
 C3 C2 H2A 108.6 . . ?
 C3 C2 H2B 108.6 . . ?
 H2A C2 H2B 107.6 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -17.2(11) . . . . ?
 Zn1 O11 C11 C12 -172.9(4) . . . . ?
 O2 C1 C2 C3 -26.4(13) . . . . ?
 O12 C11 C12 C13 -155.1(11) . . . . ?
 N13 C13 C14 O13 -10.9(11) . . . . ?
 N3 C3 C4 O3 29.4(9) . . . . ?
 C1 C2 C3 N3 71.9(11) . . . . ?
 C1 C2 C3 C4 -53.3(13) . . . . ?
 C11 C12 C13 N13 -70.4(9) . . . . ?
 C11 C12 C13 C14 52.2(16) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_0_49GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972148'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_0_49GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.341 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_0_49GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H3B      .       1.98 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 

_cell_length_a                     16.191(4)
_cell_length_b                     10.6521(5)
_cell_length_c                     14.4247(6)
_cell_angle_alpha                  90
_cell_angle_beta                   93.183(9)
_cell_angle_gamma                  90
_cell_volume                       2484.0(6)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      692
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         490000
_cell_measurement_theta_max        54.536
_cell_measurement_theta_min        9.166
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.032
_exptl_absorpt_correction_T_max    0.903
_exptl_absorpt_correction_T_min    0.549
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.49(2) GPa
 (490000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.907
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.30
_exptl_crystal_size_mid            0.30
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0250
_diffrn_reflns_av_unetI/netI       0.0190
_diffrn_reflns_Laue_measured_fraction_full  0.341
_diffrn_reflns_Laue_measured_fraction_max  0.292
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -10
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              5033
_diffrn_reflns_point_group_measured_fraction_full  0.341
_diffrn_reflns_point_group_measured_fraction_max  0.292
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.268
_diffrn_reflns_theta_min           4.583
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.341
_diffrn_measured_fraction_theta_max  0.292
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  692
_reflns_number_total               816
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.302
_refine_diff_density_min           -0.169
_refine_diff_density_rms           0.044
_refine_ls_goodness_of_fit_ref     1.110
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       196
_refine_ls_number_reflns           816
_refine_ls_number_restraints       14
_refine_ls_R_factor_all            0.0364
_refine_ls_R_factor_gt             0.0272
_refine_ls_restrained_S_all        1.102
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0407P)²+4.3878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0692
_refine_ls_wR_factor_ref           0.0742
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2W-H2W
 1 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
Zn1 Zn 0.73180(7) 0.50506(5) 0.45075(4) 0.0258(7) Uani 1 1 d . . . . . 
O4 O 0.6789(5) 0.8724(3) 0.5528(3) 0.037(4) Uani 1 1 d . . . . . 
O2 O 0.5477(4) 0.7609(3) 0.3982(2) 0.026(3) Uani 1 1 d . . . . . 
O1 O 0.6392(4) 0.6085(3) 0.4055(2) 0.039(4) Uani 1 1 d . . . . . 
O14 O 0.7566(5) 0.0476(3) 0.4173(3) 0.043(4) Uani 1 1 d . . . . . 
O11 O 0.7557(5) 0.3763(4) 0.3617(3) 0.039(4) Uani 1 1 d . . . . . 
O13 O 0.8743(5) 0.1439(3) 0.4586(3) 0.035(4) Uani 1 1 d . . . . .
O12 O 0.6298(6) 0.3330(4) 0.3006(4) 0.038(5) Uani 1 1 d D . . . . 
O3 O 0.5761(5) 1.0068(3) 0.5830(3) 0.042(4) Uani 1 1 d . . . . . 
N13 N 0.8915(6) 0.2513(4) 0.2946(3) 0.036(5) Uani 1 1 d . . . . . 
H13A H 0.9079 0.2549 0.2368 0.043 Uiso 1 1 calc R . . . . 
H13B H 0.9336 0.2272 0.3327 0.043 Uiso 1 1 calc R . . . . 
H13C H 0.8741 0.3267 0.3116 0.043 Uiso 1 1 calc R . . . . 
O1W O 0.6054(6) 0.9869(4) 0.3291(4) 0.069(4) Uani 1 1 d G . . . .  
H1WA H 0.6467 1.0253 0.3535 0.0803 Uiso 1 1 d G . . . . 
H1WB H 0.5979 0.9261 0.3652 0.0803 Uiso 1 1 d G . . . . 
N3 N 0.4652(8) 0.8197(6) 0.5691(4) 0.046(6) Uani 1 1 d . . . . .  
H3A H 0.4593 0.8351 0.5085 0.055 Uiso 1 1 calc R . . . . 
H3B H 0.4514 0.8878 0.6005 0.055 Uiso 1 1 calc R . . . . 
H3C H 0.4324 0.7562 0.5833 0.055 Uiso 1 1 calc R . . . . 
O2W O 0.5000 0.5203(6) 0.2500 0.064(6) Uani 1 2 d SD . . . .
H2W H 0.555(5) 0.478(7) 0.249(7) 0.085(5) Uiso 1 1 d D . . . . 
C1 C 0.5885(6) 0.6811(4) 0.4427(4) 0.028(4) Uani 1 1 d . . . . . 
C4 C 0.6081(7) 0.9003(5) 0.5741(4) 0.030(6) Uani 1 1 d . . . . . 
C11 C 0.7031(10) 0.3133(6) 0.3102(6) 0.028(2) Uani 1 1 d U . . . . 
C14 C 0.8192(7) 0.1173(4) 0.4005(4) 0.0271(19) Uani 1 1 d U . . . . 
C12 C 0.7437(10) 0.2087(6) 0.2572(5) 0.034(7) Uani 1 1 d . . . . . 
H12A H 0.7044 0.1403 0.2491 0.040 Uiso 1 1 calc R . . . . 
H12B H 0.7545 0.2400 0.1959 0.040 Uiso 1 1 calc R . . . . 
C13 C 0.8214(9) 0.1575(6) 0.2993(4) 0.029(7) Uani 1 1 d . . . . .  
H13 H 0.8359 0.0836 0.2631 0.035 Uiso 1 1 calc R . . . . 
C3 C 0.5506(10) 0.7870(7) 0.5938(5) 0.026(7) Uani 1 1 d . . . . . 
H3 H 0.5550 0.7719 0.6609 0.032 Uiso 1 1 calc R . . . . 
C2 C 0.5775(5) 0.6670(4) 0.5467(3) 0.031(5) Uani 1 1 d . . . . . 
H2A H 0.5366 0.6023 0.5558 0.038 Uiso 1 1 calc R . . . . 
H2B H 0.6294 0.6390 0.5766 0.038 Uiso 1 1 calc R . . . . 


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.950(6) 7_666 ?
 Zn1 O1 1.944(6) . ?
 Zn1 O14 1.983(4) 7_656 ?
 Zn1 O11 1.933(4) . ?
 O4 C4 1.240(12) . ?
 O2 C1 1.234(9) . ?
 O1 C1 1.268(8) . ?
 O14 C14 1.291(10) . ?
 O11 C11 1.287(17) . ?
 O13 C14 1.223(11) . ?
 O12 C11 1.206(19) . ?
 O3 C4 1.257(8) . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.516(16) . ?
 O1W H1WA 0.8444 . ?
 O1W H1WB 0.8441 . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.45(2) . ?
 O2W H2W 1.00(5) . ?
 C1 C2 1.528(6) . ?
 C4 C3 1.559(15) . ?
 C11 C12 1.522(8) . ?
 C14 C13 1.523(7) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.47(2) . ?
 C13 H13 0.9800 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.523(7) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O14 100.6(2) 7_666 7_656 ?
 O1 Zn1 O4 99.8(2) . 7_666 ?
 O1 Zn1 O14 120.8(2) . 7_656 ?
 O11 Zn1 O4 106.3(2) . 7_666 ?
 O11 Zn1 O1 111.0(3) . . ?
 O11 Zn1 O14 115.2(2) . 7_656 ?
 C4 O4 Zn1 122.9(4) . 7_666 ?
 C1 O1 Zn1 135.2(4) . . ?
 C14 O14 Zn1 108.0(5) . 7_656 ?
 C11 O11 Zn1 127.1(8) . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 109.5 . . ?
 H1WA O1W H1WB 104.7 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 109.5 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 109.5 . . ?
 O2 C1 O1 122.7(4) . . ?
 O2 C1 C2 119.4(5) . . ?
 O1 C1 C2 117.9(6) . . ?
 O4 C4 O3 129.3(7) . . ?
 O4 C4 C3 115.4(6) . . ?
 O3 C4 C3 115.3(9) . . ?
 O11 C11 C12 112.4(14) . . ?
 O12 C11 O11 126.2(7) . . ?
 O12 C11 C12 121.3(14) . . ?
 O14 C14 C13 113.7(9) . . ?
 O13 C14 O14 123.6(5) . . ?
 O13 C14 C13 122.6(8) . . ?
 C11 C12 H12A 108.1 . . ?
 C11 C12 H12B 108.1 . . ?
 H12A C12 H12B 107.3 . . ?
 C13 C12 C11 116.6(11) . . ?
 C13 C12 H12A 108.1 . . ?
 C13 C12 H12B 108.1 . . ?
 N13 C13 C14 106.5(9) . . ?
 N13 C13 H13 107.6 . . ?
 C14 C13 H13 107.6 . . ?
 C12 C13 N13 111.3(6) . . ?
 C12 C13 C14 115.8(9) . . ?
 C12 C13 H13 107.6 . . ?
 N3 C3 C4 109.9(7) . . ?
 N3 C3 H3 107.2 . . ?
 N3 C3 C2 112.6(11) . . ?
 C4 C3 H3 107.2 . . ?
 C2 C3 C4 112.4(8) . . ?
 C2 C3 H3 107.2 . . ?
 C1 C2 H2A 108.7 . . ?
 C1 C2 H2B 108.7 . . ?
 C3 C2 C1 114.0(4) . . ?
 C3 C2 H2A 108.7 . . ?
 C3 C2 H2B 108.7 . . ?
 H2A C2 H2B 107.6 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -19.4(10) . . . . ?
 Zn1 O11 C11 C12 -172.9(4) . . . . ?
 O2 C1 C2 C3 -27.9(12) . . . . ?
 O12 C11 C12 C13 -155.2(11) . . . . ?
 N13 C13 C14 O13 -10.8(10) . . . . ?
 N3 C3 C4 O3 31.0(8) . . . . ?
 C1 C2 C3 N3 72.1(10) . . . . ?
 C1 C2 C3 C4 -52.6(12) . . . . ?
 C11 C12 C13 N13 -70.6(9) . . . . ?
 C11 C12 C13 C14 51.2(16) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_0_79GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972149'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_0_79GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.352 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_0_79GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.02 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_0_79GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H3B      .       1.94 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 

_cell_length_a                     16.098(2)
_cell_length_b                     10.605(2)
_cell_length_c                     14.405(2)
_cell_angle_alpha                  90
_cell_angle_beta                   93.218(16)
_cell_angle_gamma                  90
_cell_volume                       2455.3(7)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      571
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         790000
_cell_measurement_theta_max        26.862
_cell_measurement_theta_min        3.705
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.056
_exptl_absorpt_correction_T_max    0.902
_exptl_absorpt_correction_T_min    0.698
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.79(2) GPa
 (790000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.929
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0636
_diffrn_reflns_av_unetI/netI       0.0507
_diffrn_reflns_Laue_measured_fraction_full  0.352
_diffrn_reflns_Laue_measured_fraction_max  0.311
_diffrn_reflns_limit_h_max         18
_diffrn_reflns_limit_h_min         -18
_diffrn_reflns_limit_k_max         10
_diffrn_reflns_limit_k_min         -10
_diffrn_reflns_limit_l_max         15
_diffrn_reflns_limit_l_min         -15
_diffrn_reflns_number              4921
_diffrn_reflns_point_group_measured_fraction_full  0.352
_diffrn_reflns_point_group_measured_fraction_max  0.311
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.862
_diffrn_reflns_theta_min           3.705
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.352
_diffrn_measured_fraction_theta_max  0.311
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  571
_reflns_number_total               824
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.443
_refine_diff_density_min           -0.440
_refine_diff_density_rms           0.111
_refine_ls_goodness_of_fit_ref     1.145
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       196
_refine_ls_number_reflns           824
_refine_ls_number_restraints       32
_refine_ls_R_factor_all            0.0989
_refine_ls_R_factor_gt             0.0620
_refine_ls_restrained_S_all        1.121
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.1168P)²+15.7225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1739
_refine_ls_wR_factor_ref           0.1988
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2W-H2W
 1 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(O2W) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
Zn1 Zn 0.73234(10) 0.50539(16) 0.45125(12) 0.0332(8) Uani 1 1 d . . . . .  
O4 O 0.6772(5) 0.8718(10) 0.5519(7) 0.041(3) Uani 1 1 d . . . . . 
O2 O 0.5478(6) 0.7613(11) 0.3980(7) 0.032(3) Uani 1 1 d U . . . . 
O1 O 0.6400(6) 0.6080(10) 0.4060(7) 0.042(3) Uani 1 1 d . . . . . 
O14 O 0.7553(7) 0.0453(11) 0.4166(7) 0.053(3) Uani 1 1 d . . . . . 
O11 O 0.7553(6) 0.3770(13) 0.3601(9) 0.051(4) Uani 1 1 d . . . . . 
O13 O 0.8728(8) 0.1429(13) 0.4587(9) 0.053(4) Uani 1 1 d . . . . . 
O12 O 0.6285(7) 0.3329(9) 0.2995(8) 0.049(3) Uani 1 1 d D . . . . 
O3 O 0.5758(6) 1.0055(10) 0.5822(8) 0.045(3) Uani 1 1 d . . . . . 
N13 N 0.8913(7) 0.2536(12) 0.2936(8) 0.037(3) Uani 1 1 d . . . . . 
H13A H 0.9036 0.2635 0.2346 0.044 Uiso 1 1 calc R . . . . 
H13B H 0.9364 0.2276 0.3269 0.044 Uiso 1 1 calc R . . . . 
H13C H 0.8742 0.3267 0.3161 0.044 Uiso 1 1 calc R . . . . 
O1W O 0.6014(9) 0.9870(15) 0.3282(9) 0.076(5) Uani 1 1 d G . . . . 
H1WA H 0.6435 1.0264 0.3494 0.114 Uiso 1 1 d G . . . . 
H1WB H 0.5890 0.9389 0.3718 0.114 Uiso 1 1 d G . . . . 
N3 N 0.46595(11) 0.82054(17) 0.56868(13) 0.056(4) Uani 1 1 d . . . . . 
H3A H 0.4608 0.8449 0.5102 0.044 Uiso 1 1 calc R . . . . 
H3B H 0.4505 0.8821 0.6050 0.044 Uiso 1 1 calc R . . . . 
H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc R . . . . 
O2W O 0.5000 0.522(3) 0.2500 0.068(6) Uani 1 2 d SDU . . . . 
H2W H 0.532(7) 0.453(12) 0.281(10) 0.04(5) Uiso 1 1 d D . . . . 
C1 C 0.5893(11) 0.680(2) 0.4426(13) 0.040(4) Uani 1 1 d U . . . . 
C4 C 0.6031(9) 0.8995(17) 0.5728(11) 0.037(4) Uani 1 1 d U . . . . 
C11 C 0.7035(12) 0.3127(17) 0.3105(12) 0.032(4) Uani 1 1 d U . . . . 
C14 C 0.8185(12) 0.1178(17) 0.3993(12) 0.041(5) Uani 1 1 d . . . . . 
C12 C 0.7419(9) 0.2078(14) 0.2567(11) 0.036(4) Uani 1 1 d . . . . . 
H12A H 0.7511 0.2382 0.1945 0.043 Uiso 1 1 calc R . . . . 
H12B H 0.7025 0.1387 0.2507 0.043 Uiso 1 1 calc R . . . . 
C13 C 0.8236(9) 0.1573(15) 0.2992(10) 0.038(4) Uani 1 1 d . . . . .  
H13 H 0.8391 0.0833 0.2634 0.046 Uiso 1 1 calc R . . . . 
C3 C 0.5487(9) 0.7862(15) 0.5913(11) 0.039(4) Uani 1 1 d . . . . .  
H3 H 0.5520 0.7725 0.6587 0.046 Uiso 1 1 calc R . . . . 
C2 C 0.5752(9) 0.6650(14) 0.5470(9) 0.033(4) Uani 1 1 d . . . . .  
H2A H 0.5327 0.6014 0.5547 0.039 Uiso 1 1 calc R . . . . 
H2B H 0.6262 0.6355 0.5789 0.039 Uiso 1 1 calc R . . . . 


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.956(9) 7_666 ?
 Zn1 O1 1.926(10) . ?
 Zn1 O14 1.977(10) 7_656 ?
 Zn1 O11 1.942(10) . ?
 O4 C4 1.282(16) . ?
 O2 C1 1.25(2) . ?
 O1 C1 1.256(19) . ?
 O14 C14 1.310(19) . ?
 O11 C11 1.27(2) . ?
 O13 C14 1.218(19) . ?
 O12 C11 1.23(2) . ?
 O3 C4 1.217(17) . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.499(18) . ?
 O1W H1WA 0.8396 . ?
 O1W H1WB 0.8415 . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.402(15) . ?
 O2W H2W 0.99(5) . ?
 C1 C2 1.54(2) . ?
 C4 C3 1.52(2) . ?
 C11 C12 1.51(2) . ?
 C14 C13 1.51(2) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.52(2) . ?
 C13 H13 0.9800 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.508(19) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O14 99.7(4) 7_666 7_656 ?
 O1 Zn1 O4 100.2(4) . 7_666 ?
 O1 Zn1 O14 120.9(4) . 7_656 ?
 O1 Zn1 O11 109.9(6) . . ?
 O11 Zn1 O4 106.3(4) . 7_666 ?
 O11 Zn1 O14 116.6(6) . 7_656 ?
 C4 O4 Zn1 123.9(11) . 7_666 ?
 C1 O1 Zn1 135.1(12) . . ?
 C14 O14 Zn1 107.8(11) . 7_656 ?
 C11 O11 Zn1 127.9(11) . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 109.5 . . ?
 H1WA O1W H1WB 104.6 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 109.5 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 111.00 . . ?
 C3 N3 H3C 108.00 . . ?
 O2 C1 O1 123.1(17) . . ?
 O2 C1 C2 118.0(16) . . ?
 O1 C1 C2 118.8(15) . . ?
 O4 C4 C3 114.5(15) . . ?
 O3 C4 O4 125.7(14) . . ?
 O3 C4 C3 119.7(13) . . ?
 O11 C11 C12 114.3(17) . . ?
 O12 C11 O11 126.2(17) . . ?
 O12 C11 C12 119.4(15) . . ?
 O14 C14 C13 115.4(16) . . ?
 O13 C14 O14 122.0(16) . . ?
 O13 C14 C13 122.3(16) . . ?
 C11 C12 H12A 108.5 . . ?
 C11 C12 H12B 108.5 . . ?
 C11 C12 C13 115.1(16) . . ?
 H12A C12 H12B 107.5 . . ?
 C13 C12 H12A 108.5 . . ?
 C13 C12 H12B 108.5 . . ?
 N13 C13 C14 108.7(13) . . ?
 N13 C13 C12 110.8(12) . . ?
 N13 C13 H13 108.1 . . ?
 C14 C13 C12 113.1(12) . . ?
 C14 C13 H13 108.1 . . ?
 C12 C13 H13 108.1 . . ?
 N3 C3 C4 108.2(13) . . ?
 N3 C3 H3 105.0 . . ?
 N3 C3 C2 114.3(12) . . ?
 C4 C3 H3 106.9 . . ?
 C2 C3 C4 114.9(11) . . ?
 C2 C3 H3 106.9 . . ?
 C1 C2 H2A 109.1 . . ?
 C1 C2 H2B 109.1 . . ?
 C3 C2 C1 112.6(13) . . ?
 C3 C2 H2A 109.1 . . ?
 C3 C2 H2B 109.1 . . ?
 H2A C2 H2B 107.8 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -21(3) . . . . ?
 Zn1 O11 C11 C12 -171.6(10) . . . . ?
 O2 C1 C2 C3 -30(3) . . . . ?
 O12 C11 C12 C13 -157.6(15) . . . . ?
 N13 C13 C14 O13 -14(2) . . . . ?
 N3 C3 C4 O3 33.0(19) . . . . ?
 C1 C2 C3 N3 74.0(17) . . . . ?
 C1 C2 C3 C4 -50.4(19) . . . . ?
 C11 C12 C13 N13 -69.0(15) . . . . ?
 C11 C12 C13 C14 53.3(18) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_0_85GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972150'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_0_85GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.204 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_0_85GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02617 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_0_85GPa
;
PROBLEM: Short Inter D-H..H-D       H1WB     ..H3B      .       1.94 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                    16.027(2) 
_cell_length_b                    10.5656(8) 
_cell_length_c                    14.3681(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.12(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2429.5(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_pressure        850000 
_cell_measurement_reflns_used     366 
_cell_measurement_theta_min       4.788 
_cell_measurement_theta_max       27.090 
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.950 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1464 
_exptl_absorpt_coefficient_mu     2.078 
_exptl_absorpt_correction_type    'integration' 
_exptl_absorpt_correction_T_min   0.695 
_exptl_absorpt_correction_T_max   0.901
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.85(2) GPa
 (850000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O11-C11
 1.27 with sigma of 0.05
 O1-C1
 1.25 with sigma of 0.05
 N3-C3
 1.4 with sigma of 0.05
 O4-C4
 1.25 with sigma of 0.05
 O12-C11
 1.25 with sigma of 0.05
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
 O1W-H1WA
 0.85 with sigma of 0.05
 O1W-H1WB
 0.85 with sigma of 0.05
 H1WA-H1WB
 1.34 with sigma of 0.05
 O2-H1WB
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O12) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C11) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C12) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C13) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O14) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O11) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O13) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O1W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O2W) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ? 
_diffrn_ambient_temperature       296(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'multiwire proportional' 
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_source                     'sealed x-ray tube'
_diffrn_reflns_number             5840 
_diffrn_reflns_av_R_equivalents   0.0886 
_diffrn_reflns_av_sigmaI/netI     0.0553 
_diffrn_reflns_limit_h_min        -3 
_diffrn_reflns_limit_h_max        3 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          4.79 
_diffrn_reflns_theta_max          27.09 
_reflns_number_total              549 
_reflns_number_gt                 366 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0000P)²+18.3211P] where P=(Fo²+2Fc²)/3'  
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0024(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          549 
_refine_ls_number_parameters      196 
_refine_ls_number_restraints      114 
_refine_ls_R_factor_all           0.0852 
_refine_ls_R_factor_gt            0.0417 
_refine_ls_wR_factor_ref          0.0738 
_refine_ls_wR_factor_gt           0.0614 
_refine_ls_goodness_of_fit_ref    1.143 
_refine_ls_restrained_S_all       1.034 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Zn1 Zn 0.7327(3) 0.50538(10) 0.45152(7) 0.036(5) Uani 1 1 d . . . 
O4 O 0.6821(19) 0.8699(8) 0.5530(6) 0.047(3) Uani 1 1 d DU . . 
O2 O 0.5444(13) 0.7613(5) 0.3993(4) 0.04(2) Uani 1 1 d D . . 
O1 O 0.6397(18) 0.6085(6) 0.4065(4) 0.038(3) Uani 1 1 d DU . . 
O14 O 0.7556(16) 0.0454(8) 0.4167(5) 0.049(3) Uani 1 1 d U . . 
O11 O 0.7568(15) 0.3774(6) 0.3617(5) 0.055(3) Uani 1 1 d DU . . 
O13 O 0.8715(16) 0.1431(7) 0.4586(5) 0.045(4) Uani 1 1 d U . . 
O12 O 0.625(2) 0.3358(10) 0.2995(7) 0.056(6) Uani 1 1 d DU . . 
O3 O 0.5716(17) 1.0069(6) 0.5838(5) 0.046(4) Uani 1 1 d U . . 
N13 N 0.894(2) 0.2494(8) 0.2930(6) 0.06(3) Uani 1 1 d . . . 
H13A H 0.9092 0.2550 0.2345 0.069 Uiso 1 1 calc R . . 
H13B H 0.9368 0.2215 0.3293 0.069 Uiso 1 1 calc R . . 
H13C H 0.8784 0.3254 0.3125 0.069 Uiso 1 1 calc R . . 
O1W O 0.6011(16) 0.9878(12) 0.3254(8) 0.068(3) Uani 1 1 d GDU . . 
H1WA H 0.6515 0.9969 0.3427 0.103 Uiso 1 1 d GD . . 
H1WB H 0.5821 0.9390 0.3650 0.103 Uiso 1 1 d GD . . 
N3 N 0.464(2) 0.8206(10) 0.5688(7) 0.046(5) Uani 1 1 d DU . . 
H3A H 0.4584 0.8274 0.5070 0.055 Uiso 1 1 calc R . . 
H3B H 0.4526 0.8944 0.5947 0.055 Uiso 1 1 calc R . . 
H3C H 0.4299 0.7614 0.5882 0.055 Uiso 1 1 calc R . . 
O2W O 0.5000 0.5215(14) 0.2500 0.071(6) Uani 1 2 d SDU . . 
H2W H 0.541(9) 0.475(11) 0.269(13) 0.12(8) Uiso 1 1 d D . . 
C1 C 0.587(2) 0.6796(9) 0.4430(6) 0.025(3) Uani 1 1 d DU . . 
C4 C 0.610(2) 0.8989(12) 0.5731(8) 0.027(4) Uani 1 1 d DU . . 
C11 C 0.702(2) 0.3159(16) 0.3068(10) 0.037(5) Uani 1 1 d DU . . 
C14 C 0.814(2) 0.1161(10) 0.4010(8) 0.06(4) Uani 1 1 d . . . 
C12 C 0.738(3) 0.2085(10) 0.2541(7) 0.041(4) Uani 1 1 d U . . 
H12A H 0.7458 0.2360 0.1909 0.049 Uiso 1 1 calc R . . 
H12B H 0.6972 0.1400 0.2509 0.049 Uiso 1 1 calc R . . 
C13 C 0.821(2) 0.1577(9) 0.2974(6) 0.031(3) Uani 1 1 d U . . 
H13 H 0.8355 0.0822 0.2621 0.037 Uiso 1 1 calc R . . 
C3 C 0.549(2) 0.7858(10) 0.5952(9) 0.039(4) Uani 1 1 d DU . . 
H3 H 0.5534 0.7710 0.6627 0.047 Uiso 1 1 calc R . . 
C2 C 0.5734(19) 0.6651(8) 0.5472(5) 0.031(3) Uani 1 1 d U . . 
H2A H 0.5299 0.6027 0.5549 0.038 Uiso 1 1 calc R . . 
H2B H 0.6244 0.6328 0.5779 0.038 Uiso 1 1 calc R . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Zn1 O4 1.90(2) 7_666 ? 
Zn1 O11 1.922(9) . ? 
Zn1 O1 1.93(2) . ? 
Zn1 O14 1.967(8) 7_656 ? 
O4 C4 1.25(4) . ? 
O4 Zn1 1.90(2) 7_666 ? 
O2 C1 1.25(2) . ? 
O1 C1 1.27(3) . ? 
O14 C14 1.22(3) . ? 
O14 Zn1 1.967(8) 7_656 ? 
O11 C11 1.32(3) . ? 
O13 C14 1.24(3) . ? 
O12 C11 1.26(4) . ? 
O3 C4 1.31(2) . ? 
N13 C13 1.52(4) . ? 
N13 H13A 0.8900 . ? 
N13 H13B 0.8900 . ? 
N13 H13C 0.8900 . ? 
O1W H1WA 0.8366 . ? 
O1W H1WB 0.8377 . ? 
N3 C3 1.44(4) . ? 
N3 H3A 0.8900 . ? 
N3 H3B 0.8900 . ? 
N3 H3C 0.8900 . ? 
O2W H2W 0.85(5) . ? 
C1 C2 1.533(14) . ? 
C4 C3 1.58(4) . ? 
C11 C12 1.49(3) . ? 
C14 C13 1.563(14) . ? 
C12 C13 1.54(5) . ? 
C12 H12A 0.9700 . ? 
C12 H12B 0.9700 . ? 
C13 H13 0.9800 . ? 
C3 C2 1.509(17) . ? 
C3 H3 0.9800 . ? 
C2 H2A 0.9700 . ? 
C2 H2B 0.9700 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O4 Zn1 O11 107.1(8) 7_666 . ? 
O4 Zn1 O1 98.1(8) 7_666 . ? 
O11 Zn1 O1 110.6(6) . . ? 
O4 Zn1 O14 101.0(7) 7_666 7_656 ? 
O11 Zn1 O14 116.3(4) . 7_656 ? 
O1 Zn1 O14 120.5(7) . 7_656 ? 
C4 O4 Zn1 121.0(11) . 7_666 ? 
C1 O1 Zn1 135.9(9) . . ? 
C14 O14 Zn1 108.1(13) . 7_656 ? 
C11 O11 Zn1 127(2) . . ? 
C13 N13 H13A 109.5 . . ? 
C13 N13 H13B 109.5 . . ? 
H13A N13 H13B 109.5 . . ? 
C13 N13 H13C 109.5 . . ? 
H13A N13 H13C 109.5 . . ? 
H13B N13 H13C 109.5 . . ? 
H1WA O1W H1WB 104.4 . . ? 
C3 N3 H3A 109.5 . . ? 
C3 N3 H3B 109.5 . . ? 
H3A N3 H3B 109.5 . . ? 
C3 N3 H3C 109.5 . . ? 
H3A N3 H3C 109.5 . . ? 
H3B N3 H3C 109.5 . . ? 
O2 C1 O1 124.1(11) . . ? 
O2 C1 C2 117(2) . . ? 
O1 C1 C2 118.6(15) . . ? 
O4 C4 O3 133(2) . . ? 
O4 C4 C3 116.6(16) . . ? 
O3 C4 C3 110(3) . . ? 
O12 C11 O11 126(2) . . ? 
O12 C11 C12 119(3) . . ? 
O11 C11 C12 115(3) . . ? 
O14 C14 O13 124.4(13) . . ? 
O14 C14 C13 117(2) . . ? 
O13 C14 C13 118(3) . . ? 
C11 C12 C13 113.8(19) . . ? 
C11 C12 H12A 108.8 . . ? 
C13 C12 H12A 108.8 . . ? 
C11 C12 H12B 108.8 . . ? 
C13 C12 H12B 108.8 . . ? 
H12A C12 H12B 107.7 . . ? 
N13 C13 C12 114.4(13) . . ? 
N13 C13 C14 108.6(18) . . ? 
C12 C13 C14 112(3) . . ? 
N13 C13 H13 107.2 . . ? 
C12 C13 H13 107.2 . . ? 
C14 C13 H13 107.2 . . ? 
N3 C3 C2 110.8(19) . . ? 
N3 C3 C4 109.5(16) . . ? 
C2 C3 C4 112(2) . . ? 
N3 C3 H3 108.2 . . ? 
C2 C3 H3 108.2 . . ? 
C4 C3 H3 108.2 . . ? 
C3 C2 C1 114.6(8) . . ? 
C3 C2 H2A 108.6 . . ? 
C1 C2 H2A 108.6 . . ? 
C3 C2 H2B 108.6 . . ? 
C1 C2 H2B 108.6 . . ? 
H2A C2 H2B 107.6 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C1 C2 C3 N3 73(3) . . . . ? 
C1 C2 C3 C4 -50(3) . . . . ? 
N3 C3 C4 O3 32.7(15) . . . . ? 
O2 C1 C2 C3 -31(3) . . . . ? 
C11 C12 C13 N13 -68(2) . . . . ? 
C11 C12 C13 C14 56(2) . . . . ? 
N13 C13 C14 O13 -11(2) . . . . ? 
O12 C11 C12 C13 -155(2) . . . . ? 
Zn1 O1 C1 C2 -18(3) . . . . ? 
Zn1 O11 C11 C12 -171.4(9) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.204 
_diffrn_reflns_theta_full              27.09 
_diffrn_measured_fraction_theta_full   0.204 
_refine_diff_density_max    0.194 
_refine_diff_density_min   -0.188 
_refine_diff_density_rms    0.048 

_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_1_15GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972151'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_1_15GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.191 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_1_15GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03883 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT415_zinc-aspartate_sesquihydrate_1_15GPa
;
PROBLEM: Short Inter D-H..H-X       H2W      ..H13      .       1.99 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_1_15GPa
;
PROBLEM: Short Inter D-H..H-D       H1WB     ..H3B      .       2.03 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     16.005(3)
_cell_length_b                     10.4707(8)
_cell_length_c                     14.2629(10)
_cell_angle_alpha                  90
_cell_angle_beta                   93.08(3)
_cell_angle_gamma                  90
_cell_volume                       2386.8(5)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      332
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         1150000 
_cell_measurement_theta_max        0.900
_cell_measurement_theta_min        0.690
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.115
_exptl_absorpt_correction_T_max    27.015
_exptl_absorpt_correction_T_min    3.74
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 1.15(2) GPa
 (1150000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.985
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0695
_diffrn_reflns_av_unetI/netI       0.0355
_diffrn_reflns_Laue_measured_fraction_full  0.191
_diffrn_reflns_Laue_measured_fraction_max  0.166
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         13
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              4732
_diffrn_reflns_point_group_measured_fraction_full  0.191
_diffrn_reflns_point_group_measured_fraction_max  0.166
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.015
_diffrn_reflns_theta_min           3.740
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.191
_diffrn_measured_fraction_theta_max  0.166
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_source                     'sealed x-ray tube'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  332
_reflns_number_total               436
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max           0.163
_refine_diff_density_min           -0.140
_refine_diff_density_rms           0.036
_refine_ls_goodness_of_fit_ref     1.080
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       196
_refine_ls_number_reflns           436
_refine_ls_number_restraints       134
_refine_ls_R_factor_all            0.0530
_refine_ls_R_factor_gt             0.0314
_refine_ls_restrained_S_all        0.956
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0394P)²+10.5512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0678
_refine_ls_wR_factor_ref           0.0772
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O11-C11
 1.25 with sigma of 0.05
 N3-C3
 1.4 with sigma of 0.05
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
 O1W-H1WA
 0.85 with sigma of 0.05
 O1W-H1WB
 0.85 with sigma of 0.05
 H1WA-H1WB
 1.34 with sigma of 0.05
 O2-H1WB
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N13) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq:
with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2W)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7342(4) 0.50578(9) 0.45238(7) 0.031(2) Uani 1 1 d . U . . .
 O4 O 0.681(3) 0.8672(9) 0.5518(7) 0.043(4) Uani 1 1 d . U . . .
 O2 O 0.5417(16) 0.7615(6) 0.3992(4) 0.034(5) Uani 1 1 d D U . . .
 O1 O 0.641(3) 0.6084(7) 0.4066(5) 0.036(3) Uani 1 1 d . U . . .
 O14 O 0.752(2) 0.0453(8) 0.4140(5) 0.050(3) Uani 1 1 d . U . . .
 O11 O 0.755(2) 0.3781(7) 0.3600(5) 0.051(3) Uani 1 1 d D U . . .
 O13 O 0.869(2) 0.1410(7) 0.4583(5) 0.044(5) Uani 1 1 d . U . . .
 O12 O 0.628(3) 0.3387(12) 0.2978(9) 0.055(6) Uani 1 1 d D U . . .
 O3 O 0.570(2) 1.0080(6) 0.5850(5) 0.044(5) Uani 1 1 d . U . . .
 N13 N 0.890(2) 0.2487(7) 0.2914(5) 0.035(5) Uani 1 1 d . U . . .
 H13A H 0.902048 0.260648 0.231680 0.042 Uiso 1 1 calc GR . . . .
 H13B H 0.935479 0.218320 0.323216 0.042 Uiso 1 1 calc GR . . . .
 H13C H 0.875645 0.322745 0.316286 0.042 Uiso 1 1 calc GR . . . .
 O1W O 0.600(2) 0.9877(11) 0.3208(6) 0.065(5) Uani 1 1 d D U . . .
 H1WA H 0.647946 0.986475 0.349458 0.097 Uiso 1 1 d DG . . . .
 H1WB H 0.571482 0.932492 0.349269 0.097 Uiso 1 1 d DG . . . .
 N3 N 0.463(3) 0.8190(11) 0.5690(7) 0.044(5) Uani 1 1 d D U . . .
 H3A H 0.458011 0.829716 0.507056 0.053 Uiso 1 1 calc GR . . . .
 H3B H 0.450015 0.891253 0.597471 0.053 Uiso 1 1 calc GR . . . .
 H3C H 0.429201 0.756877 0.585829 0.053 Uiso 1 1 calc GR . . . .
 O2W O 0.500000 0.5222(15) 0.250000 0.065(6) Uani 1 2 d DS TU P . .
 H2W H 0.557846 0.486394 0.253083 0.16(10) Uiso 1 1 d DG . . . .
 C1 C 0.583(3) 0.6792(10) 0.4439(7) 0.029(3) Uani 1 1 d . U . . .
 C4 C 0.607(5) 0.9000(12) 0.5722(9) 0.023(4) Uani 1 1 d . U . . .
 C11 C 0.697(4) 0.3184(17) 0.3063(12) 0.029(5) Uani 1 1 d D U . . .
 C14 C 0.814(3) 0.1144(10) 0.3988(8) 0.030(4) Uani 1 1 d . U . . .
 C12 C 0.739(4) 0.2082(10) 0.2522(8) 0.037(4) Uani 1 1 d . U . . .
 H12A H 0.699387 0.138367 0.245108 0.044 Uiso 1 1 calc R . . . .
 H12B H 0.749627 0.238699 0.189713 0.044 Uiso 1 1 calc R . . . .
 C13 C 0.820(3) 0.1557(9) 0.2963(7) 0.029(3) Uani 1 1 d . U . . .
 H13 H 0.835105 0.079955 0.260390 0.035 Uiso 1 1 calc R . . . .
 C3 C 0.548(3) 0.7853(11) 0.5958(9) 0.037(5) Uani 1 1 d D U . . .
 H3 H 0.552212 0.771523 0.663808 0.045 Uiso 1 1 calc R . . . .
 C2 C 0.573(2) 0.6632(8) 0.5485(6) 0.029(3) Uani 1 1 d . U . . .
 H2A H 0.530070 0.599040 0.557809 0.035 Uiso 1 1 calc R . . . .
 H2B H 0.624761 0.632569 0.578007 0.035 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.90(4) 7_666 ?
 Zn1 O1 1.92(4) . ?
 Zn1 O14 1.981(8) 7_656 ?
 Zn1 O11 1.918(9) . ?
 O4 C4 1.28(9) . ?
 O2 C1 1.24(3) . ?
 O1 C1 1.32(5) . ?
 O14 C14 1.26(5) . ?
 O11 C11 1.33(4) . ?
 O13 C14 1.23(5) . ?
 O12 C11 1.13(9) . ?
 O3 C4 1.29(4) . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.49(4) . ?
 O1W H1WA 0.8521 . ?
 O1W H1WB 0.8511 . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.43(5) . ?
 O2W H2W 0.9976 . ?
 C1 C2 1.518(16) . ?
 C4 C3 1.58(6) . ?
 C11 C12 1.56(4) . ?
 C14 C13 1.534(15) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.52(6) . ?
 C13 H13 0.9800 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.51(2) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9600 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 98.0(14) 7_666 . ?
 O4 Zn1 O14 100.0(9) 7_666 7_656 ?
 O4 Zn1 O11 108.5(11) 7_666 . ?
 O1 Zn1 O14 121.7(9) . 7_656 ?
 O11 Zn1 O1 108.4(8) . . ?
 O11 Zn1 O14 117.2(4) . 7_656 ?
 C4 O4 Zn1 119.2(14) . 7_666 ?
 C1 O1 Zn1 136.4(11) . . ?
 C14 O14 Zn1 105.6(17) . 7_656 ?
 C11 O11 Zn1 126(2) . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 109.5 . . ?
 H1WA O1W H1WB 104.6 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 109.5 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 109.5 . . ?
 O2 C1 O1 123.2(14) . . ?
 O2 C1 C2 120(3) . . ?
 O1 C1 C2 117(2) . . ?
 O4 C4 O3 135(4) . . ?
 O4 C4 C3 115(2) . . ?
 O3 C4 C3 111(5) . . ?
 O11 C11 C12 109(4) . . ?
 O12 C11 O11 129(2) . . ?
 O12 C11 C12 122(3) . . ?
 O14 C14 C13 115(3) . . ?
 O13 C14 O14 124.2(15) . . ?
 O13 C14 C13 121(4) . . ?
 C11 C12 H12A 108.2 . . ?
 C11 C12 H12B 108.2 . . ?
 H12A C12 H12B 107.3 . . ?
 C13 C12 C11 116(2) . . ?
 C13 C12 H12A 108.2 . . ?
 C13 C12 H12B 108.2 . . ?
 N13 C13 C14 109(2) . . ?
 N13 C13 C12 112.0(16) . . ?
 N13 C13 H13 107.5 . . ?
 C14 C13 H13 107.5 . . ?
 C12 C13 C14 113(3) . . ?
 C12 C13 H13 107.5 . . ?
 N3 C3 C4 109(3) . . ?
 N3 C3 H3 108.2 . . ?
 N3 C3 C2 111(2) . . ?
 C4 C3 H3 108.2 . . ?
 C2 C3 C4 112(3) . . ?
 C2 C3 H3 108.2 . . ?
 C1 C2 H2A 109.0 . . ?
 C1 C2 H2B 109.0 . . ?
 C3 C2 C1 113.0(10) . . ?
 C3 C2 H2A 109.0 . . ?
 C3 C2 H2B 109.0 . . ?
 H2A C2 H2B 107.8 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -14(5) . . . . ?
 Zn1 O11 C11 C12 -171.5(10) . . . . ?
 O2 C1 C2 C3 -29(5) . . . . ?
 O12 C11 C12 C13 -156(3) . . . . ?
 N13 C13 C14 O13 -12(3) . . . . ?
 N3 C3 C4 O3 35(2) . . . . ?
 C1 C2 C3 N3 71(4) . . . . ?
 C1 C2 C3 C4 -51(4) . . . . ?
 C11 C12 C13 N13 -70(3) . . . . ?
 C11 C12 C13 C14 53(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_1_44GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972152'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_1_44GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.193 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_1_44GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03917 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT415_zinc-aspartate_sesquihydrate_1_44GPa
;
PROBLEM: Short Inter D-H..H-X       H2W      ..H13      .       1.96 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_1_44GPa
;
PROBLEM: Short Inter D-H..H-D       H1WB     ..H3B      .       1.99 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     15.950(3)
_cell_length_b                     10.4707(8)
_cell_length_c                     14.2629(10)
_cell_angle_alpha                  90
_cell_angle_beta                   93.08(3)
_cell_angle_gamma                  90
_cell_volume                       2378.6(5)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      333
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         1440000 
_cell_measurement_theta_max        27.015
_cell_measurement_theta_min        3.742
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.122
_exptl_absorpt_correction_T_max    0.899
_exptl_absorpt_correction_T_min    0.689
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 1.44(2) GPa
 (1440000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.992
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0632
_diffrn_reflns_av_unetI/netI       0.0355
_diffrn_reflns_Laue_measured_fraction_full  0.193
_diffrn_reflns_Laue_measured_fraction_max  0.167
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         13
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              4750
_diffrn_reflns_point_group_measured_fraction_full  0.193
_diffrn_reflns_point_group_measured_fraction_max  0.167
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.015
_diffrn_reflns_theta_min           3.742
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.193
_diffrn_measured_fraction_theta_max  0.167
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  333
_reflns_number_total               437
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.163
_refine_diff_density_min           -0.145
_refine_diff_density_rms           0.036
_refine_ls_goodness_of_fit_ref     1.084
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       196
_refine_ls_number_reflns           437
_refine_ls_number_restraints       110
_refine_ls_R_factor_all            0.0521
_refine_ls_R_factor_gt             0.0306
_refine_ls_restrained_S_all        0.981
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0398P)²+8.8556P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0667
_refine_ls_wR_factor_ref           0.0760
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2W-H2W
 1 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(N13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(O2W) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1Wa,H1Wb)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C2(H2a,H2b)
4.d Idealised Me refined as rotating group:
 N13(H13a,H13b,H13c), N3(H3a,H3b,H3c)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7344(3) 0.50578(9) 0.45237(7) 0.048(7) Uani 1 1 d . . . . .
 O4 O 0.680(3) 0.8673(10) 0.5517(7) 0.043(4) Uani 1 1 d . U . . .
 O2 O 0.5414(16) 0.7614(6) 0.3991(4) 0.035(5) Uani 1 1 d . U . . .
 O1 O 0.642(3) 0.6084(7) 0.4066(5) 0.036(3) Uani 1 1 d . U . . .
 O14 O 0.751(2) 0.0454(8) 0.4140(5) 0.051(3) Uani 1 1 d . U . . .
 O11 O 0.756(2) 0.3780(6) 0.3602(5) 0.053(3) Uani 1 1 d . U . . .
 O13 O 0.870(3) 0.1410(7) 0.4583(5) 0.043(5) Uani 1 1 d . U . . .
 O12 O 0.628(3) 0.3390(14) 0.2981(9) 0.058(7) Uani 1 1 d D U . . .
 O3 O 0.571(2) 1.0081(6) 0.5856(5) 0.044(5) Uani 1 1 d . U . . .
 N13 N 0.890(2) 0.2491(8) 0.2913(5) 0.036(5) Uani 1 1 d . U . . .
 H13A H 0.902011 0.261259 0.231597 0.043 Uiso 1 1 calc GR . . . .
 H13B H 0.935850 0.219295 0.323109 0.043 Uiso 1 1 calc GR . . . .
 H13C H 0.875233 0.322969 0.316229 0.043 Uiso 1 1 calc GR . . . .
 O1W O 0.599(2) 0.9876(13) 0.3209(8) 0.066(5) Uani 1 1 d . U . . .
 H1WA H 0.647766 0.987709 0.345264 0.090 Uiso 1 1 d G . . . .
 H1WB H 0.573520 0.935027 0.352538 0.090 Uiso 1 1 d G . . . .
 N3 N 0.462(3) 0.8194(12) 0.5692(7) 0.044(5) Uani 1 1 d . U . . .
 H3A H 0.455852 0.832236 0.507521 0.053 Uiso 1 1 calc GR . . . .
 H3B H 0.447851 0.890281 0.599169 0.053 Uiso 1 1 calc GR . . . .
 H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc R . . . . 
 O2W O 0.500000 0.5222(15) 0.250000 0.066(7) Uani 1 2 d DS TU P . .
 H2W H 0.558(6) 0.487(11) 0.250(14) 0.09(9) Uiso 1 1 d D . . . .
 C1 C 0.584(4) 0.6789(10) 0.4439(7) 0.05(7) Uani 1 1 d . . . . .
 C4 C 0.607(5) 0.9002(12) 0.5722(9) 0.023(4) Uani 1 1 d . U . . .
 C11 C 0.695(5) 0.3182(18) 0.3057(12) 0.028(5) Uani 1 1 d . U . . .
 C14 C 0.816(4) 0.1146(10) 0.3990(8) 0.031(4) Uani 1 1 d . U . . .
 C12 C 0.738(4) 0.2086(11) 0.2521(8) 0.037(4) Uani 1 1 d . U . . .
 H12A H 0.698754 0.138268 0.245150 0.045 Uiso 1 1 calc R . . . .
 H12B H 0.748473 0.239142 0.189566 0.045 Uiso 1 1 calc R . . . .
 C13 C 0.821(3) 0.1561(9) 0.2963(7) 0.03(4) Uani 1 1 d . . . . .
 H13 H 0.836265 0.080663 0.260080 0.039 Uiso 1 1 calc R . . . .
 C3 C 0.550(4) 0.7854(11) 0.5956(9) 0.038(5) Uani 1 1 d . U . . .
 H3 H 0.554825 0.771707 0.663670 0.046 Uiso 1 1 calc R . . . .
 C2 C 0.573(2) 0.6631(7) 0.5486(5) 0.029(3) Uani 1 1 d . U . . .
 H2A H 0.529403 0.600307 0.557710 0.035 Uiso 1 1 calc R . . . .
 H2B H 0.624838 0.630823 0.578302 0.035 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.91(4) 7_666 ?
 Zn1 O1 1.91(4) . ?
 Zn1 O14 1.981(8) 7_656 ?
 Zn1 O11 1.919(9) . ?
 O4 C4 1.26(9) . ?
 O2 C1 1.25(3) . ?
 O1 C1 1.31(5) . ?
 O14 C14 1.29(5) . ?
 O11 C11 1.36(5) . ?
 O13 C14 1.21(5) . ?
 O12 C11 1.09(11) . ?
 O3 C4 1.29(4) . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.48(4) . ?
 O1W H1WA 0.8323 . ?
 O1W H1WB 0.8325 . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8200 . ?
 N3 C3 1.48(8) . ?
 O2W H2W 0.99(6) . ?
 C1 C2 1.523(16) . ?
 C4 C3 1.55(6) . ?
 C11 C12 1.56(5) . ?
 C14 C13 1.535(15) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.54(6) . ?
 C13 H13 0.9800 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.50(2) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 98.1(14) 7_666 . ?
 O4 Zn1 O14 99.8(9) 7_666 7_656 ?
 O4 Zn1 O11 108.1(11) 7_666 . ?
 O1 Zn1 O14 121.9(9) . 7_656 ?
 O1 Zn1 O11 108.7(8) . . ?
 O11 Zn1 O14 117.0(4) . 7_656 ?
 C4 O4 Zn1 119.1(16) . 7_666 ?
 C1 O1 Zn1 136.3(11) . . ?
 C14 O14 Zn1 105.0(16) . 7_656 ?
 C11 O11 Zn1 124(3) . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 109.5 . . ?
 H1WA O1W H1WB 104.4 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 103.0 . . ?
 H3B N3 H3C 119.0 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 106.0 . . ?
 O2 C1 O1 123.6(14) . . ?
 O2 C1 C2 119(3) . . ?
 O1 C1 C2 117(2) . . ?
 O4 C4 O3 135(5) . . ?
 O4 C4 C3 113(2) . . ?
 O3 C4 C3 112(5) . . ?
 O11 C11 C12 108(5) . . ?
 O12 C11 O11 129(3) . . ?
 O12 C11 C12 124(4) . . ?
 O14 C14 C13 114(3) . . ?
 O13 C14 O14 124.2(16) . . ?
 O13 C14 C13 122(4) . . ?
 C11 C12 H12A 108.0 . . ?
 C11 C12 H12B 108.0 . . ?
 H12A C12 H12B 107.3 . . ?
 C13 C12 C11 117(3) . . ?
 C13 C12 H12A 108.0 . . ?
 C13 C12 H12B 108.0 . . ?
 N13 C13 C14 108(3) . . ?
 N13 C13 C12 112.0(16) . . ?
 N13 C13 H13 107.6 . . ?
 C14 C13 C12 114(3) . . ?
 C14 C13 H13 107.6 . . ?
 C12 C13 H13 107.6 . . ?
 N3 C3 C4 109(3) . . ?
 N3 C3 H3 108.1 . . ?
 N3 C3 C2 110(3) . . ?
 C4 C3 H3 108.1 . . ?
 C2 C3 C4 114(4) . . ?
 C2 C3 H3 108.1 . . ?
 C1 C2 H2A 109.0 . . ?
 C1 C2 H2B 109.0 . . ?
 C3 C2 C1 112.9(10) . . ?
 C3 C2 H2A 109.0 . . ?
 C3 C2 H2B 109.0 . . ?
 H2A C2 H2B 107.8 . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_1_62GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972153'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_1_62GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.166 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_1_62GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0305 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_1_62GPa
;
PROBLEM: Short Inter D-H..H-D       H1WB     ..H3B      .       1.95 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;  
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H30 N4 O19 Zn2' 
_chemical_formula_weight          713.18 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    15.916(5) 
_cell_length_b                    10.4593(12) 
_cell_length_c                    14.2566(15) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.09(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      2369.9(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_pressure        1620000 
_cell_measurement_reflns_used     316 
_cell_measurement_theta_min       3.745 
_cell_measurement_theta_max       27.030 
 
_exptl_crystal_description        plate 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.999 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1464 
_exptl_absorpt_coefficient_mu     2.130 
_exptl_absorpt_correction_T_min   0.688 
_exptl_absorpt_correction_T_max   0.969
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 1.62(2) GPa
 (1620000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C3-N3
 1.37 with sigma of 0.01
 O12-C11
 1.24 with sigma of 0.01
 C4-O4
 1.34 with sigma of 0.01
 C1-C3
 2.52 with sigma of 0.01
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N13) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(O2W) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ? 
_diffrn_ambient_temperature       296(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_reflns_number             4699 
_diffrn_reflns_av_R_equivalents   0.1007 
_diffrn_reflns_av_sigmaI/netI     0.0496 
_diffrn_reflns_limit_h_min        -3 
_diffrn_reflns_limit_h_max        3 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.75 
_diffrn_reflns_theta_max          27.03 
_reflns_number_total              433 
_reflns_number_gt                 316 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0636P)²+0.3086P] where P=(Fo²+2Fc²)/3' 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_number_reflns          433 
_refine_ls_number_parameters      196 
_refine_ls_number_restraints      138 
_refine_ls_R_factor_all           0.0655 
_refine_ls_R_factor_gt            0.0393 
_refine_ls_wR_factor_ref          0.0991 
_refine_ls_wR_factor_gt           0.0863 
_refine_ls_goodness_of_fit_ref    1.141 
_refine_ls_restrained_S_all       0.969 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Zn1 Zn 0.7346(4) 0.50574(9) 0.45275(7) 0.050(8) Uani 1 1 d . . . 
O4 O 0.685(3) 0.8658(10) 0.5525(8) 0.047(6) Uani 1 1 d DU . . 
O2 O 0.5414(15) 0.7599(6) 0.3991(4) 0.040(9) Uani 1 1 d U . . 
O1 O 0.641(3) 0.6082(7) 0.4068(5) 0.042(5) Uani 1 1 d U . . 
O14 O 0.749(2) 0.0450(9) 0.4137(5) 0.052(5) Uani 1 1 d U . . 
O11 O 0.7560(19) 0.3781(7) 0.3604(5) 0.059(5) Uani 1 1 d U . . 
O13 O 0.867(2) 0.1406(7) 0.4584(5) 0.043(9) Uani 1 1 d U . . 
O12 O 0.625(2) 0.3381(14) 0.2979(11) 0.056(10) Uani 1 1 d DU . . 
O3 O 0.568(2) 1.0089(6) 0.5857(6) 0.048(9) Uani 1 1 d U . . 
N13 N 0.890(3) 0.2486(7) 0.2908(5) 0.037(4) Uani 1 1 d U . . 
H13A H 0.8944 0.2735 0.2315 0.045 Uiso 1 1 calc R . . 
H13B H 0.9381 0.2110 0.3110 0.045 Uiso 1 1 calc R . . 
H13C H 0.8809 0.3163 0.3265 0.045 Uiso 1 1 calc R . . 
O1W O 0.597(3) 0.9887(11) 0.3191(7) 0.071(5) Uani 1 1 d GU . . 
H1WB H 0.5595 0.9411 0.3406 0.107 Uiso 1 1 d G . . 
H1WA H 0.6410 0.9732 0.3541 0.107 Uiso 1 1 d G . . 
N3 N 0.463(2) 0.8212(11) 0.5690(7) 0.042(5) Uani 1 1 d DU . . 
H3A H 0.4604 0.8383 0.5078 0.051 Uiso 1 1 calc R . . 
H3B H 0.4502 0.8910 0.6008 0.051 Uiso 1 1 calc R . . 
H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc R . . 
O2W O 0.5000 0.5233(17) 0.2500 0.067(6) Uani 1 2 d SDU . . 
C1 C 0.580(3) 0.6799(11) 0.4446(7) 0.034(5) Uani 1 1 d DU . . 
C4 C 0.607(3) 0.9015(12) 0.5701(10) 0.028(6) Uani 1 1 d DU . . 
C11 C 0.702(2) 0.321(2) 0.3052(16) 0.033(7) Uani 1 1 d DU . . 
C14 C 0.810(4) 0.1150(12) 0.3972(8) 0.034(5) Uani 1 1 d U . . 
C13 C 0.819(3) 0.1562(9) 0.2963(7) 0.033(5) Uani 1 1 d U . . 
H13 H 0.8337 0.0799 0.2606 0.040 Uiso 1 1 calc R . . 
C3 C 0.543(2) 0.7830(11) 0.5962(9) 0.040(6) Uani 1 1 d DU . . 
H3 H 0.5467 0.7702 0.6644 0.048 Uiso 1 1 calc R . . 
C12 C 0.740(3) 0.2090(10) 0.2512(8) 0.038(5) Uani 1 1 d U . . 
H12A H 0.6990 0.1409 0.2448 0.046 Uiso 1 1 calc R . . 
H12B H 0.7517 0.2381 0.1886 0.046 Uiso 1 1 calc R . . 
C2 C 0.573(2) 0.6610(7) 0.5488(5) 0.032(5) Uani 1 1 d U . . 
H2A H 0.6268 0.6356 0.5773 0.039 Uiso 1 1 calc R . . 
H2B H 0.5329 0.5928 0.5589 0.039 Uiso 1 1 calc R . . 
H2W H 0.549(6) 0.486(10) 0.251(13) 0.10(8) Uiso 1 1 d D . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Zn1 O4 1.85(3) 7_666 ? 
Zn1 O11 1.919(9) . ? 
Zn1 O1 1.92(3) . ? 
Zn1 O14 1.980(8) 7_656 ? 
O4 C4 1.340(11) . ? 
O4 Zn1 1.85(3) 7_666 ? 
O2 C1 1.21(3) . ? 
O1 C1 1.35(4) . ? 
O14 C14 1.25(5) . ? 
O14 Zn1 1.980(8) 7_656 ? 
O11 C11 1.28(3) . ? 
O13 C14 1.25(5) . ? 
O12 C11 1.238(11) . ? 
O3 C4 1.31(3) . ? 
N13 C13 1.49(5) . ? 
N13 H13A 0.8900 . ? 
N13 H13B 0.8900 . ? 
N13 H13C 0.8900 . ? 
O1W H1WB 0.8500 . ? 
O1W H1WA 0.8502 . ? 
N3 C3 1.371(11) . ? 
N3 H3A 0.8900 . ? 
N3 H3B 0.8900 . ? 
N3 H3C 0.8500 . ? 
O2W H2W 0.87(5) . ? 
C1 C2 1.510(14) . ? 
C4 C3 1.66(4) . ? 
C11 C12 1.54(4) . ? 
C14 C13 1.516(16) . ? 
C13 C12 1.48(6) . ? 
C13 H13 0.9800 . ? 
C3 C2 1.529(19) . ? 
C3 H3 0.9800 . ? 
C12 H12A 0.9700 . ? 
C12 H12B 0.9700 . ? 
C2 H2A 0.9700 . ? 
C2 H2B 0.9700 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O4 Zn1 O11 109.2(10) 7_666 . ? 
O4 Zn1 O1 96.0(10) 7_666 . ? 
O11 Zn1 O1 108.5(8) . . ? 
O4 Zn1 O14 100.3(8) 7_666 7_656 ? 
O11 Zn1 O14 117.0(5) . 7_656 ? 
O1 Zn1 O14 122.4(9) . 7_656 ? 
C4 O4 Zn1 117.0(13) . 7_666 ? 
C1 O1 Zn1 136.7(11) . . ? 
C14 O14 Zn1 105.9(17) . 7_656 ? 
C11 O11 Zn1 128(2) . . ? 
C13 N13 H13A 109.5 . . ? 
C13 N13 H13B 109.5 . . ? 
H13A N13 H13B 109.5 . . ? 
C13 N13 H13C 109.5 . . ? 
H13A N13 H13C 109.5 . . ? 
H13B N13 H13C 109.5 . . ? 
H1WB O1W H1WA 104.5 . . ? 
C3 N3 H3A 109.5 . . ? 
C3 N3 H3B 109.5 . . ? 
H3A N3 H3B 109.5 . . ? 
C3 N3 H3C 103.0 . . ? 
H3A N3 H3C 107.0 . . ? 
H3B N3 H3C 118.0 . . ? 
O2 C1 O1 121.6(13) . . ? 
O2 C1 C2 123(2) . . ? 
O1 C1 C2 115(2) . . ? 
O3 C4 O4 136(2) . . ? 
O3 C4 C3 108(3) . . ? 
O4 C4 C3 115.0(19) . . ? 
O12 C11 O11 128(3) . . ? 
O12 C11 C12 119(3) . . ? 
O11 C11 C12 113(3) . . ? 
O13 C14 O14 122.3(14) . . ? 
O13 C14 C13 120(4) . . ? 
O14 C14 C13 117(3) . . ? 
C12 C13 N13 111.2(16) . . ? 
C12 C13 C14 113(3) . . ? 
N13 C13 C14 110(3) . . ? 
C12 C13 H13 107.3 . . ? 
N13 C13 H13 107.3 . . ? 
C14 C13 H13 107.3 . . ? 
N3 C3 C2 114.8(19) . . ? 
N3 C3 C4 106.8(18) . . ? 
C2 C3 C4 109(2) . . ? 
N3 C3 H3 108.8 . . ? 
C2 C3 H3 108.8 . . ? 
C4 C3 H3 108.8 . . ? 
C13 C12 C11 114.4(18) . . ? 
C13 C12 H12A 108.7 . . ? 
C11 C12 H12A 108.7 . . ? 
C13 C12 H12B 108.7 . . ? 
C11 C12 H12B 108.7 . . ? 
H12A C12 H12B 107.6 . . ? 
C1 C2 C3 111.7(10) . . ? 
C1 C2 H2A 109.3 . . ? 
C3 C2 H2A 109.3 . . ? 
C1 C2 H2B 109.3 . . ? 
C3 C2 H2B 109.3 . . ? 
H2A C2 H2B 107.9 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C1 C2 C3 N3 66(3) . . . . ? 
C1 C2 C3 C4 -54(4) . . . . ? 
N3 C3 C4 O3 36.8(14) . . . . ? 
O2 C1 C2 C3 -25(5) . . . . ? 
C11 C12 C13 N13 -70(2) . . . . ? 
C11 C12 C13 C14 55(3) . . . . ? 
N13 C13 C14 O13 -12(3) . . . . ? 
O12 C11 C12 C13 -152(3) . . . . ? 
Zn1 O1 C1 C2 -13(5) . . . . ? 
Zn1 O11 C11 C12 -170.9(9) . . . . ? 
Zn1 O4 C4 C3 167.6(10) . 7_666 7_666 7_666 ? 
Zn1 O14 C14 C13 -173.5(19) . 7_656 7_656 7_656 ? 
 
_diffrn_measured_fraction_theta_max    0.166 
_diffrn_reflns_theta_full              27.03 
_diffrn_measured_fraction_theta_full   0.166 
_refine_diff_density_max    0.147 
_refine_diff_density_min   -0.155 
_refine_diff_density_rms    0.041 

_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_1_82GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972154'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_1_82GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.193 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_1_82GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03133 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_1_82GPa
;
PROBLEM: Short Inter D-H..H-D       H1WB     ..H3B      .       1.86 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                    15.819(4) 
_cell_length_b                    10.4316(10) 
_cell_length_c                    14.2229(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.03(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2343.8(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_pressure        1820000 
_cell_measurement_reflns_used     332 
_cell_measurement_theta_max       27.006
_cell_measurement_theta_min       3.755
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.154
_exptl_absorpt_correction_T_max    0.898
_exptl_absorpt_correction_T_min    0.685
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 1.82(2) GPa
 (1820000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.021
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'mot measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0676
_diffrn_reflns_av_unetI/netI       0.0372
_diffrn_reflns_Laue_measured_fraction_full  0.193
_diffrn_reflns_Laue_measured_fraction_max  0.168
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         13
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              4678
_diffrn_reflns_point_group_measured_fraction_full  0.193
_diffrn_reflns_point_group_measured_fraction_max  0.168
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.006
_diffrn_reflns_theta_min           3.755
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.193
_diffrn_measured_fraction_theta_max  0.168
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  332
_reflns_number_total               429
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.135
_refine_diff_density_min           -0.176
_refine_diff_density_rms           0.035
_refine_ls_goodness_of_fit_ref     1.114
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       196
_refine_ls_number_reflns           429
_refine_ls_number_restraints       130
_refine_ls_R_factor_all            0.0577
_refine_ls_R_factor_gt             0.0324
_refine_ls_restrained_S_all        0.980
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0472P)²+6.8691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0679
_refine_ls_wR_factor_ref           0.0811
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C3-C4
 1.5 with sigma of 0.05
 C3-N3
 1.49 with sigma of 0.05
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?

loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
Zn1 Zn 0.7344(3) 0.50599(9) 0.45303(6) 0.0301(19) Uani 1 1 d U . . . .
O4 O 0.683(3) 0.8665(8) 0.5511(6) 0.037(3) Uani 1 1 d U . . . . 
O2 O 0.5420(15) 0.7604(5) 0.3999(4) 0.034(4) Uani 1 1 d U . . . . 
O1 O 0.640(2) 0.6081(6) 0.4072(4) 0.036(3) Uani 1 1 d U . . . . 
O14 O 0.7485(18) 0.0441(7) 0.4128(5) 0.048(3) Uani 1 1 d U . . . . 
O11 O 0.7563(19) 0.3787(6) 0.3593(4) 0.050(3) Uani 1 1 d U . . . . 
O13 O 0.870(2) 0.1402(6) 0.4581(5) 0.042(4) Uani 1 1 d U . . . . 
O12 O 0.629(3) 0.3409(12) 0.2980(8) 0.053(6) Uani 1 1 d DU . . . . 
O3 O 0.5727(19) 1.0083(5) 0.5852(5) 0.043(4) Uani 1 1 d U . . . . 
N13 N 0.892(2) 0.2472(7) 0.2906(5) 0.032(4) Uani 1 1 d U . . . . 
H13A H 0.9063 0.2545 0.2312 0.039 Uiso 1 1 calc R . . . . 
H13B H 0.9359 0.2187 0.3261 0.039 Uiso 1 1 calc R . . . . 
H13C H 0.8761 0.3234 0.3117 0.039 Uiso 1 1 calc R . . . . 
O1W O 0.593(2) 0.9883(10) 0.3171(9) 0.066(5) Uani 1 1 d GU . . . .  
H1WA H 0.6523 0.9747 0.3405 0.099 Uiso 1 1 d G . . . . 
H1WB H 0.5771 0.9419 0.3659 0.099 Uiso 1 1 d G . . . . 
N3 N 0.459(2) 0.8194(10) 0.5680(6) 0.044(5) Uani 1 1 d DU . . . . 
H3A H 0.4546 0.8342 0.5063 0.053 Uiso 1 1 calc R . . . . 
H3B H 0.4444 0.8897 0.5987 0.053 Uiso 1 1 calc R . . . . 
H3C H 0.4245 0.7554 0.5819 0.053 Uiso 1 1 calc R . . . . 
O2W O 0.5000 0.5238(12) 0.2500 0.054(5) Uani 1 2 d SDU . . . . 
C1 C 0.580(3) 0.6788(9) 0.4444(6) 0.031(3) Uani 1 1 d U . . . . 
C4 C 0.605(4) 0.8995(11) 0.5730(8) 0.023(4) Uani 1 1 d DU . . . . 
C11 C 0.698(4) 0.3174(15) 0.3046(10) 0.024(4) Uani 1 1 d U . . . . 
C14 C 0.810(3) 0.1132(9) 0.3981(7) 0.027(3) Uani 1 1 d U . . . . 
C13 C 0.820(3) 0.1544(8) 0.2955(6) 0.029(3) Uani 1 1 d U . . . . 
H13 H 0.8340 0.0779 0.2596 0.034 Uiso 1 1 calc R . . . . 
C3 C 0.547(2) 0.7844(10) 0.5962(8) 0.030(4) Uani 1 1 d DU . . . .  
H3 H 0.5506 0.7709 0.6644 0.036 Uiso 1 1 calc R . . . . 
C12 C 0.740(3) 0.2093(8) 0.2512(6) 0.029(3) Uani 1 1 d U . . . .  
H12A H 0.6988 0.1403 0.2426 0.034 Uiso 1 1 calc R . . . . 
H12B H 0.7515 0.2408 0.1891 0.034 Uiso 1 1 calc R . . . . 
C2 C 0.570(2) 0.6619(7) 0.5493(5) 0.028(3) Uani 1 1 d U . . . .  
H2A H 0.5266 0.5983 0.5591 0.034 Uiso 1 1 calc R . . . . 
H2B H 0.6228 0.6302 0.5782 0.034 Uiso 1 1 calc R . . . . 
H2W H 0.547(6) 0.483(10) 0.257(17) 0.16(8) Uiso 1 1 d D . . . . 
 

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.87(4) 7_666 ?
 Zn1 O1 1.92(4) . ?
 Zn1 O14 1.983(8) 7_656 ?
 Zn1 O11 1.926(9) . ?
 Zn1 C14 2.584(19) 7_656 ?
 O4 C4 1.33(8) . ?
 O2 C1 1.20(3) . ?
 O1 C1 1.34(5) . ?
 O14 C14 1.24(5) . ?
 O11 C11 1.34(5) . ?
 O13 C14 1.27(5) . ?
 O12 C11 1.12(10) . ?
 O3 C4 1.26(3) . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.50(5) . ?
 O1W H1WA 0.9959 . ?
 O1W H1WB 0.8901 . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.47(5) . ?
 O2W H2W 0.86(6) . ?
 O2W H2W 0.86(6) 2_655 ?
 C1 C2 1.518(16) . ?
 C4 C3 1.56(4) . ?
 C11 C12 1.53(5) . ?
 C14 C13 1.536(16) . ?
 C13 H13 0.9800 . ?
 C13 C12 1.50(6) . ?
 C3 H3 0.9800 . ?
 C3 C2 1.497(19) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 97.4(14) 7_666 . ?
 O4 Zn1 O14 99.0(9) 7_666 7_656 ?
 O4 Zn1 O11 108.4(11) 7_666 . ?
 O4 Zn1 C14 126.1(9) 7_666 7_656 ?
 O1 Zn1 O14 122.5(9) . 7_656 ?
 O1 Zn1 O11 108.2(8) . . ?
 O1 Zn1 C14 107.8(10) . 7_656 ?
 O14 Zn1 C14 27.6(13) 7_656 7_656 ?
 O11 Zn1 O14 117.7(5) . 7_656 ?
 O11 Zn1 C14 107.6(4) . 7_656 ?
 C4 O4 Zn1 118.8(12) . 7_666 ?
 C1 O1 Zn1 136.9(11) . . ?
 C14 O14 Zn1 104.3(17) . 7_656 ?
 C11 O11 Zn1 126(3) . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 109.5 . . ?
 H1WA O1W H1WB 87.5 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 109.5 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 109.5 . . ?
 H2W O2W H2W 120(10) . 2_655 ?
 O2 C1 O1 121.8(16) . . ?
 O2 C1 C2 122(3) . . ?
 O1 C1 C2 116(3) . . ?
 O4 C4 C3 114.5(19) . . ?
 O3 C4 O4 131(4) . . ?
 O3 C4 C3 115(4) . . ?
 O11 C11 C12 110(5) . . ?
 O12 C11 O11 126(2) . . ?
 O12 C11 C12 124(4) . . ?
 O14 C14 Zn1 48.1(8) . 7_656 ?
 O14 C14 O13 125.4(14) . . ?
 O14 C14 C13 116(3) . . ?
 O13 C14 Zn1 77.4(10) . 7_656 ?
 O13 C14 C13 118(4) . . ?
 C13 C14 Zn1 163(2) . 7_656 ?
 N13 C13 C14 110(3) . . ?
 N13 C13 H13 107.7 . . ?
 N13 C13 C12 111.3(17) . . ?
 C14 C13 H13 107.7 . . ?
 C12 C13 C14 112(3) . . ?
 C12 C13 H13 107.7 . . ?
 N3 C3 C4 108(2) . . ?
 N3 C3 H3 108.3 . . ?
 N3 C3 C2 110(2) . . ?
 C4 C3 H3 108.3 . . ?
 C2 C3 C4 114(3) . . ?
 C2 C3 H3 108.3 . . ?
 C11 C12 H12A 108.1 . . ?
 C11 C12 H12B 108.1 . . ?
 C13 C12 C11 117(3) . . ?
 C13 C12 H12A 108.1 . . ?
 C13 C12 H12B 108.1 . . ?
 H12A C12 H12B 107.3 . . ?
 C1 C2 H2A 109.2 . . ?
 C1 C2 H2B 109.2 . . ?
 C3 C2 C1 112.2(10) . . ?
 C3 C2 H2A 109.2 . . ?
 C3 C2 H2B 109.2 . . ?
 H2A C2 H2B 107.9 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -13(5) . . . . ?
 Zn1 O11 C11 C12 -170.9(11) . . . . ?
 O2 C1 C2 C3 -27(5) . . . . ?
 O12 C11 C12 C13 -154(3) . . . . ?
 N13 C13 C14 O13 -13(3) . . . . ?
 N3 C3 C4 O3 36(2) . . . . ?
 C1 C2 C3 N3 71(4) . . . . ?
 C1 C2 C3 C4 -50(4) . . . . ?
 C11 C12 C13 N13 -71(3) . . . . ?
 C11 C12 C13 C14 52(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_2_15GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972155'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_2_15GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.193 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_2_15GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02633 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_2_15GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H3B      .       2.07 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     15.782(4) 
_cell_length_b                     10.3838(9) 
_cell_length_c                     14.1615(13) 
_cell_angle_alpha                  90.00 
_cell_angle_beta                   92.99(3) 
_cell_angle_gamma                  90.00 
_cell_volume                       2317.5(6) 
_cell_formula_units_Z              4
_cell_measurement_reflns_used      316
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         2150000 
_cell_measurement_theta_max        26.652
_cell_measurement_theta_min        3.77
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.178
_exptl_absorpt_correction_T_max    0.917
_exptl_absorpt_correction_T_min    0.682
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 2.15(2) GPa
 (2150000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.044
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.04
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0688
_diffrn_reflns_av_unetI/netI       0.0399
_diffrn_reflns_Laue_measured_fraction_full  0.193
_diffrn_reflns_Laue_measured_fraction_max  0.176
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         13
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              4622
_diffrn_reflns_point_group_measured_fraction_full  0.193
_diffrn_reflns_point_group_measured_fraction_max  0.176
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.652
_diffrn_reflns_theta_min           3.770
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.193
_diffrn_measured_fraction_theta_max  0.176
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  316
_reflns_number_total               427
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max           0.166
_refine_diff_density_min           -0.158
_refine_diff_density_rms           0.042
_refine_ls_goodness_of_fit_ref     1.095
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       199
_refine_ls_number_reflns           427
_refine_ls_number_restraints       134
_refine_ls_R_factor_all            0.0603
_refine_ls_R_factor_gt             0.0343
_refine_ls_restrained_S_all        0.926
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+27.4439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0587
_refine_ls_wR_factor_ref           0.0698
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C3-C4
 1.5 with sigma of 0.05
 N3-C3
 1.5 with sigma of 0.05
 O12-C11
 1.3 with sigma of 0.05
 C4-O4
 1.4 with sigma of 0.01
 C3-C1
 2.52 with sigma of 0.01
 C1-C4
 2.96 with sigma of 0.01
 N13-C13
 1.45 with sigma of 0.01
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
 O1W-H1WA
 0.85 with sigma of 0.05
 O1W-H1WB
 0.85 with sigma of 0.05
 H1WA-H1WB
 1.34 with sigma of 0.05
 O2-H1WB
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O14) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.7355(4) 0.50599(11) 0.45344(7) 0.039(6) Uani 1 1 d . . . . .
O4 O 0.683(2) 0.8657(8) 0.5513(6) 0.040(3) Uani 1 1 d D U . . . 
O2 O 0.5414(17) 0.7599(6) 0.4006(4) 0.033(4) Uani 1 1 d D U . . . 
O1 O 0.642(3) 0.6066(7) 0.4073(5) 0.038(3) Uani 1 1 d . U . . . 
O14 O 0.745(2) 0.0442(8) 0.4122(5) 0.049(3) Uani 1 1 d . U . . .  
O11 O 0.757(2) 0.3785(7) 0.3585(5) 0.054(3) Uani 1 1 d . U . . . 
O13 O 0.868(2) 0.1383(7) 0.4579(5) 0.040(4) Uani 1 1 d . U . . . 
O12 O 0.623(2) 0.3410(11) 0.2964(8) 0.049(6) Uani 1 1 d D U . . . 
O3 O 0.571(2) 1.0081(6) 0.5866(5) 0.041(4) Uani 1 1 d . U . . .
N13 N 0.888(2) 0.2458(8) 0.2892(5) 0.034(4) Uani 1 1 d D U . . . 
H13A H 0.9008 0.2569 0.2292 0.040 Uiso 1 1 calc GR . . . . 
H13B H 0.9359 0.2261 0.3282 0.037 Uiso 1 1 calc GR . . . .
H13C H 0.8731 0.3209 0.3135 0.040 Uiso 1 1 calc GR . . . .
O1W O 0.592(2) 0.9889(11) 0.3148(7) 0.071(9) Uani 1 1 d D U . . . 
H1WA H 0.640(6) 0.982(17) 0.343(15) 0.106 Uiso 1 1 d DR . . . . 
H1WB H 0.560(8) 0.936(9) 0.341(12) 0.106 Uiso 1 1 d DR . . . .
N3 N 0.459(3) 0.8188(11) 0.5693(7) 0.040(5) Uani 1 1 d D U . . . 
H3A H 0.4569 0.8514 0.5111 0.048 Uiso 1 1 calc GR . . . . 
H3B H 0.4404 0.8772 0.6093 0.048 Uiso 1 1 calc GR . . . .
H3C H 0.4262 0.7490 0.5704 0.048 Uiso 1 1 calc GR . . . .
O2W O 0.5000 0.5236(15) 0.2500 0.060(6) Uani 1 2 d DS TU P . .
C1 C 0.580(3) 0.6767(9) 0.4444(6) 0.029(3) Uani 1 1 d D U . . . 
C4 C 0.600(2) 0.8992(11) 0.5728(8) 0.027(4) Uani 1 1 d D U . . . 
C11 C 0.703(3) 0.3181(16) 0.3042(11) 0.027(5) Uani 1 1 d D U . . . 
C14 C 0.815(3) 0.1144(12) 0.3972(8) 0.034(4) Uani 1 1 d . U . . .
C13 C 0.819(2) 0.1542(9) 0.2942(6) 0.026(3) Uani 1 1 d D U . . .
H13 H 0.8338 0.0777 0.2581 0.031 Uiso 1 1 calc R . . . .
C3 C 0.546(2) 0.7837(11) 0.5973(9) 0.036(4) Uani 1 1 d D U . . .
H3 H 0.5510 0.7706 0.6659 0.043 Uiso 1 1 calc R . . . .
C12 C 0.739(3) 0.2086(9) 0.2490(7) 0.030(3) Uani 1 1 d . U . . .
H12A H 0.6971 0.1405 0.2422 0.036 Uiso 1 1 calc R . . . .
H12B H 0.7505 0.2390 0.1862 0.036 Uiso 1 1 calc R . . . .
C2 C 0.568(2) 0.6613(8) 0.5498(5) 0.023(3) Uani 1 1 d . U . . . 
H2A H 0.5231 0.5993 0.5586 0.028 Uiso 1 1 calc R . . . .
H2B H 0.6198 0.6269 0.5799 0.028 Uiso 1 1 calc R . . . .
H2W H 0.546(8) 0.482(14) 0.241(12) 0.10(9) Uiso 1 1 d D . . . .
 

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.85(3) 7_666 ?
 Zn1 O1 1.90(4) . ?
 Zn1 O14 1.981(10) 7_656 ?
 Zn1 O11 1.930(11) . ?
 O4 C4 1.400(14) . ?
 O2 C1 1.20(3) . ?
 O1 C1 1.35(5) . ?
 O14 C14 1.34(6) . ?
 O11 C11 1.29(4) . ?
 O13 C14 1.20(5) . ?
 O12 C11 1.28(6) . ?
 O3 C4 1.24(2) . ?
 N13 C13 1.456(13) . ?
 N3 C3 1.46(5) . ?
 C1 C2 1.522(16) . ?
 C4 C3 1.52(4) . ?
 C11 C12 1.51(4) . ?
 C14 C13 1.521(17) . ?
 C13 C12 1.49(6) . ?
 C3 C2 1.49(2) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 96.9(11) 7_666 . ?
 O4 Zn1 O14 98.5(9) 7_666 7_656 ?
 O4 Zn1 O11 108.7(12) 7_666 . ?
 O1 Zn1 O14 123.8(11) . 7_656 ?
 O1 Zn1 O11 107.5(9) . . ?
 O11 Zn1 O14 117.7(6) . 7_656 ?
 C4 O4 Zn1 118.9(12) . 7_666 ?
 C1 O1 Zn1 136.9(11) . . ?
 C14 O14 Zn1 101.8(19) . 7_656 ?
 C11 O11 Zn1 128(3) . . ?
 O2 C1 O1 122.6(16) . . ?
 O2 C1 C2 120(3) . . ?
 O1 C1 C2 117(2) . . ?
 O4 C4 C3 113(2) . . ?
 O3 C4 O4 128(2) . . ?
 O3 C4 C3 118(3) . . ?
 O11 C11 C12 115(4) . . ?
 O12 C11 O11 126(3) . . ?
 O12 C11 C12 120(3) . . ?
 O14 C14 C13 112(3) . . ?
 O13 C14 O14 123.5(18) . . ?
 O13 C14 C13 124(4) . . ?
 N13 C13 C14 107(2) . . ?
 N13 C13 C12 110.6(17) . . ?
 C12 C13 C14 116(3) . . ?
 N3 C3 C4 106(2) . . ?
 N3 C3 C2 109(2) . . ?
 C2 C3 C4 115(3) . . ?
 C13 C12 C11 113(2) . . ?
 C3 C2 C1 113.2(10) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -12(5) . . . . ?
 Zn1 O11 C11 C12 -170.3(11) . . . . ?
 O2 C1 C2 C3 -29(5) . . . . ?
 O12 C11 C12 C13 -154(3) . . . . ?
 N13 C13 C14 O13 -11(3) . . . . ?
 N3 C3 C4 O3 38.7(19) . . . . ?
 C1 C2 C3 N3 73(4) . . . . ?
 C1 C2 C3 C4 -46(5) . . . . ?
 C11 C12 C13 N13 -70(3) . . . . ?
 C11 C12 C13 C14 53(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_2_49GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972156'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_2_49GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.193 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_2_49GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03017 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_2_49GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H3B      .       2.05 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     15.731(3) 
_cell_length_b                     10.3513(6) 
_cell_length_c                     14.1190(9) 
_cell_angle_alpha                  90.00 
_cell_angle_beta                   92.92(2) 
_cell_angle_gamma                  90.00 
_cell_volume                       2296.1(4) 
_cell_formula_units_Z              4
_cell_measurement_reflns_used      320
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         2490000 
_cell_measurement_theta_max        26.737
_cell_measurement_theta_min        3.780
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.198
_exptl_absorpt_correction_T_max    0.896
_exptl_absorpt_correction_T_min    0.680
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 2.49(2) GPa
 (2490000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.063
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0690
_diffrn_reflns_av_unetI/netI       0.0394
_diffrn_reflns_Laue_measured_fraction_full  0.193
_diffrn_reflns_Laue_measured_fraction_max  0.175
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         13
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              4599
_diffrn_reflns_point_group_measured_fraction_full  0.193
_diffrn_reflns_point_group_measured_fraction_max  0.175
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.737
_diffrn_reflns_theta_min           3.780
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.193
_diffrn_measured_fraction_theta_max  0.175
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  320
_reflns_number_total               424
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.136
_refine_diff_density_min           -0.135
_refine_diff_density_rms           0.035
_refine_ls_goodness_of_fit_ref     1.106
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       199
_refine_ls_number_reflns           424
_refine_ls_number_restraints       129
_refine_ls_R_factor_all            0.0532
_refine_ls_R_factor_gt             0.0291
_refine_ls_restrained_S_all        0.981
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0339P)²+6.1011P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0572
_refine_ls_wR_factor_ref           0.0668
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C4-O4
 1.44 with sigma of 0.05
 C11-O12
 1.25 with sigma of 0.02
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 2 with sigma of 0.05
 O1W-H1WA
 0.85 with sigma of 0.05
 O1W-H1WB
 0.85 with sigma of 0.05
 H1WA-H1WB
 1.34 with sigma of 0.05
 O2-H1WB
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(N13) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O2W) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.004 and sigma
for terminal atoms of 0.008
4.a Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7360(3) 0.50630(9) 0.45372(6) 0.040(6) Uani 1 1 d . . . . .
 O4 O 0.685(2) 0.8655(8) 0.5507(6) 0.040(3) Uani 1 1 d D U . . .
 O2 O 0.5401(14) 0.7607(5) 0.4008(3) 0.033(4) Uani 1 1 d D U . . .
 O1 O 0.642(2) 0.6070(6) 0.4075(4) 0.036(3) Uani 1 1 d . U . . .
 O14 O 0.7471(19) 0.0438(8) 0.4116(5) 0.053(3) Uani 1 1 d . U . . .
 O11 O 0.7581(18) 0.3799(6) 0.3580(4) 0.052(3) Uani 1 1 d . U . . .
 O13 O 0.8679(19) 0.1397(6) 0.4576(4) 0.041(4) Uani 1 1 d . U . . .
 O12 O 0.6234(19) 0.3416(10) 0.2969(7) 0.053(6) Uani 1 1 d D U . . .
 O3 O 0.5710(18) 1.0083(5) 0.5867(4) 0.041(4) Uani 1 1 d . U . . .
 N13 N 0.891(2) 0.2463(6) 0.2890(5) 0.035(4) Uani 1 1 d . U . . .
 H13A H 0.9036 0.2570 0.2288 0.042 Uiso 1 1 calc GR . . . .
 H13B H 0.9359 0.2261 0.3282 0.037 Uiso 1 1 calc GR . . . .
 H13C H 0.8764 0.3221 0.3133 0.042 Uiso 1 1 calc GR . . . .
 O1W O 0.588(2) 0.9893(8) 0.3129(6) 0.072(5) Uani 1 1 d D U . . .
 H1WA H 0.636(6) 0.978(14) 0.347(13) 0.098 Uiso 1 1 d DR . . . .
 H1WB H 0.555(6) 0.936(8) 0.338(10) 0.098 Uiso 1 1 d DR . . . .
 N3 N 0.461(3) 0.8194(9) 0.5691(6) 0.034(5) Uani 1 1 d . U . . .
 H3A H 0.4608 0.8449 0.5102 0.044 Uiso 1 1 calc GR . . . .
 H3B H 0.4427 0.8787 0.6087 0.041 Uiso 1 1 calc GR . . . .
 H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc GR . . . .
 O2W O 0.5000 0.5261(11) 0.2500 0.055(5) Uani 1 2 d DS TU P . .
 C1 C 0.583(3) 0.6778(9) 0.4455(6) 0.027(3) Uani 1 1 d . U . . .
 C4 C 0.598(3) 0.8988(11) 0.5724(8) 0.028(4) Uani 1 1 d D U . . .
 C11 C 0.702(2) 0.3200(14) 0.3029(10) 0.025(4) Uani 1 1 d D U . . .
 C14 C 0.811(3) 0.1132(9) 0.3974(7) 0.029(3) Uani 1 1 d . U . . .
 C13 C 0.818(3) 0.1541(8) 0.2939(6) 0.027(3) Uani 1 1 d . U . . .
 H13 H 0.8320 0.0769 0.2578 0.032 Uiso 1 1 calc R . . . .
 C3 C 0.542(3) 0.7827(10) 0.5982(8) 0.035(4) Uani 1 1 d . U . . .
 H3 H 0.5445 0.7708 0.6671 0.042 Uiso 1 1 calc R . . . .
 C12 C 0.736(3) 0.2091(8) 0.2491(6) 0.031(3) Uani 1 1 d . U . . .
 H12A H 0.7466 0.2374 0.1852 0.037 Uiso 1 1 calc R . . . .
 H12B H 0.6937 0.1411 0.2444 0.037 Uiso 1 1 calc R . . . .
 C2 C 0.569(2) 0.6591(7) 0.5511(5) 0.029(3) Uani 1 1 d . U . . .
 H2A H 0.5255 0.5936 0.5585 0.034 Uiso 1 1 calc R . . . .
 H2B H 0.6212 0.6285 0.5825 0.034 Uiso 1 1 calc R . . . .
 H2W H 0.542(6) 0.475(8) 0.238(8) 0.09(6) Uiso 1 1 d D . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.83(3) 7_666 ?
 Zn1 O1 1.90(3) . ?
 Zn1 O14 1.977(8) 7_656 ?
 Zn1 O11 1.923(9) . ?
 Zn1 C14 2.574(18) 7_656 ?
 O4 C4 1.45(6) . ?
 O2 C1 1.24(3) . ?
 O1 C1 1.32(5) . ?
 O14 C14 1.26(5) . ?
 O11 C11 1.31(3) . ?
 O13 C14 1.25(4) . ?
 O12 C11 1.25(3) . ?
 O3 C4 1.23(2) . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.48(4) . ?
 O1W H1WA 0.87(7) . ?
 O1W H1WB 0.83(6) . ?
 N3 H3A 0.8700 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8000 . ?
 N3 C3 1.38(7) . ?
 O2W H2W 0.86(6) . ?
 O2W H2W 0.86(6) 2_655 ?
 C1 C2 1.530(17) . ?
 C4 C3 1.54(5) . ?
 C11 C12 1.49(3) . ?
 C14 C13 1.532(14) . ?
 C13 H13 0.9800 . ?
 C13 C12 1.53(5) . ?
 C3 H3 0.9800 . ?
 C3 C2 1.51(2) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 96.4(11) 7_666 . ?
 O4 Zn1 O14 99.1(8) 7_666 7_656 ?
 O4 Zn1 O11 108.7(10) 7_666 . ?
 O4 Zn1 C14 126.6(8) 7_666 7_656 ?
 O1 Zn1 O14 122.9(9) . 7_656 ?
 O1 Zn1 O11 107.3(8) . . ?
 O1 Zn1 C14 107.4(9) . 7_656 ?
 O14 Zn1 C14 28.4(12) 7_656 7_656 ?
 O11 Zn1 O14 118.5(4) . 7_656 ?
 O11 Zn1 C14 108.4(4) . 7_656 ?
 C4 O4 Zn1 119.0(11) . 7_666 ?
 C1 O1 Zn1 135.9(11) . . ?
 C14 O14 Zn1 103.2(16) . 7_656 ?
 C11 O11 Zn1 127(2) . . ?
 H13A N13 H13B 114.0 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 100.0 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 114.0 . . ?
 C13 N13 H13C 109.5 . . ?
 H1WA O1W H1WB 103(10) . . ?
 H3A N3 H3B 114.0 . . ?
 H3A N3 H3C 114.0 . . ?
 H3B N3 H3C 108.0 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 102.0 . . ?
 H2W O2W H2W 106(10) . 2_655 ?
 O2 C1 O1 123.3(13) . . ?
 O2 C1 C2 119(3) . . ?
 O1 C1 C2 118(2) . . ?
 O4 C4 C3 114(2) . . ?
 O3 C4 O4 126(3) . . ?
 O3 C4 C3 118(4) . . ?
 O11 C11 C12 115(3) . . ?
 O12 C11 O11 126(2) . . ?
 O12 C11 C12 118(2) . . ?
 O14 C14 Zn1 48.4(7) . 7_656 ?
 O14 C14 C13 115(3) . . ?
 O13 C14 Zn1 77.0(10) . 7_656 ?
 O13 C14 O14 125.4(14) . . ?
 O13 C14 C13 120(3) . . ?
 C13 C14 Zn1 162(2) . 7_656 ?
 N13 C13 C14 109(2) . . ?
 N13 C13 H13 107.5 . . ?
 N13 C13 C12 112.2(15) . . ?
 C14 C13 H13 107.5 . . ?
 C12 C13 C14 113(3) . . ?
 C12 C13 H13 107.5 . . ?
 N3 C3 C4 104(2) . . ?
 N3 C3 H3 109.4 . . ?
 N3 C3 C2 112(2) . . ?
 C4 C3 H3 109.4 . . ?
 C2 C3 C4 113(3) . . ?
 C2 C3 H3 109.4 . . ?
 C11 C12 C13 113.0(18) . . ?
 C11 C12 H12A 109.0 . . ?
 C11 C12 H12B 109.0 . . ?
 C13 C12 H12A 109.0 . . ?
 C13 C12 H12B 109.0 . . ?
 H12A C12 H12B 107.8 . . ?
 C1 C2 H2A 109.2 . . ?
 C1 C2 H2B 109.2 . . ?
 C3 C2 C1 112.2(10) . . ?
 C3 C2 H2A 109.2 . . ?
 C3 C2 H2B 109.2 . . ?
 H2A C2 H2B 107.9 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -16(5) . . . . ?
 Zn1 O11 C11 C12 -168.6(9) . . . . ?
 O2 C1 C2 C3 -31(5) . . . . ?
 O12 C11 C12 C13 -153(2) . . . . ?
 N13 C13 C14 O13 -12(3) . . . . ?
 N3 C3 C4 O3 41(2) . . . . ?
 C1 C2 C3 N3 70(4) . . . . ?
 C1 C2 C3 C4 -47(4) . . . . ?
 C11 C12 C13 N13 -67(2) . . . . ?
 C11 C12 C13 C14 56(2) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_2_91GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972157'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_2_91GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.190 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_2_91GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.029 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_2_91GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H3B      .       1.97 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     15.680(3) 
_cell_length_b                     10.3060(8) 
_cell_length_c                     14.0720(12) 
_cell_angle_alpha                  90.00 
_cell_angle_beta                   92.80(3) 
_cell_angle_gamma                  90.00 
_cell_volume                       2271.3(6) 
_cell_formula_units_Z              4
_cell_measurement_reflns_used      312
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         2490000 
_cell_measurement_theta_max        26.834
_cell_measurement_theta_min        3.792
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.222
_exptl_absorpt_correction_T_max    0.895
_exptl_absorpt_correction_T_min    0.677
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 2.91(2) GPa
 (2910000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.086
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0710
_diffrn_reflns_av_unetI/netI       0.0396
_diffrn_reflns_Laue_measured_fraction_full  0.190
_diffrn_reflns_Laue_measured_fraction_max  0.170
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              4527
_diffrn_reflns_point_group_measured_fraction_full  0.190
_diffrn_reflns_point_group_measured_fraction_max  0.170
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.834
_diffrn_reflns_theta_min           3.792
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.190
_diffrn_measured_fraction_theta_max  0.170
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  312
_reflns_number_total               413
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max           0.133
_refine_diff_density_min           -0.122
_refine_diff_density_rms           0.036
_refine_ls_goodness_of_fit_ref     1.091
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       199
_refine_ls_number_reflns           413
_refine_ls_number_restraints       130
_refine_ls_R_factor_all            0.0544
_refine_ls_R_factor_gt             0.0317
_refine_ls_restrained_S_all        0.945
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+21.7186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0530
_refine_ls_wR_factor_ref           0.0615
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O4-C4
 1.34 with sigma of 0.02
 C11-O12
 1.26 with sigma of 0.05
 C14-N13
 2.43 with sigma of 0.02
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 1.95 with sigma of 0.05
 O1W-H1WA
 0.85 with sigma of 0.05
 O1W-H1WB
 0.85 with sigma of 0.05
 H1WA-H1WB
 1.34 with sigma of 0.05
 O2-H1WB
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O2W) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7366(3) 0.50612(10) 0.45405(7) 0.048(6) Uani 1 1 d . . . . .
 O4 O 0.679(2) 0.8643(8) 0.5506(6) 0.038(3) Uani 1 1 d D U . . .
 O2 O 0.5389(16) 0.7599(6) 0.4017(4) 0.034(4) Uani 1 1 d D U . . .
 O1 O 0.640(2) 0.6060(7) 0.4081(5) 0.035(3) Uani 1 1 d . U . . .
 O14 O 0.742(2) 0.0430(8) 0.4107(5) 0.054(3) Uani 1 1 d . U . . .
 O11 O 0.757(2) 0.3808(7) 0.3574(5) 0.054(3) Uani 1 1 d . U . . .
 O13 O 0.867(2) 0.1395(7) 0.4578(5) 0.040(4) Uani 1 1 d . U . . .
 O12 O 0.622(2) 0.3419(11) 0.2958(8) 0.051(6) Uani 1 1 d D U . . .
 O3 O 0.5720(19) 1.0086(6) 0.5868(5) 0.040(4) Uani 1 1 d . U . . .
 N13 N 0.892(2) 0.2459(7) 0.2884(5) 0.035(4) Uani 1 1 d D U . . .
 H13A H 0.9061 0.2544 0.2283 0.042 Uiso 1 1 calc GR . . . .
 H13B H 0.9357 0.2148 0.3235 0.042 Uiso 1 1 calc GR . . . .
 H13C H 0.8768 0.3230 0.3109 0.042 Uiso 1 1 calc GR . . . .
 O1W O 0.587(2) 0.9892(10) 0.3112(6) 0.071(5) Uani 1 1 d D U . . .
 H1WA H 0.634(7) 0.980(16) 0.347(14) 0.106 Uiso 1 1 d DR . . . .
 H1WB H 0.554(8) 0.938(8) 0.342(12) 0.106 Uiso 1 1 d DR . . . .
 N3 N 0.457(3) 0.8189(11) 0.5683(7) 0.037(5) Uani 1 1 d . U . . .
 H3A H 0.4570 0.8500 0.5092 0.044 Uiso 1 1 calc GR . . . .
 H3B H 0.4384 0.8796 0.6071 0.044 Uiso 1 1 calc GR . . . .
 H3C H 0.4233 0.7497 0.5696 0.044 Uiso 1 1 calc GR . . . .
 O2W O 0.5000 0.5250(11) 0.2500 0.054(5) Uani 1 2 d DS TU P . .
 C1 C 0.581(4) 0.6760(10) 0.4459(6) 0.029(3) Uani 1 1 d . U . . .
 C4 C 0.600(2) 0.8984(13) 0.5727(8) 0.028(4) Uani 1 1 d D U . . .
 C11 C 0.701(3) 0.3204(16) 0.3037(11) 0.028(5) Uani 1 1 d D U . . .
 C14 C 0.815(3) 0.1122(11) 0.3974(8) 0.030(3) Uani 1 1 d D U . . .
 C13 C 0.817(3) 0.1535(9) 0.2926(6) 0.028(3) Uani 1 1 d . U . . .
 H13 H 0.8310 0.0762 0.2560 0.034 Uiso 1 1 calc R . . . .
 C3 C 0.541(4) 0.7829(11) 0.5982(9) 0.032(4) Uani 1 1 d . U . . .
 H3 H 0.5443 0.7710 0.6674 0.038 Uiso 1 1 calc R . . . .
 C12 C 0.739(3) 0.2089(10) 0.2475(7) 0.035(3) Uani 1 1 d . U . . .
 H12A H 0.6967 0.1408 0.2392 0.042 Uiso 1 1 calc R . . . .
 H12B H 0.7518 0.2405 0.1848 0.042 Uiso 1 1 calc R . . . .
 C2 C 0.566(2) 0.6581(8) 0.5517(5) 0.029(3) Uani 1 1 d . U . . .
 H2A H 0.5219 0.5941 0.5593 0.035 Uiso 1 1 calc R . . . .
 H2B H 0.6185 0.6255 0.5833 0.035 Uiso 1 1 calc R . . . .
 H2W H 0.545(9) 0.477(14) 0.238(10) 0.10(10) Uiso 1 1 d D . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.88(3) 7_666 ?
 Zn1 O1 1.91(3) . ?
 Zn1 O14 1.983(10) 7_656 ?
 Zn1 O11 1.914(11) . ?
 Zn1 C14 2.583(18) 7_656 ?
 O4 C4 1.34(3) . ?
 O2 C1 1.24(4) . ?
 O1 C1 1.31(6) . ?
 O14 C14 1.37(5) . ?
 O11 C11 1.30(4) . ?
 O13 C14 1.18(4) . ?
 O12 C11 1.26(6) . ?
 O3 C4 1.24(3) . ?
 N13 C13 1.51(5) . ?
 N3 C3 1.42(8) . ?
 C1 C2 1.53(2) . ?
 C4 C3 1.55(5) . ?
 C11 C12 1.53(4) . ?
 C14 C13 1.537(15) . ?
 C13 C12 1.46(6) . ?
 C3 C2 1.50(2) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 98.7(11) 7_666 . ?
 O4 Zn1 O14 97.3(10) 7_666 7_656 ?
 O4 Zn1 O11 108.0(11) 7_666 . ?
 O4 Zn1 C14 127.6(8) 7_666 7_656 ?
 O1 Zn1 O14 123.8(11) . 7_656 ?
 O1 Zn1 O11 106.3(9) . . ?
 O1 Zn1 C14 104.8(10) . 7_656 ?
 O14 Zn1 C14 31.5(14) 7_656 7_656 ?
 O11 Zn1 O14 118.9(6) . 7_656 ?
 O11 Zn1 C14 109.1(5) . 7_656 ?
 C4 O4 Zn1 118.8(12) . 7_666 ?
 C1 O1 Zn1 136.4(13) . . ?
 C14 O14 Zn1 99.2(19) . 7_656 ?
 C11 O11 Zn1 127(3) . . ?
 O2 C1 O1 123.5(17) . . ?
 O2 C1 C2 118(3) . . ?
 O1 C1 C2 118(3) . . ?
 O4 C4 C3 114(2) . . ?
 O3 C4 O4 128(3) . . ?
 O3 C4 C3 117(4) . . ?
 O11 C11 C12 113(4) . . ?
 O12 C11 O11 128(3) . . ?
 O12 C11 C12 120(3) . . ?
 O14 C14 Zn1 49.3(8) . 7_656 ?
 O14 C14 C13 109(3) . . ?
 O13 C14 Zn1 76.2(12) . 7_656 ?
 O13 C14 O14 125.2(17) . . ?
 O13 C14 C13 125(3) . . ?
 C13 C14 Zn1 158(3) . 7_656 ?
 N13 C13 C14 105(2) . . ?
 C12 C13 N13 111.6(18) . . ?
 C12 C13 C14 118(3) . . ?
 N3 C3 C4 106(2) . . ?
 N3 C3 C2 111(3) . . ?
 C2 C3 C4 113(4) . . ?
 C13 C12 C11 114(2) . . ?
 C3 C2 C1 112.0(12) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -17(6) . . . . ?
 Zn1 O11 C11 C12 -169.2(11) . . . . ?
 O2 C1 C2 C3 -31(6) . . . . ?
 O12 C11 C12 C13 -152(3) . . . . ?
 N13 C13 C14 O13 -6(4) . . . . ?
 N3 C3 C4 O3 41(2) . . . . ?
 C1 C2 C3 N3 71(4) . . . . ?
 C1 C2 C3 C4 -48(5) . . . . ?
 C11 C12 C13 N13 -71(3) . . . . ?
 C11 C12 C13 C14 51(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_3_54GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972158'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_3_54GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.192 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_3_54GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02917 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_3_54GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H3B      .       1.96 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     15.612(4) 
_cell_length_b                     10.2330(9) 
_cell_length_c                     13.9799(14) 
_cell_angle_alpha                  90.00 
_cell_angle_beta                   92.78(3) 
_cell_angle_gamma                  90.00 
_cell_volume                       2230.7(7) 
_cell_formula_units_Z              4
_cell_measurement_reflns_used      305
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         3540000 
_cell_measurement_theta_max        27.026
_cell_measurement_theta_min        3.717
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.263
_exptl_absorpt_correction_T_max    0.893
_exptl_absorpt_correction_T_min    0.672
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 3.54(2) GPa
 (3540000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.124
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0729
_diffrn_reflns_av_unetI/netI       0.0421
_diffrn_reflns_Laue_measured_fraction_full  0.192
_diffrn_reflns_Laue_measured_fraction_max  0.170
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              4443
_diffrn_reflns_point_group_measured_fraction_full  0.192
_diffrn_reflns_point_group_measured_fraction_max  0.170
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.026
_diffrn_reflns_theta_min           3.717
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.192
_diffrn_measured_fraction_theta_max  0.170
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  305
_reflns_number_total               413
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max           0.123
_refine_diff_density_min           -0.179
_refine_diff_density_rms           0.039
_refine_ls_goodness_of_fit_ref     1.140
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       199
_refine_ls_number_reflns           413
_refine_ls_number_restraints       129
_refine_ls_R_factor_all            0.0576
_refine_ls_R_factor_gt             0.0332
_refine_ls_restrained_S_all        0.988
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+16.5695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0504
_refine_ls_wR_factor_ref           0.0574
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O4-C4
 1.27 with sigma of 0.03
 O12-C11
 1.2 with sigma of 0.03
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 1.9 with sigma of 0.05
 O1W-H1WA
 0.85 with sigma of 0.05
 O1W-H1WB
 0.85 with sigma of 0.05
 H1WA-H1WB
 1.34 with sigma of 0.05
 O2-H1WB
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7373(3) 0.50605(11) 0.45450(7) 0.042(6) Uani 1 1 d . . . . .
 O4 O 0.679(2) 0.8628(8) 0.5499(6) 0.036(3) Uani 1 1 d D U . . .
 O2 O 0.5378(16) 0.7596(6) 0.4021(4) 0.030(4) Uani 1 1 d D U . . .
 O1 O 0.638(3) 0.6046(7) 0.4088(4) 0.035(3) Uani 1 1 d . U . . .
 O14 O 0.741(2) 0.0421(8) 0.4093(5) 0.053(3) Uani 1 1 d . U . . .
 O11 O 0.758(2) 0.3814(6) 0.3559(5) 0.049(3) Uani 1 1 d . U . . .
 O13 O 0.866(2) 0.1387(7) 0.4579(5) 0.037(4) Uani 1 1 d . U . . .
 O12 O 0.621(2) 0.3439(11) 0.2953(8) 0.053(6) Uani 1 1 d D U . . .
 O3 O 0.5719(18) 1.0088(6) 0.5874(4) 0.039(4) Uani 1 1 d . U . . .
 N13 N 0.891(2) 0.2459(7) 0.2872(5) 0.032(4) Uani 1 1 d . U . . .
 H13A H 0.9043 0.2556 0.2264 0.039 Uiso 1 1 calc GR . . . .
 H13B H 0.9359 0.2130 0.3208 0.039 Uiso 1 1 calc GR . . . .
 H13C H 0.8774 0.3232 0.3113 0.039 Uiso 1 1 calc GR . . . .
 O1W O 0.583(2) 0.9898(10) 0.3089(5) 0.066(5) Uani 1 1 d D U . . .
 H1WA H 0.632(7) 0.977(15) 0.343(15) 0.100 Uiso 1 1 d DR . . . .
 H1WB H 0.551(8) 0.939(8) 0.344(12) 0.100 Uiso 1 1 d DR . . . .
 N3 N 0.453(3) 0.8198(11) 0.5684(6) 0.035(5) Uani 1 1 d . U . . .
 H3A H 0.4608 0.8449 0.5102 0.044 Uiso 1 1 calc GR . . . .
 H3B H 0.4318 0.8721 0.6123 0.042 Uiso 1 1 calc GR . . . .
 H3C H 0.4200 0.7491 0.5615 0.042 Uiso 1 1 calc GR . . . .
 O2W O 0.5000 0.5261(12) 0.2500 0.051(6) Uani 1 2 d DS TU P . .
 C1 C 0.577(4) 0.6765(10) 0.4464(6) 0.029(3) Uani 1 1 d . U . . .
 C4 C 0.603(3) 0.8971(13) 0.5727(9) 0.027(4) Uani 1 1 d D U . . .
 C11 C 0.696(2) 0.3207(15) 0.3014(11) 0.023(4) Uani 1 1 d D U . . .
 C14 C 0.809(4) 0.1126(11) 0.3969(8) 0.030(4) Uani 1 1 d . U . . .
 C12 C 0.736(3) 0.2089(10) 0.2469(7) 0.034(4) Uani 1 1 d . U . . .
 H12A H 0.6943 0.1395 0.2386 0.041 Uiso 1 1 calc R . . . .
 H12B H 0.7492 0.2400 0.1836 0.041 Uiso 1 1 calc R . . . .
 C13 C 0.815(3) 0.1533(8) 0.2925(6) 0.024(3) Uani 1 1 d . U . . .
 H13 H 0.8290 0.0747 0.2563 0.029 Uiso 1 1 calc R . . . .
 C3 C 0.537(3) 0.7818(10) 0.5982(8) 0.026(4) Uani 1 1 d . U . . .
 H3 H 0.5398 0.7697 0.6678 0.031 Uiso 1 1 calc R . . . .
 C2 C 0.561(2) 0.6565(8) 0.5528(5) 0.029(3) Uani 1 1 d . U . . .
 H2A H 0.5151 0.5936 0.5590 0.034 Uiso 1 1 calc R . . . .
 H2B H 0.6123 0.6215 0.5854 0.034 Uiso 1 1 calc R . . . .
 H2W H 0.547(8) 0.480(12) 0.235(9) 0.10(8) Uiso 1 1 d D . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.88(3) 7_666 ?
 Zn1 O1 1.93(4) . ?
 Zn1 O14 1.983(10) 7_656 ?
 Zn1 O11 1.920(11) . ?
 Zn1 C14 2.54(2) 7_656 ?
 O4 C4 1.30(4) . ?
 O2 C1 1.20(3) . ?
 O1 C1 1.33(6) . ?
 O14 C14 1.31(6) . ?
 O11 C11 1.36(4) . ?
 O13 C14 1.24(5) . ?
 O12 C11 1.20(4) . ?
 O3 C4 1.26(3) . ?
 N13 C13 1.51(5) . ?
 N3 C3 1.44(8) . ?
 C1 C2 1.53(2) . ?
 C4 C3 1.60(6) . ?
 C11 C12 1.53(4) . ?
 C14 C13 1.526(16) . ?
 C12 C13 1.48(6) . ?
 C3 C2 1.49(2) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 99.3(11) 7_666 . ?
 O4 Zn1 O14 96.6(9) 7_666 7_656 ?
 O4 Zn1 O11 107.9(11) 7_666 . ?
 O4 Zn1 C14 126.2(10) 7_666 7_656 ?
 O1 Zn1 O14 123.4(10) . 7_656 ?
 O1 Zn1 C14 105.5(11) . 7_656 ?
 O14 Zn1 C14 30.6(15) 7_656 7_656 ?
 O11 Zn1 O1 105.9(9) . . ?
 O11 Zn1 O14 119.9(6) . 7_656 ?
 O11 Zn1 C14 109.7(4) . 7_656 ?
 C4 O4 Zn1 117.6(13) . 7_666 ?
 C1 O1 Zn1 137.4(14) . . ?
 C14 O14 Zn1 98.8(18) . 7_656 ?
 C11 O11 Zn1 124(3) . . ?
 O2 C1 O1 122.8(18) . . ?
 O2 C1 C2 120(3) . . ?
 O1 C1 C2 117(3) . . ?
 O4 C4 C3 117(2) . . ?
 O3 C4 O4 130(3) . . ?
 O3 C4 C3 112(4) . . ?
 O11 C11 C12 109(4) . . ?
 O12 C11 O11 129(2) . . ?
 O12 C11 C12 123(3) . . ?
 O14 C14 Zn1 50.6(8) . 7_656 ?
 O14 C14 C13 112(3) . . ?
 O13 C14 Zn1 76.4(11) . 7_656 ?
 O13 C14 O14 126.9(17) . . ?
 O13 C14 C13 121(4) . . ?
 C13 C14 Zn1 162(3) . 7_656 ?
 C13 C12 C11 115.3(19) . . ?
 N13 C13 C14 108(3) . . ?
 C12 C13 N13 112.0(17) . . ?
 C12 C13 C14 115(4) . . ?
 N3 C3 C4 109.0(19) . . ?
 N3 C3 C2 110(3) . . ?
 C2 C3 C4 112(3) . . ?
 C3 C2 C1 110.6(11) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 -20(6) . . . . ?
 Zn1 O11 C11 C12 -168.0(10) . . . . ?
 O2 C1 C2 C3 -32(5) . . . . ?
 O12 C11 C12 C13 -152(3) . . . . ?
 N13 C13 C14 O13 -10(4) . . . . ?
 N3 C3 C4 O3 39.1(18) . . . . ?
 C1 C2 C3 N3 73(4) . . . . ?
 C1 C2 C3 C4 -48(4) . . . . ?
 C11 C12 C13 N13 -71(3) . . . . ?
 C11 C12 C13 C14 53(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_sesquihydrate_3_92GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972159'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_sesquihydrate_3_92GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.189 Why? 
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT316_zinc-aspartate_sesquihydrate_3_92GPa
;
PROBLEM: Too many H on C in C=N Moiety in Main Residue ..         C3 Check 
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT341_zinc-aspartate_sesquihydrate_3_92GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04167 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_sesquihydrate_3_92GPa
;
PROBLEM: Short Inter D-H..H-D       H1WB     ..H3B      .       1.80 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate sesquihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 3(H2 O)'
_chemical_formula_sum              'C16 H30 N4 O19 Zn2'
_chemical_formula_weight           713.18
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     15.550(3)
_cell_length_b                     10.2262(7)
_cell_length_c                     13.9663(11)
_cell_angle_alpha                  90
_cell_angle_beta                   92.62(3)
_cell_angle_gamma                  90
_cell_volume                       2218.6(4)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      292
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         3920000 
_cell_measurement_theta_max        27.050
_cell_measurement_theta_min        3.724
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.275
_exptl_absorpt_correction_T_max    0.892
_exptl_absorpt_correction_T_min    0.671
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 3.92(2) GPa
 (3920000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.135
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               1464
_exptl_crystal_size_max            0.20
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0765
_diffrn_reflns_av_unetI/netI       0.0457
_diffrn_reflns_Laue_measured_fraction_full  0.189
_diffrn_reflns_Laue_measured_fraction_max  0.168
_diffrn_reflns_limit_h_max         3
_diffrn_reflns_limit_h_min         -3
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              4400
_diffrn_reflns_point_group_measured_fraction_full  0.189
_diffrn_reflns_point_group_measured_fraction_max  0.168
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.050
_diffrn_reflns_theta_min           3.724
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.189
_diffrn_measured_fraction_theta_max  0.168
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  292
_reflns_number_total               407
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max           0.146
_refine_diff_density_min           -0.178
_refine_diff_density_rms           0.042
_refine_ls_goodness_of_fit_ref     1.098
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       196
_refine_ls_number_reflns           407
_refine_ls_number_restraints       125
_refine_ls_R_factor_all            0.0633
_refine_ls_R_factor_gt             0.0333
_refine_ls_restrained_S_all        0.953
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0239P)²+19.0079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0609
_refine_ls_wR_factor_ref           0.0735
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N13-C13
 1.4 with sigma of 0.01
 C4-O4
 1.3 with sigma of 0.05
 C11-O12
 1.2 with sigma of 0.05
 O2W-H2W
 0.85 with sigma of 0.05
 O12-H2W
 1.85 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2W) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1Wa,H1Wb)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C2(H2a,H2b)
4.d Idealised Me refined as rotating group:
 N13(H13a,H13b,H13c), N3(H3a,H3b,H3c)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7371(5) 0.50611(13) 0.45476(9) 0.039(8) Uani 1 1 d . . . . .
 O4 O 0.683(3) 0.8608(11) 0.5494(7) 0.039(4) Uani 1 1 d D U . . .
 O2 O 0.538(2) 0.7597(7) 0.4025(5) 0.031(5) Uani 1 1 d . U . . .
 O1 O 0.639(3) 0.6032(9) 0.4084(6) 0.038(3) Uani 1 1 d . U . . .
 O14 O 0.740(3) 0.0421(11) 0.4091(7) 0.057(4) Uani 1 1 d . U . . .
 O11 O 0.759(3) 0.3822(9) 0.3549(6) 0.053(4) Uani 1 1 d . U . . .
 O13 O 0.866(3) 0.1399(9) 0.4579(6) 0.043(5) Uani 1 1 d . U . . .
 O12 O 0.621(3) 0.3436(14) 0.2953(10) 0.056(7) Uani 1 1 d D U . . .
 O3 O 0.571(3) 1.0085(8) 0.5868(6) 0.041(5) Uani 1 1 d . U . . .
 N13 N 0.887(3) 0.2452(9) 0.2869(7) 0.036(5) Uani 1 1 d D U . . .
 H13A H 0.9032 0.2616 0.2371 0.037 Uiso 1 1 calc R . . . . 
 H13B H 0.9359 0.2261 0.3282 0.037 Uiso 1 1 calc R . . . . 
 H13C H 0.8752 0.3250 0.3180 0.037 Uiso 1 1 calc R . . . . 
 O1W O 0.581(3) 0.9885(13) 0.3074(7) 0.067(6) Uani 1 1 d . U . . .
 H1WA H 0.635287 0.975314 0.345508 0.101 Uiso 1 1 d G . . . .
 H1WB H 0.555092 0.951324 0.353999 0.101 Uiso 1 1 d G . . . .
 N3 N 0.46595(11) 0.82054(17) 0.56868(13) 0.033(6) Uani 1 1 d . U . . .
 H3A H 0.4608 0.8449 0.5102 0.044 Uiso 1 1 calc R . . . .
 H3B H 0.4505 0.8821 0.6050 0.044 Uiso 1 1 calc R . . . .
 H3C H 0.4344 0.7541 0.5766 0.044 Uiso 1 1 calc R . . . . 
 O2W O 0.500000 0.5268(14) 0.250000 0.052(7) Uani 1 2 d DS TU P . .
 C1 C 0.578(5) 0.6751(13) 0.4467(8) 0.028(4) Uani 1 1 d . U . . .
 C4 C 0.604(4) 0.8968(15) 0.5729(10) 0.024(5) Uani 1 1 d D U . . .
 C11 C 0.698(3) 0.3226(18) 0.3009(13) 0.022(5) Uani 1 1 d D U . . .
 C14 C 0.810(5) 0.1117(13) 0.3958(9) 0.030(4) Uani 1 1 d . U . . .
 C12 C 0.736(4) 0.2090(11) 0.2459(8) 0.032(4) Uani 1 1 d . U . . .
 H12A H 0.746721 0.238171 0.181480 0.038 Uiso 1 1 calc R . . . .
 H12B H 0.693684 0.139348 0.240780 0.038 Uiso 1 1 calc R . . . .
 C13 C 0.820(3) 0.1530(11) 0.2914(8) 0.024(4) Uani 1 1 d D U . . .
 H13 H 0.835880 0.075561 0.254830 0.029 Uiso 1 1 calc R . . . .
 C3 C 0.534(4) 0.7805(13) 0.5988(10) 0.030(5) Uani 1 1 d . U . . .
 H3 H 0.535788 0.768394 0.668454 0.036 Uiso 1 1 calc R . . . .
 C2 C 0.560(3) 0.6555(10) 0.5532(7) 0.030(4) Uani 1 1 d . U . . .
 H2A H 0.514966 0.591374 0.558842 0.036 Uiso 1 1 calc R . . . .
 H2B H 0.611784 0.622002 0.586690 0.036 Uiso 1 1 calc R . . . .
 H2W H 0.546(10) 0.474(14) 0.239(12) 0.10(10) Uiso 1 1 d D . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O4 1.85(3) 7_666 ?
 Zn1 O1 1.91(4) . ?
 Zn1 O14 1.981(12) 7_656 ?
 Zn1 O11 1.925(12) . ?
 Zn1 C14 2.54(3) 7_656 ?
 O4 C4 1.34(6) . ?
 O2 C1 1.22(4) . ?
 O1 C1 1.33(7) . ?
 O14 C14 1.32(7) . ?
 O11 C11 1.33(5) . ?
 O13 C14 1.23(6) . ?
 O12 C11 1.21(6) . ?
 O3 C4 1.27(3) . ?
 N13 C13 1.410(13) . ?
 N3 C3 1.19(5) . ?
 C1 C2 1.54(2) . ?
 C4 C3 1.66(6) . ?
 C11 C12 1.53(4) . ?
 C14 C13 1.533(19) . ?
 C12 C13 1.54(6) . ?
 C3 C2 1.49(3) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O4 Zn1 O1 97.8(14) 7_666 . ?
 O4 Zn1 O14 96.9(11) 7_666 7_656 ?
 O4 Zn1 O11 108.8(13) 7_666 . ?
 O4 Zn1 C14 126.3(11) 7_666 7_656 ?
 O1 Zn1 O14 124.3(13) . 7_656 ?
 O1 Zn1 O11 105.0(10) . . ?
 O1 Zn1 C14 105.7(13) . 7_656 ?
 O14 Zn1 C14 30.8(17) 7_656 7_656 ?
 O11 Zn1 O14 120.1(7) . 7_656 ?
 O11 Zn1 C14 110.4(5) . 7_656 ?
 C4 O4 Zn1 115.7(14) . 7_666 ?
 C1 O1 Zn1 136.3(16) . . ?
 C14 O14 Zn1 99(2) . 7_656 ?
 C11 O11 Zn1 125(3) . . ?
 O2 C1 O1 123.1(19) . . ?
 O2 C1 C2 118(4) . . ?
 O1 C1 C2 119(3) . . ?
 O4 C4 C3 118(2) . . ?
 O3 C4 O4 132(4) . . ?
 O3 C4 C3 110(4) . . ?
 O11 C11 C12 111(4) . . ?
 O12 C11 O11 129(3) . . ?
 O12 C11 C12 120(3) . . ?
 O14 C14 Zn1 50.3(10) . 7_656 ?
 O14 C14 C13 114(3) . . ?
 O13 C14 Zn1 75.6(13) . 7_656 ?
 O13 C14 O14 126(2) . . ?
 O13 C14 C13 120(5) . . ?
 C13 C14 Zn1 163(3) . 7_656 ?
 C11 C12 C13 115(2) . . ?
 N13 C13 C14 110(2) . . ?
 N13 C13 C12 110.5(17) . . ?
 C14 C13 C12 112(4) . . ?
 N3 C3 C4 104.9(18) . . ?
 N3 C3 C2 112(3) . . ?
 C2 C3 C4 109(4) . . ?
 C3 C2 C1 111.5(13) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O2 C1 C2 C3 -31(6) . . . . ?
 O12 C11 C12 C13 -153(3) . . . . ?
 N13 C13 C14 O13 -13(4) . . . . ?
 N3 C3 C4 O3 38(2) . . . . ?
 C1 C2 C3 N3 72(5) . . . . ?
 C1 C2 C3 C4 -49(5) . . . . ?
 C11 C12 C13 N13 -67(3) . . . . ?
 C11 C12 C13 C14 55(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_0_001GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972160'

_audit_creation_date               2019-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' -1.5491 0.6778
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.7873(3)
_cell_length_b                     9.5061(3)
_cell_length_c                     9.8114(3)
_cell_angle_alpha                  111.784(3)
_cell_angle_beta                   105.625(3)
_cell_angle_gamma                  107.721(3)
_cell_volume                       653.73(4)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      2677
_cell_measurement_temperature      296(2)
_cell_measurement_theta_max        76.254
_cell_measurement_theta_min        5.384
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      3.183
_exptl_absorpt_correction_T_max    0.938
_exptl_absorpt_correction_T_min    0.717
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.857
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.10
_exptl_crystal_size_min            0.02
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0199
_diffrn_reflns_av_unetI/netI       0.0112
_diffrn_reflns_Laue_measured_fraction_full  0.998
_diffrn_reflns_Laue_measured_fraction_max  0.988
_diffrn_reflns_limit_h_max         9
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         11
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         12
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              13265
_diffrn_reflns_point_group_measured_fraction_full  0.998
_diffrn_reflns_point_group_measured_fraction_max  0.988
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           76.254
_diffrn_reflns_theta_min           5.384
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.998
_diffrn_measured_fraction_theta_max  0.988
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           150
_diffrn_standards_interval_count   26
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_source                     'sealed x-ray tube'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  2677
_reflns_number_total               2706
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.361
_refine_diff_density_min           -0.382
_refine_diff_density_rms           0.051
_refine_ls_extinction_coef         0.0057(5)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref     1.091
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       199
_refine_ls_number_reflns           2706
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0242
_refine_ls_R_factor_gt             0.0240
_refine_ls_restrained_S_all        1.091
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0323P)²+0.3903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0648
_refine_ls_wR_factor_ref           0.0649
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
2.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
2.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.71338(3) 0.32287(3) 0.54502(2) 0.02403(10) Uani 1 1 d . . . . .
 O1 O 0.64345(16) 0.34223(15) 0.72174(14) 0.0283(3) Uani 1 1 d . . . . .
 O2 O 0.57225(16) 0.27339(15) 0.89453(14) 0.0298(3) Uani 1 1 d . . . . .
 O14 O 1.10055(15) 0.75024(16) 0.46798(14) 0.0310(3) Uani 1 1 d . . . . .
 O4 O 0.50319(16) -0.11786(15) 0.63065(14) 0.0324(3) Uani 1 1 d . . . . .
 O11 O 0.72596(19) 0.50154(16) 0.49431(15) 0.0378(3) Uani 1 1 d . . . . .
 O1W O 0.23254(17) 0.02884(16) 0.77486(16) 0.0345(3) Uani 1 1 d . . . . .
 H1WA H 0.340238 0.092262 0.803331 0.052 Uiso 1 1 d G . . . .
 H1WB H 0.196709 -0.048038 0.677750 0.052 Uiso 1 1 d G . . . .
 O13 O 0.92845(17) 0.50309(17) 0.24279(17) 0.0388(3) Uani 1 1 d . . . . .
 O3 O 0.50923(18) -0.16090(16) 0.84088(15) 0.0374(3) Uani 1 1 d . . . . .
 O12 O 0.84265(19) 0.73004(18) 0.73867(15) 0.0392(3) Uani 1 1 d . . . . .
 O2W O 0.2269(2) 0.3194(2) 1.0024(2) 0.0511(4) Uani 1 1 d . . . . .
 H2WA H 0.218738 0.220466 0.954567 0.077 Uiso 1 1 d G . . . .
 H2WB H 0.218624 0.329127 1.089515 0.077 Uiso 1 1 d G . . . .
 N13 N 0.62832(18) 0.52692(19) 0.21564(17) 0.0290(3) Uani 1 1 d . . . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.7820(2) 0.15150(18) 1.05345(17) 0.0315(3) Uani 1 1 d . . . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C1 C 0.6580(2) 0.27527(19) 0.81203(18) 0.0221(3) Uani 1 1 d . . . . .
 C4 C 0.5710(2) -0.08268(19) 0.77797(19) 0.0241(3) Uani 1 1 d . . . . .
 C14 C 0.9503(2) 0.6363(2) 0.34881(19) 0.0242(3) Uani 1 1 d . . . . .
 C11 C 0.7887(2) 0.6605(2) 0.5899(2) 0.0258(3) Uani 1 1 d . . . . .
 C12 C 0.7913(2) 0.7641(2) 0.5036(2) 0.0254(3) Uani 1 1 d . . . . .
 H12A H 0.893776 0.874522 0.573857 0.030 Uiso 1 1 calc R . . . .
 H12B H 0.686412 0.782128 0.486345 0.030 Uiso 1 1 calc R . . . .
 C13 C 0.7974(2) 0.6821(2) 0.34022(19) 0.0246(3) Uani 1 1 d . . . . .
 H13 H 0.812732 0.764412 0.301412 0.030 Uiso 1 1 calc R . . . .
 C2 C 0.7876(2) 0.2006(2) 0.8223(2) 0.0269(3) Uani 1 1 d . . . . .
 H2A H 0.906071 0.292826 0.894831 0.032 Uiso 1 1 calc R . . . .
 H2B H 0.783972 0.146034 0.715300 0.032 Uiso 1 1 calc R . . . .
 C3 C 0.7547(2) 0.0723(2) 0.88178(19) 0.0255(3) Uani 1 1 d . . . . .
 H3 H 0.842687 0.029647 0.877107 0.031 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.9555(11) . ?
 Zn1 O14 1.9776(12) 2_766 ?
 Zn1 O4 1.9679(12) 2_656 ?
 Zn1 O11 1.9203(13) . ?
 O1 C1 1.2701(19) . ?
 O2 C1 1.2465(19) . ?
 O14 C14 1.281(2) . ?
 O4 C4 1.270(2) . ?
 O11 C11 1.276(2) . ?
 O1W H1WA 0.8499 . ?
 O1W H1WB 0.8500 . ?
 O13 C14 1.220(2) . ?
 O3 C4 1.226(2) . ?
 O12 C11 1.230(2) . ?
 O2W H2WA 0.8500 . ?
 O2W H2WB 0.8504 . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.492(2) . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.481(2) . ?
 C1 C2 1.515(2) . ?
 C4 C3 1.538(2) . ?
 C14 C13 1.524(2) . ?
 C11 C12 1.518(2) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.525(2) . ?
 C13 H13 0.9800 . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C3 1.522(2) . ?
 C3 H3 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 119.50(5) . 2_766 ?
 O1 Zn1 O4 96.87(5) . 2_656 ?
 O4 Zn1 O14 102.06(5) 2_656 2_766 ?
 O11 Zn1 O1 113.53(5) . . ?
 O11 Zn1 O14 114.64(6) . 2_766 ?
 O11 Zn1 O4 106.77(5) . 2_656 ?
 C1 O1 Zn1 131.64(11) . . ?
 C14 O14 Zn1 110.34(10) . 2_766 ?
 C4 O4 Zn1 125.56(11) . 2_656 ?
 C11 O11 Zn1 129.48(11) . . ?
 H1WA O1W H1WB 104.5 . . ?
 H2WA O2W H2WB 104.4 . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 109.5 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 109.5 . . ?
 C3 N3 H3A 109.5 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 109.5 . . ?
 O1 C1 C2 118.45(14) . . ?
 O2 C1 O1 121.88(15) . . ?
 O2 C1 C2 119.64(14) . . ?
 O4 C4 C3 113.75(14) . . ?
 O3 C4 O4 127.36(16) . . ?
 O3 C4 C3 118.84(14) . . ?
 O14 C14 C13 115.30(14) . . ?
 O13 C14 O14 123.85(15) . . ?
 O13 C14 C13 120.73(15) . . ?
 O11 C11 C12 113.83(14) . . ?
 O12 C11 O11 125.68(16) . . ?
 O12 C11 C12 120.49(15) . . ?
 C11 C12 H12A 108.7 . . ?
 C11 C12 H12B 108.7 . . ?
 C11 C12 C13 114.04(13) . . ?
 H12A C12 H12B 107.6 . . ?
 C13 C12 H12A 108.7 . . ?
 C13 C12 H12B 108.7 . . ?
 N13 C13 C14 108.61(13) . . ?
 N13 C13 C12 111.84(13) . . ?
 N13 C13 H13 107.4 . . ?
 C14 C13 C12 114.03(13) . . ?
 C14 C13 H13 107.3 . . ?
 C12 C13 H13 107.4 . . ?
 C1 C2 H2A 108.5 . . ?
 C1 C2 H2B 108.5 . . ?
 C1 C2 C3 115.28(13) . . ?
 H2A C2 H2B 107.5 . . ?
 C3 C2 H2A 108.5 . . ?
 C3 C2 H2B 108.5 . . ?
 N3 C3 C4 108.71(13) . . ?
 N3 C3 C2 111.96(13) . . ?
 N3 C3 H3 107.1 . . ?
 C4 C3 H3 107.1 . . ?
 C2 C3 C4 114.55(13) . . ?
 C2 C3 H3 107.1 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 17.6(2) . . . . ?
 Zn1 O14 C14 C13 176.84(10) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -171.30(10) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 174.20(12) . . . . ?
 O2 C1 C2 C3 22.0(2) . . . . ?
 O12 C11 C12 C13 155.34(16) . . . . ?
 N13 C13 C14 O13 14.0(2) . . . . ?
 N3 C3 C4 O3 -29.7(2) . . . . ?
 C1 C2 C3 N3 -65.97(18) . . . . ?
 C1 C2 C3 C4 58.40(19) . . . . ?
 C11 C12 C13 N13 69.02(17) . . . . ?
 C11 C12 C13 C14 -54.71(18) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_0_05GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972161'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_0_05GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.193 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_0_05GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.05667 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_dihydrate_0_05GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H2WA     .       2.06 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.7874(12)
_cell_length_b                     9.4894(15)
_cell_length_c                     9.812(3)
_cell_angle_alpha                  111.913(19)
_cell_angle_beta                   105.549(16)
_cell_angle_gamma                  107.728(13)
_cell_volume                       652.1(2)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      393
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         50000 
_cell_measurement_theta_max        27.340
_cell_measurement_theta_min        3.788
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      1.940
_exptl_absorpt_correction_T_max    0.925
_exptl_absorpt_correction_T_min    0.634
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.05(2) GPa
 (50000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.862
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0521
_diffrn_reflns_av_unetI/netI       0.0405
_diffrn_reflns_Laue_measured_fraction_full  0.193
_diffrn_reflns_Laue_measured_fraction_max  0.163
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         7
_diffrn_reflns_limit_l_min         -7
_diffrn_reflns_number              2655
_diffrn_reflns_point_group_measured_fraction_full  0.193
_diffrn_reflns_point_group_measured_fraction_max  0.163
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.340
_diffrn_reflns_theta_min           3.788
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.193
_diffrn_measured_fraction_theta_max  0.163
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  393
_reflns_number_total               479
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.279
_refine_diff_density_min           -0.317
_refine_diff_density_rms           0.072
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.120
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           479
_refine_ls_number_restraints       132
_refine_ls_R_factor_all            0.0621
_refine_ls_R_factor_gt             0.0461
_refine_ls_restrained_S_all        0.950
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.1035P)²+1.0950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1208
_refine_ls_wR_factor_ref           0.1347
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O4-C4
 1.28 with sigma of 0.03
 C11-O11
 1.25 with sigma of 0.03
 O13-C14
 1.27 with sigma of 0.02
 O12-C11
 1.21 with sigma of 0.03
 N3-C3
 1.44 with sigma of 0.02
 C13-C12
 1.49 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq: with
sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7142(3) 0.3234(5) 0.5464(8) 0.028(2) Uani 1 1 d . U . . .
 O1 O 0.646(2) 0.346(4) 0.725(5) 0.028(3) Uani 1 1 d . U . . .
 O2 O 0.5698(18) 0.270(3) 0.890(5) 0.033(5) Uani 1 1 d . U . . .
 O14 O 1.1008(19) 0.753(3) 0.473(5) 0.033(3) Uani 1 1 d . U . . .
 O4 O 0.501(2) -0.120(3) 0.621(5) 0.044(4) Uani 1 1 d D U . . .
 O11 O 0.7272(19) 0.502(3) 0.498(5) 0.050(4) Uani 1 1 d D U . . .
 O1W O 0.229(3) 0.028(3) 0.773(5) 0.039(5) Uani 1 1 d . U . . .
 H1WA H 0.339706 0.090904 0.823655 0.058 Uiso 1 1 d G . . . .
 H1WB H 0.214100 -0.047681 0.682640 0.058 Uiso 1 1 d G . . . .
 O13 O 0.9263(17) 0.500(3) 0.238(4) 0.043(5) Uani 1 1 d D U . . .
 O3 O 0.5090(18) -0.161(3) 0.842(4) 0.043(5) Uani 1 1 d . U . . .
 O12 O 0.841(2) 0.727(4) 0.733(5) 0.043(7) Uani 1 1 d D U . . .
 O2W O 0.225(2) 0.318(4) 1.003(6) 0.066(6) Uani 1 1 d . U . . .
 H2WA H 0.247907 0.235171 0.963035 0.098 Uiso 1 1 d G . . . .
 H2WB H 0.176532 0.296431 1.061845 0.098 Uiso 1 1 d G . . . .
 N13 N 0.626(2) 0.523(4) 0.211(6) 0.030(5) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.778(2) 0.146(3) 1.042(5) 0.031(6) Uani 1 1 d D U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C1 C 0.655(3) 0.273(4) 0.807(7) 0.027(4) Uani 1 1 d . U . . .
 C4 C 0.564(2) -0.085(3) 0.770(5) 0.026(4) Uani 1 1 d D U . . .
 C14 C 0.949(2) 0.638(4) 0.351(5) 0.027(4) Uani 1 1 d D U . . .
 C11 C 0.786(3) 0.659(3) 0.586(5) 0.039(7) Uani 1 1 d D U . . .
 C12 C 0.787(2) 0.759(4) 0.494(6) 0.018(4) Uani 1 1 d D U . . .
 H12A H 0.679509 0.772511 0.473034 0.022 Uiso 1 1 calc R . . . .
 H12B H 0.886233 0.871361 0.564684 0.022 Uiso 1 1 calc R . . . .
 C13 C 0.799(2) 0.681(4) 0.337(6) 0.022(4) Uani 1 1 d D U . . .
 H13 H 0.815194 0.763133 0.298392 0.026 Uiso 1 1 calc R . . . .
 C2 C 0.786(3) 0.195(5) 0.815(7) 0.025(4) Uani 1 1 d . U . . .
 H2A H 0.779628 0.138528 0.707446 0.030 Uiso 1 1 calc R . . . .
 H2B H 0.905045 0.287191 0.886078 0.030 Uiso 1 1 calc R . . . .
 C3 C 0.754(2) 0.071(3) 0.876(5) 0.036(6) Uani 1 1 d D U . . .
 H3 H 0.840650 0.026723 0.869972 0.043 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.96(4) . ?
 Zn1 O14 1.993(14) 2_766 ?
 Zn1 O4 1.93(3) 2_656 ?
 Zn1 O11 1.909(9) . ?
 O1 C1 1.25(3) . ?
 O2 C1 1.25(4) . ?
 O14 C14 1.29(4) . ?
 O4 C4 1.28(4) . ?
 O11 C11 1.25(3) . ?
 O1W H1WA 0.8498 . ?
 O1W H1WB 0.8484 . ?
 O13 C14 1.27(2) . ?
 O3 C4 1.27(3) . ?
 O12 C11 1.21(4) . ?
 O2W H2WA 0.8476 . ?
 O2W H2WB 0.8501 . ?
 N13 H13A 0.8600 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.52(4) . ?
 N3 H3A 0.9100 . ?
 N3 H3B 0.9400 . ?
 N3 H3C 0.9100 . ?
 N3 C3 1.44(3) . ?
 C1 C2 1.54(2) . ?
 C4 C3 1.58(3) . ?
 C14 C13 1.49(2) . ?
 C11 C12 1.53(4) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.49(3) . ?
 C13 H13 0.9800 . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C3 1.49(3) . ?
 C3 H3 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 120.9(9) . 2_766 ?
 O4 Zn1 O1 95.6(10) 2_656 . ?
 O4 Zn1 O14 101.7(11) 2_656 2_766 ?
 O11 Zn1 O1 112.7(11) . . ?
 O11 Zn1 O14 114.2(6) . 2_766 ?
 O11 Zn1 O4 108.3(11) . 2_656 ?
 C1 O1 Zn1 130(2) . . ?
 C14 O14 Zn1 109(2) . 2_766 ?
 C4 O4 Zn1 122.7(11) . 2_656 ?
 C11 O11 Zn1 132(3) . . ?
 H1WA O1W H1WB 104.4 . . ?
 H2WA O2W H2WB 104.4 . . ?
 H13A N13 H13B 112.0 . . ?
 H13A N13 H13C 113.0 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 107.0 . . ?
 C13 N13 H13B 108.0 . . ?
 C13 N13 H13C 107.0 . . ?
 H3A N3 H3B 104.0 . . ?
 H3A N3 H3C 105.0 . . ?
 H3B N3 H3C 102.0 . . ?
 C3 N3 H3A 115.0 . . ?
 C3 N3 H3B 114.0 . . ?
 C3 N3 H3C 116.0 . . ?
 O1 C1 C2 119(3) . . ?
 O2 C1 O1 121.5(17) . . ?
 O2 C1 C2 120(2) . . ?
 O4 C4 C3 113(2) . . ?
 O3 C4 O4 132(2) . . ?
 O3 C4 C3 115(3) . . ?
 O14 C14 C13 116(3) . . ?
 O13 C14 O14 124.4(18) . . ?
 O13 C14 C13 119(2) . . ?
 O11 C11 C12 114(3) . . ?
 O12 C11 O11 123(3) . . ?
 O12 C11 C12 123(3) . . ?
 C11 C12 H12A 108.3 . . ?
 C11 C12 H12B 108.3 . . ?
 H12A C12 H12B 107.4 . . ?
 C13 C12 C11 116(2) . . ?
 C13 C12 H12A 108.3 . . ?
 C13 C12 H12B 108.3 . . ?
 N13 C13 H13 107.8 . . ?
 C14 C13 N13 110(2) . . ?
 C14 C13 C12 114(2) . . ?
 C14 C13 H13 107.8 . . ?
 C12 C13 N13 110(2) . . ?
 C12 C13 H13 107.8 . . ?
 C1 C2 H2A 108.6 . . ?
 C1 C2 H2B 108.6 . . ?
 H2A C2 H2B 107.5 . . ?
 C3 C2 C1 115(2) . . ?
 C3 C2 H2A 108.6 . . ?
 C3 C2 H2B 108.6 . . ?
 N3 C3 C4 107(2) . . ?
 N3 C3 C2 114(3) . . ?
 N3 C3 H3 107.4 . . ?
 C4 C3 H3 107.4 . . ?
 C2 C3 C4 113(3) . . ?
 C2 C3 H3 107.4 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 21(6) . . . . ?
 Zn1 O14 C14 C13 174.3(16) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -171.0(15) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 173.9(10) . . . . ?
 O2 C1 C2 C3 20(7) . . . . ?
 O12 C11 C12 C13 152(2) . . . . ?
 N13 C13 C14 O13 17(3) . . . . ?
 N3 C3 C4 O3 -31(2) . . . . ?
 C1 C2 C3 N3 -64(4) . . . . ?
 C1 C2 C3 C4 59(6) . . . . ?
 C11 C12 C13 N13 70.8(16) . . . . ?
 C11 C12 C13 C14 -52.7(17) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_0_15GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972162'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_0_15GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.192 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_0_15GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04667 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_dihydrate_0_15GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H2WA     .       1.98 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.7725(11)
_cell_length_b                     9.4694(14)
_cell_length_c                     9.803(3)
_cell_angle_alpha                  111.906(19)
_cell_angle_beta                   105.503(16)
_cell_angle_gamma                  107.777(12)
_cell_volume                       649.0(2)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      389 
_cell_measurement_temperature      296(2) 
_cell_measurement_pressure         150000 
_cell_measurement_theta_max        27.174
_cell_measurement_theta_min        3.798
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      1.949
_exptl_absorpt_correction_T_max    0.907
_exptl_absorpt_correction_T_min    0.633
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.15(2) GPa
 (150000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.871
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0684
_diffrn_reflns_av_unetI/netI       0.0539
_diffrn_reflns_Laue_measured_fraction_full  0.192
_diffrn_reflns_Laue_measured_fraction_max  0.164
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -10
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         7
_diffrn_reflns_limit_l_min         -7
_diffrn_reflns_number              2630
_diffrn_reflns_point_group_measured_fraction_full  0.192
_diffrn_reflns_point_group_measured_fraction_max  0.164
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.174
_diffrn_reflns_theta_min           3.798
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.192
_diffrn_measured_fraction_theta_max  0.164
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  389
_reflns_number_total               474
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.278
_refine_diff_density_min           -0.269
_refine_diff_density_rms           0.074
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.126
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           474
_refine_ls_number_restraints       132
_refine_ls_R_factor_all            0.0693
_refine_ls_R_factor_gt             0.0515
_refine_ls_restrained_S_all        0.966
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0808P)²+2.3162P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1102
_refine_ls_wR_factor_ref           0.1287
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O4-C4
 1.34 with sigma of 0.01
 O11-C11
 1.32 with sigma of 0.01
 O13-C14
 1.37 with sigma of 0.03
 O12-C11
 1.2 with sigma of 0.02
 N3-C3
 1.52 with sigma of 0.02
 C13-C12
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(N13) \\sim Ueq:
with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
Zn1 Zn 0.7133(3) 0.3224(4) 0.5446(7) 0.0281(19) Uani 1 1 d . U . . .
O1 O 0.642(2) 0.339(3) 0.713(5) 0.028(3) Uani 1 1 d . U . . .
O2 O 0.5696(16) 0.270(3) 0.886(4) 0.031(4) Uani 1 1 d . U . . .
O14 O 1.1038(18) 0.759(3) 0.481(4) 0.029(3) Uani 1 1 d . U . . .
O4 O 0.503(2) -0.120(3) 0.620(4) 0.043(4) Uani 1 1 d D U . . .
O11 O 0.7231(16) 0.496(2) 0.485(3) 0.047(3) Uani 1 1 d D U . . .
O1W O 0.228(2) 0.024(3) 0.767(4) 0.030(4) Uani 1 1 d . U . . .
H1WA H 0.3362 0.0949 0.8293 0.045 Uiso 1 1 d G . . . .
H1WB H 0.2302 -0.0545 0.6901 0.045 Uiso 1 1 d G . . . .
O13 O 0.9257(16) 0.500(3) 0.236(4) 0.036(4) Uani 1 1 d D U . . .
O3 O 0.5115(16) -0.161(3) 0.844(4) 0.043(4) Uani 1 1 d . U . . .
O12 O 0.841(2) 0.735(3) 0.738(4) 0.047(6) Uani 1 1 d D U . . .
O2W O 0.2233(19) 0.315(3) 0.999(5) 0.063(5) Uani 1 1 d . U . . .
H2WA H 0.2547 0.2434 0.9616 0.095 Uiso 1 1 d G . . . .
H2WB H 0.1757 0.2884 1.0585 0.095 Uiso 1 1 d G . . . .
N13 N 0.629(2) 0.525(4) 0.216(5) 0.032(4) Uani 1 1 d . U . . .
H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
N3 N 0.7811(19) 0.155(3) 1.054(5) 0.032(5) Uani 1 1 d D U . . .
H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
C1 C 0.656(2) 0.274(4) 0.808(6) 0.026(3) Uani 1 1 d . U . . .
C4 C 0.564(2) -0.083(3) 0.777(4) 0.026(4) Uani 1 1 d D U . . .
C14 C 0.956(2) 0.646(3) 0.365(5) 0.020(4) Uani 1 1 d D U . . .
C11 C 0.790(3) 0.659(3) 0.594(4) 0.038(7) Uani 1 1 d D U . . .
C12 C 0.7920(19) 0.768(3) 0.510(5) 0.025(4) Uani 1 1 d D U . . .
H12A H 0.8947 0.8786 0.5814 0.031 Uiso 1 1 calc R . . . .
H12B H 0.6868 0.7853 0.4942 0.031 Uiso 1 1 calc R U . . .
C13 C 0.7979(18) 0.686(3) 0.344(5) 0.022(4) Uani 1 1 d D U . . .
H13 H 0.8146 0.7691 0.3054 0.026 Uiso 1 1 calc R . . . .
C2 C 0.789(2) 0.202(4) 0.827(7) 0.026(3) Uani 1 1 d . U . . .
H2A H 0.7947 0.1536 0.7231 0.031 Uiso 1 1 calc R . . . .
H2B H 0.9048 0.2969 0.9054 0.031 Uiso 1 1 calc R . . . .
C3 C 0.756(2) 0.070(3) 0.878(5) 0.036(5) Uani 1 1 d D U . . .
H3 H 0.8429 0.0251 0.8723 0.044 Uiso 1 1 calc R . . . .
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.89(4) . ?
 Zn1 O14 2.013(15) 2_766 ?
 Zn1 O4 1.92(3) 2_656 ?
 Zn1 O11 1.924(10) . ?
 O1 C1 1.29(4) . ?
 O2 C1 1.22(4) . ?
 O14 C14 1.25(4) . ?
 O4 C4 1.344(13) . ?
 O11 C11 1.321(13) . ?
 O1W H1WA 0.8501 . ?
 O1W H1WB 0.8501 . ?
 O13 C14 1.37(3) . ?
 O3 C4 1.24(3) . ?
 O12 C11 1.20(3) . ?
 O2W H2WA 0.8101 . ?
 O2W H2WB 0.8726 . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.9100 . ?
 N13 H13C 0.8700 . ?
 N13 C13 1.51(5) . ?
 N3 H3A 0.8600 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.9100 . ?
 N3 C3 1.52(3) . ?
 C1 C2 1.520(19) . ?
 C4 C3 1.57(3) . ?
 C14 C13 1.53(2) . ?
 C11 C12 1.54(4) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.55(3) . ?
 C13 H13 0.9800 . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C3 1.50(3) . ?
 C3 H3 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 122.1(10) . 2_766 ?
 O1 Zn1 O4 93.3(11) . 2_656 ?
 O1 Zn1 O11 115.6(10) . . ?
 O4 Zn1 O14 101.2(11) 2_656 2_766 ?
 O11 Zn1 O14 113.1(6) . 2_766 ?
 O11 Zn1 O4 106.5(10) . 2_656 ?
 C1 O1 Zn1 133(2) . . ?
 C14 O14 Zn1 108(2) . 2_766 ?
 C4 O4 Zn1 121.2(12) . 2_656 ?
 C11 O11 Zn1 122.9(19) . . ?
 H1WA O1W H1WB 104.5 . . ?
 H2WA O2W H2WB 105.4 . . ?
 H13A N13 H13B 108.0 . . ?
 H13A N13 H13C 112.0 . . ?
 H13B N13 H13C 110.0 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 107.0 . . ?
 C13 N13 H13C 109.5 . . ?
 H3A N3 H3B 113.0 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 107.0 . . ?
 C3 N3 H3A 111.0 . . ?
 C3 N3 H3B 108.0 . . ?
 C3 N3 H3C 107.0 . . ?
 O1 C1 C2 119(3) . . ?
 O2 C1 O1 122.9(15) . . ?
 O2 C1 C2 118(3) . . ?
 O4 C4 C3 111(2) . . ?
 O3 C4 O4 132(2) . . ?
 O3 C4 C3 116(3) . . ?
 O14 C14 O13 126.3(19) . . ?
 O14 C14 C13 119(3) . . ?
 O13 C14 C13 114(3) . . ?
 O11 C11 C12 111(3) . . ?
 O12 C11 O11 134(3) . . ?
 O12 C11 C12 116(3) . . ?
 C11 C12 H12A 108.9 . . ?
 C11 C12 H12B 108.9 . . ?
 C11 C12 C13 113(2) . . ?
 H12A C12 H12B 107.7 . . ?
 C13 C12 H12A 108.9 . . ?
 C13 C12 H12B 108.9 . . ?
 N13 C13 C14 110(3) . . ?
 N13 C13 C12 113(2) . . ?
 N13 C13 H13 108.2 . . ?
 C14 C13 C12 110(3) . . ?
 C14 C13 H13 108.2 . . ?
 C12 C13 H13 108.2 . . ?
 C1 C2 H2A 107.8 . . ?
 C1 C2 H2B 107.8 . . ?
 H2A C2 H2B 107.1 . . ?
 C3 C2 C1 118.1(18) . . ?
 C3 C2 H2A 107.8 . . ?
 C3 C2 H2B 107.8 . . ?
 N3 C3 C4 106(2) . . ?
 N3 C3 H3 109.2 . . ?
 C4 C3 H3 109.2 . . ?
 C2 C3 N3 108(3) . . ?
 C2 C3 C4 114(3) . . ?
 C2 C3 H3 109.2 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 17(6) . . . . ?
 Zn1 O14 C14 C13 172.6(18) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -170.4(15) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 175.8(11) . . . . ?
 O2 C1 C2 C3 25(7) . . . . ?
 O12 C11 C12 C13 157(2) . . . . ?
 N13 C13 C14 O13 20(3) . . . . ?
 N3 C3 C4 O3 -37(3) . . . . ?
 C1 C2 C3 N3 -68(5) . . . . ?
 C1 C2 C3 C4 50(6) . . . . ?
 C11 C12 C13 N13 67.7(17) . . . . ?
 C11 C12 C13 C14 -54.9(17) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_0_40GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972163'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_0_40GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.192 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_0_40GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04667 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_dihydrate_0_40GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H3C      .       2.09 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.7385(18)
_cell_length_b                     9.419(3)
_cell_length_c                     9.773(6)
_cell_angle_alpha                  111.86(4)
_cell_angle_beta                   105.42(3)
_cell_angle_gamma                  107.88(2)
_cell_volume                       641.4(5)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      380
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         400000 
_cell_measurement_theta_max        27.319
_cell_measurement_theta_min        3.820
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      1.973
_exptl_absorpt_correction_T_max    0.906
_exptl_absorpt_correction_T_min    0.629
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.40(2) GPa
 (400000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.893
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0647
_diffrn_reflns_av_unetI/netI       0.0622
_diffrn_reflns_Laue_measured_fraction_full  0.192
_diffrn_reflns_Laue_measured_fraction_max  0.164
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         7
_diffrn_reflns_limit_l_min         -7
_diffrn_reflns_number              2596
_diffrn_reflns_point_group_measured_fraction_full  0.192
_diffrn_reflns_point_group_measured_fraction_max  0.164
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.319
_diffrn_reflns_theta_min           3.820
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.192
_diffrn_measured_fraction_theta_max  0.164
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  380
_reflns_number_total               475
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.196
_refine_diff_density_min           -0.172
_refine_diff_density_rms           0.048
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.102
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           475
_refine_ls_number_restraints       131
_refine_ls_R_factor_all            0.0570
_refine_ls_R_factor_gt             0.0399
_refine_ls_restrained_S_all        0.941
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0705P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0905
_refine_ls_wR_factor_ref           0.1023
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C11-O11
 1.38 with sigma of 0.02
 O12-C11
 1.22 with sigma of 0.03
 N3-C3
 1.45 with sigma of 0.03
 C12-C13
 1.53 with sigma of 0.03
 C4-O4
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(N13) \\sim Ueq: with
sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7121(2) 0.3223(4) 0.5440(6) 0.030(2) Uani 1 1 d . U . . .
 O1 O 0.6420(18) 0.341(3) 0.719(5) 0.030(3) Uani 1 1 d . U . . .
 O2 O 0.5713(15) 0.270(2) 0.887(4) 0.035(5) Uani 1 1 d . U . . .
 O14 O 1.1015(16) 0.753(3) 0.468(4) 0.034(3) Uani 1 1 d . U . . .
 O4 O 0.5021(19) -0.119(2) 0.622(4) 0.040(4) Uani 1 1 d D U . . .
 O11 O 0.7235(15) 0.499(2) 0.488(4) 0.051(3) Uani 1 1 d D U . . .
 O1W O 0.2286(16) 0.025(3) 0.768(4) 0.035(5) Uani 1 1 d . U . . .
 H1WA H 0.339724 0.079933 0.820061 0.053 Uiso 1 1 d G . . . .
 H1WB H 0.210666 -0.081387 0.719158 0.053 Uiso 1 1 d G . . . .
 O13 O 0.9266(17) 0.497(3) 0.234(4) 0.041(5) Uani 1 1 d . U . . .
 O3 O 0.5108(14) -0.162(2) 0.844(3) 0.040(5) Uani 1 1 d . U . . .
 O12 O 0.843(2) 0.736(3) 0.744(4) 0.055(7) Uani 1 1 d D U . . .
 O2W O 0.2232(17) 0.316(3) 0.999(4) 0.061(5) Uani 1 1 d . U . . .
 H2WA H 0.241624 0.231646 0.954198 0.092 Uiso 1 1 d G . . . .
 H2WB H 0.178228 0.294249 1.060455 0.092 Uiso 1 1 d G . . . .
 N13 N 0.6287(19) 0.527(3) 0.215(5) 0.031(5) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . . 
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . . 
 N3 N 0.782(2) 0.150(3) 1.049(4) 0.037(6) Uani 1 1 d D U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . . 
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . . 
 C1 C 0.657(2) 0.272(4) 0.804(6) 0.027(3) Uani 1 1 d . U . . .
 C4 C 0.5680(18) -0.082(2) 0.776(4) 0.020(4) Uani 1 1 d D U . . .
 C14 C 0.954(2) 0.641(4) 0.356(6) 0.024(4) Uani 1 1 d . U . . .
 C11 C 0.791(2) 0.668(3) 0.601(4) 0.026(5) Uani 1 1 d D U . . .
 C12 C 0.7926(19) 0.769(3) 0.507(5) 0.021(4) Uani 1 1 d D U . . .
 H12A H 0.686910 0.786221 0.489467 0.026 Uiso 1 1 calc R . . . .
 H12B H 0.894885 0.880918 0.577071 0.026 Uiso 1 1 calc R . . . .
 C13 C 0.7993(19) 0.688(3) 0.343(5) 0.024(4) Uani 1 1 d D U . . .
 H13 H 0.816513 0.772171 0.304841 0.028 Uiso 1 1 calc R . . . .
 C2 C 0.788(2) 0.197(4) 0.813(6) 0.029(4) Uani 1 1 d . U . . .
 H2A H 0.907599 0.290114 0.880855 0.034 Uiso 1 1 calc R . . . .
 H2B H 0.779190 0.135875 0.704233 0.034 Uiso 1 1 calc R . . . .
 C3 C 0.758(2) 0.074(3) 0.882(5) 0.031(5) Uani 1 1 d D U . . .
 H3 H 0.844860 0.028019 0.876720 0.037 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.93(3) . ?
 Zn1 O14 1.978(11) 2_766 ?
 Zn1 O4 1.92(2) 2_656 ?
 Zn1 O11 1.922(8) . ?
 O1 C1 1.24(3) . ?
 O2 C1 1.24(3) . ?
 O14 C14 1.24(4) . ?
 O4 C4 1.32(2) . ?
 O11 C11 1.36(2) . ?
 O1W H1WA 0.8387 . ?
 O1W H1WB 0.8734 . ?
 O13 C14 1.32(5) . ?
 O3 C4 1.251(19) . ?
 O12 C11 1.18(3) . ?
 O2W H2WA 0.8413 . ?
 O2W H2WB 0.8471 . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.52(4) . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.45(4) . ?
 C1 C2 1.520(17) . ?
 C4 C3 1.56(3) . ?
 C14 C13 1.535(18) . ?
 C11 C12 1.55(3) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.53(3) . ?
 C13 H13 0.9800 . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C3 1.53(2) . ?
 C3 H3 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 119.1(9) . 2_766 ?
 O4 Zn1 O1 94.9(9) 2_656 . ?
 O4 Zn1 O14 102.6(9) 2_656 2_766 ?
 O4 Zn1 O11 107.0(8) 2_656 . ?
 O11 Zn1 O1 114.7(8) . . ?
 O11 Zn1 O14 114.6(5) . 2_766 ?
 C1 O1 Zn1 129.8(19) . . ?
 C14 O14 Zn1 111.2(19) . 2_766 ?
 C4 O4 Zn1 122.8(9) . 2_656 ?
 C11 O11 Zn1 123.3(17) . . ?
 H1WA O1W H1WB 102.9 . . ?
 H2WA O2W H2WB 104.6 . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 108.0 . . ?
 C13 N13 H13C 109.5 . . ?
 H3A N3 H3B 108.0 . . ?
 H3A N3 H3C 106.0 . . ?
 H3B N3 H3C 107.0 . . ?
 C3 N3 H3A 112.0 . . ?
 C3 N3 H3B 111.0 . . ?
 C3 N3 H3C 112.0 . . ?
 O1 C1 O2 120.5(14) . . ?
 O1 C1 C2 120(2) . . ?
 O2 C1 C2 120(2) . . ?
 O4 C4 C3 112.9(17) . . ?
 O3 C4 O4 130.2(18) . . ?
 O3 C4 C3 116(2) . . ?
 O14 C14 O13 124.4(15) . . ?
 O14 C14 C13 117(3) . . ?
 O13 C14 C13 118(3) . . ?
 O11 C11 C12 107(2) . . ?
 O12 C11 O11 131(2) . . ?
 O12 C11 C12 122(2) . . ?
 C11 C12 H12A 108.0 . . ?
 C11 C12 H12B 108.0 . . ?
 H12A C12 H12B 107.3 . . ?
 C13 C12 C11 117.1(19) . . ?
 C13 C12 H12A 108.0 . . ?
 C13 C12 H12B 108.0 . . ?
 N13 C13 C14 108(2) . . ?
 N13 C13 C12 112.2(17) . . ?
 N13 C13 H13 108.3 . . ?
 C14 C13 H13 108.3 . . ?
 C12 C13 C14 112(3) . . ?
 C12 C13 H13 108.3 . . ?
 C1 C2 H2A 108.7 . . ?
 C1 C2 H2B 108.7 . . ?
 C1 C2 C3 114.2(17) . . ?
 H2A C2 H2B 107.6 . . ?
 C3 C2 H2A 108.7 . . ?
 C3 C2 H2B 108.7 . . ?
 N3 C3 C4 107.3(19) . . ?
 N3 C3 C2 115(3) . . ?
 N3 C3 H3 107.5 . . ?
 C4 C3 H3 107.5 . . ?
 C2 C3 C4 111(2) . . ?
 C2 C3 H3 107.5 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 19(5) . . . . ?
 Zn1 O14 C14 C13 175.3(18) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -170.8(12) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 174.5(8) . . . . ?
 O2 C1 C2 C3 19(5) . . . . ?
 O12 C11 C12 C13 155(2) . . . . ?
 N13 C13 C14 O13 18(3) . . . . ?
 N3 C3 C4 O3 -33(2) . . . . ?
 C1 C2 C3 N3 -63(4) . . . . ?
 C1 C2 C3 C4 59(4) . . . . ?
 C11 C12 C13 N13 68.2(15) . . . . ?
 C11 C12 C13 C14 -52.9(17) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_0_70GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972164'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_0_70GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.194 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_0_70GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04667 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_dihydrate_0_70GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H2WA     .       2.09 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.687(4)
_cell_length_b                     9.359(3)
_cell_length_c                     9.7666(19)
_cell_angle_alpha                  111.78(3)
_cell_angle_beta                   105.20(3)
_cell_angle_gamma                  108.04(4)
_cell_volume                       633.9(4)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      380
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         50000 
_cell_measurement_theta_max        27.490
_cell_measurement_theta_min        3.851
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      1.996
_exptl_absorpt_correction_T_max    0.923
_exptl_absorpt_correction_T_min    0.626
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 0.70(2) GPa
 (700000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.915
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0624
_diffrn_reflns_av_unetI/netI       0.0602
_diffrn_reflns_Laue_measured_fraction_full  0.194
_diffrn_reflns_Laue_measured_fraction_max  0.163
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         7
_diffrn_reflns_limit_l_min         -7
_diffrn_reflns_number              2494
_diffrn_reflns_point_group_measured_fraction_full  0.194
_diffrn_reflns_point_group_measured_fraction_max  0.163
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.490
_diffrn_reflns_theta_min           3.851
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.194
_diffrn_measured_fraction_theta_max  0.163
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  380
_reflns_number_total               470
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.199
_refine_diff_density_min           -0.174
_refine_diff_density_rms           0.049
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.100
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           470
_refine_ls_number_restraints       131
_refine_ls_R_factor_all            0.0569
_refine_ls_R_factor_gt             0.0398
_refine_ls_restrained_S_all        0.941
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0703P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0903
_refine_ls_wR_factor_ref           0.1021
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C11-O11
 1.38 with sigma of 0.02
 O12-C11
 1.22 with sigma of 0.03
 N3-C3
 1.45 with sigma of 0.03
 C12-C13
 1.53 with sigma of 0.03
 C4-O4
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(N13) \\sim Ueq: with
sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7121(2) 0.3223(4) 0.5440(6) 0.029(2) Uani 1 1 d . U . . .
 O1 O 0.6421(18) 0.341(3) 0.719(5) 0.029(3) Uani 1 1 d . U . . .
 O2 O 0.5714(15) 0.270(2) 0.887(4) 0.034(5) Uani 1 1 d . U . . .
 O14 O 1.1015(16) 0.753(3) 0.469(4) 0.034(3) Uani 1 1 d . U . . .
 O4 O 0.5021(18) -0.120(2) 0.622(4) 0.039(4) Uani 1 1 d D U . . .
 O11 O 0.7234(15) 0.499(2) 0.488(4) 0.050(3) Uani 1 1 d D U . . .
 O1W O 0.2287(16) 0.025(3) 0.768(4) 0.034(5) Uani 1 1 d . U . . .
 H1WA H 0.339886 0.079936 0.819928 0.052 Uiso 1 1 d G . . . .
 H1WB H 0.210615 -0.080955 0.717181 0.052 Uiso 1 1 d G . . . .
 O13 O 0.9266(17) 0.497(3) 0.235(4) 0.040(5) Uani 1 1 d . U . . .
 O3 O 0.5108(14) -0.162(2) 0.844(3) 0.040(5) Uani 1 1 d . U . . .
 O12 O 0.843(2) 0.736(3) 0.744(4) 0.053(7) Uani 1 1 d D U . . .
 O2W O 0.2233(17) 0.316(3) 0.999(4) 0.060(5) Uani 1 1 d . U . . .
 H2WA H 0.240366 0.229198 0.953232 0.090 Uiso 1 1 d G . . . .
 H2WB H 0.178022 0.294565 1.061132 0.090 Uiso 1 1 d G . . . .
 N13 N 0.6285(19) 0.527(3) 0.214(5) 0.030(5) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.782(2) 0.150(3) 1.050(4) 0.036(6) Uani 1 1 d D U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C1 C 0.657(2) 0.272(4) 0.804(6) 0.026(3) Uani 1 1 d . U . . .
 C4 C 0.5678(18) -0.083(2) 0.776(4) 0.020(4) Uani 1 1 d D U . . .
 C14 C 0.954(2) 0.641(4) 0.355(6) 0.023(4) Uani 1 1 d . U . . .
 C11 C 0.791(2) 0.668(3) 0.601(4) 0.026(5) Uani 1 1 d D U . . .
 C12 C 0.7927(19) 0.769(3) 0.508(5) 0.021(4) Uani 1 1 d D U . . .
 H12A H 0.686522 0.786685 0.490410 0.025 Uiso 1 1 calc R . . . .
 H12B H 0.895539 0.881955 0.577242 0.025 Uiso 1 1 calc R . . . .
 C13 C 0.7995(19) 0.689(3) 0.344(5) 0.023(4) Uani 1 1 d D U . . .
 H13 H 0.817634 0.773778 0.306041 0.028 Uiso 1 1 calc R . . . .
 C2 C 0.788(2) 0.197(4) 0.813(6) 0.028(3) Uani 1 1 d . U . . .
 H2A H 0.908190 0.290835 0.880102 0.034 Uiso 1 1 calc R . . . .
 H2B H 0.779127 0.135154 0.704223 0.034 Uiso 1 1 calc R . . . .
 C3 C 0.758(2) 0.074(3) 0.882(5) 0.030(5) Uani 1 1 d D U . . .
 H3 H 0.845445 0.028127 0.877040 0.036 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.93(3) . ?
 Zn1 O14 1.968(11) 2_766 ?
 Zn1 O4 1.91(2) 2_656 ?
 Zn1 O11 1.911(8) . ?
 O1 C1 1.23(3) . ?
 O2 C1 1.24(3) . ?
 O14 C14 1.24(4) . ?
 O4 C4 1.32(2) . ?
 O11 C11 1.36(2) . ?
 O1W H1WA 0.8347 . ?
 O1W H1WB 0.8685 . ?
 O13 C14 1.32(5) . ?
 O3 C4 1.244(19) . ?
 O12 C11 1.18(3) . ?
 O2W H2WA 0.8502 . ?
 O2W H2WB 0.8499 . ?
 N13 H13A 0.8700 . ?
 N13 H13B 0.8900 . ?
 N13 H13C 0.8900 . ?
 N13 C13 1.52(4) . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.45(4) . ?
 C1 C2 1.512(2) . ?
 C4 C3 1.56(3) . ?
 C14 C13 1.529(2) . ?
 C11 C12 1.54(3) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.520(3) . ?
 C13 H13 0.9800 . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C3 1.530(2) . ?
 C3 H3 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 119.0(9) . 2_766 ?
 O4 Zn1 O1 95.4(8) 2_656 . ?
 O4 Zn1 O14 102.5(9) 2_656 2_766 ?
 O4 Zn1 O11 106.5(8) 2_656 . ?
 O11 Zn1 O1 114.8(8) . . ?
 O11 Zn1 O14 114.7(5) . 2_766 ?
 C1 O1 Zn1 129.8(19) . . ?
 C14 O14 Zn1 111.0(19) . 2_766 ?
 C4 O4 Zn1 123.1(9) . 2_656 ?
 C11 O11 Zn1 122.7(17) . . ?
 H1WA O1W H1WB 102.9 . . ?
 H2WA O2W H2WB 104.4 . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 111.0 . . ?
 C13 N13 H13B 108.0 . . ?
 C13 N13 H13C 108.0 . . ?
 H3A N3 H3B 108.0 . . ?
 H3A N3 H3C 107.0 . . ?
 H3B N3 H3C 107.0 . . ?
 C3 N3 H3A 111.0 . . ?
 C3 N3 H3B 111.0 . . ?
 C3 N3 H3C 112.0 . . ?
 O1 C1 O2 120.6(14) . . ?
 O1 C1 C2 120(2) . . ?
 O2 C1 C2 120(2) . . ?
 O4 C4 C3 113.4(17) . . ?
 O3 C4 O4 130.5(18) . . ?
 O3 C4 C3 116(2) . . ?
 O14 C14 O13 124.6(15) . . ?
 O14 C14 C13 116(3) . . ?
 O13 C14 C13 118(3) . . ?
 O11 C11 C12 106(2) . . ?
 O12 C11 O11 131(2) . . ?
 O12 C11 C12 122(2) . . ?
 C11 C12 H12A 108.0 . . ?
 C11 C12 H12B 108.0 . . ?
 H12A C12 H12B 107.2 . . ?
 C13 C12 C11 117.3(19) . . ?
 C13 C12 H12A 108.0 . . ?
 C13 C12 H12B 108.0 . . ?
 N13 C13 C14 107(2) . . ?
 N13 C13 C12 112.8(17) . . ?
 N13 C13 H13 108.2 . . ?
 C14 C13 H13 108.2 . . ?
 C12 C13 C14 112(3) . . ?
 C12 C13 H13 108.2 . . ?
 C1 C2 H2A 108.7 . . ?
 C1 C2 H2B 108.7 . . ?
 C1 C2 C3 114.2(17) . . ?
 H2A C2 H2B 107.6 . . ?
 C3 C2 H2A 108.7 . . ?
 C3 C2 H2B 108.7 . . ?
 N3 C3 C4 107.9(19) . . ?
 N3 C3 C2 116(3) . . ?
 N3 C3 H3 107.4 . . ?
 C4 C3 H3 107.4 . . ?
 C2 C3 C4 111(2) . . ?
 C2 C3 H3 107.4 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O2 C1 C2 C3 19(5) . . . . ?
 O12 C11 C12 C13 155(2) . . . . ?
 N13 C13 C14 O13 18(3) . . . . ?
 N3 C3 C4 O3 -33(2) . . . . ?
 C1 C2 C3 N3 -63(4) . . . . ?
 C1 C2 C3 C4 60(4) . . . . ?
 C11 C12 C13 N13 68.5(15) . . . . ?
 C11 C12 C13 C14 -52.8(17) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_1_02GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972165'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_1_02GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.192 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_1_02GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.05 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_dihydrate_1_02GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H2WA     .       2.05 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.668(4)
_cell_length_b                     9.308(4)
_cell_length_c                     9.738(3)
_cell_angle_alpha                  111.52(3)
_cell_angle_beta                   105.23(3)
_cell_angle_gamma                  108.10(4)
_cell_volume                       628.5(5)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      325
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         1020000 
_cell_measurement_theta_max        27.072
_cell_measurement_theta_min        3.868
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.013
_exptl_absorpt_correction_T_max    0.904
_exptl_absorpt_correction_T_min    0.623
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 1.02(2) GPa
 (1020000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.932
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1072
_diffrn_reflns_av_unetI/netI       0.0830
_diffrn_reflns_Laue_measured_fraction_full  0.192
_diffrn_reflns_Laue_measured_fraction_max  0.166
_diffrn_reflns_limit_h_max         4
_diffrn_reflns_limit_h_min         -4
_diffrn_reflns_limit_k_max         9
_diffrn_reflns_limit_k_min         -9
_diffrn_reflns_limit_l_max         12
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              2540
_diffrn_reflns_point_group_measured_fraction_full  0.192
_diffrn_reflns_point_group_measured_fraction_max  0.166
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.072
_diffrn_reflns_theta_min           3.868
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.192
_diffrn_measured_fraction_theta_max  0.166
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  325
_reflns_number_total               461
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.264
_refine_diff_density_min           -0.395
_refine_diff_density_rms           0.069
_refine_ls_goodness_of_fit_ref     1.107
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       199
_refine_ls_number_reflns           461
_refine_ls_number_restraints       139
_refine_ls_R_factor_all            0.0913
_refine_ls_R_factor_gt             0.0534
_refine_ls_restrained_S_all        0.926
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0402P)²+6.9565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1052
_refine_ls_wR_factor_ref           0.1387
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C13-C12 = C13-C14
 1.5 with sigma of 0.05
 C14-O14
 1.21 with sigma of 0.03
 C14-O13
 1.38 with sigma of 0.03
 C14-C13
 1.51 with sigma of 0.03
 C1-C2 = C3-C2
 1.5 with sigma of 0.05
 C1-O2
 1.2 with sigma of 0.03
 C3-C1
 2.56 with sigma of 0.01
 C4-C2
 2.56 with sigma of 0.01
 C4-C1
 3.06 with sigma of 0.01
 C11-C13
 2.6 with sigma of 0.01
 C12-C14
 2.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N13) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O1W) \\sim Ueq:
with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7053(17) 0.3217(6) 0.5392(3) 0.041(3) Uani 1 1 d . U . . .
 O1 O 0.638(6) 0.342(2) 0.7190(16) 0.048(5) Uani 1 1 d . U . . .
 O2 O 0.581(4) 0.276(2) 0.9004(15) 0.046(7) Uani 1 1 d D U . . .
 O14 O 1.095(7) 0.757(3) 0.466(2) 0.037(7) Uani 1 1 d D U . . .
 O4 O 0.504(5) -0.114(2) 0.6331(14) 0.039(5) Uani 1 1 d . U . . .
 O11 O 0.711(7) 0.508(3) 0.4925(14) 0.032(5) Uani 1 1 d . U . . .
 O1W O 0.244(6) 0.027(2) 0.7768(16) 0.040(7) Uani 1 1 d . U . . .
 H1WA H 0.349293 0.119518 0.832847 0.060 Uiso 1 1 d G . . . .
 H1WB H 0.243468 -0.025443 0.683768 0.060 Uiso 1 1 d G . . . .
 O13 O 0.949(6) 0.501(2) 0.2512(17) 0.052(8) Uani 1 1 d D U . . .
 O3 O 0.510(5) -0.164(2) 0.8426(14) 0.038(7) Uani 1 1 d . U . . .
 O12 O 0.838(6) 0.732(2) 0.7369(15) 0.043(7) Uani 1 1 d . U . . .
 O2W O 0.226(6) 0.320(3) 1.0042(19) 0.053(8) Uani 1 1 d . U . . .
 H2WA H 0.232398 0.224308 0.972901 0.080 Uiso 1 1 d G . . . .
 H2WB H 0.229006 0.346346 1.098466 0.080 Uiso 1 1 d G . . . .
 N13 N 0.634(9) 0.539(4) 0.213(2) 0.045(8) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.780(7) 0.155(3) 1.0551(19) 0.041(8) Uani 1 1 d . U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C4 C 0.588(7) -0.084(2) 0.780(2) 0.034(6) Uani 1 1 d D U . . .
 C13 C 0.797(6) 0.690(3) 0.337(2) 0.032(9) Uani 1 1 d D U . . .
 H13 H 0.818294 0.774433 0.298743 0.038 Uiso 1 1 calc R . . . .
 C11 C 0.775(9) 0.668(3) 0.590(2) 0.040(7) Uani 1 1 d D U . . .
 C12 C 0.792(5) 0.777(2) 0.5024(18) 0.031(6) Uani 1 1 d D U . . .
 H12A H 0.691699 0.804107 0.486358 0.038 Uiso 1 1 calc R . . . .
 H12B H 0.900949 0.885359 0.573198 0.038 Uiso 1 1 calc R . . . .
 C14 C 0.951(5) 0.644(3) 0.355(3) 0.040(10) Uani 1 1 d D U . . .
 C3 C 0.767(5) 0.073(2) 0.8880(18) 0.035(6) Uani 1 1 d D U . . .
 H3 H 0.860409 0.034959 0.891169 0.042 Uiso 1 1 calc R . . . .
 C2 C 0.802(7) 0.208(3) 0.827(3) 0.041(9) Uani 1 1 d D U . . .
 H2A H 0.920053 0.305139 0.901399 0.049 Uiso 1 1 calc R . . . .
 H2B H 0.800767 0.155444 0.720483 0.049 Uiso 1 1 calc R . . . .
 C1 C 0.661(5) 0.275(3) 0.817(3) 0.026(8) Uani 1 1 d D U . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.95(3) . ?
 Zn1 O14 2.08(6) 2_766 ?
 Zn1 O4 1.920(19) 2_656 ?
 Zn1 O11 1.93(4) . ?
 O1 C1 1.33(4) . ?
 O2 C1 1.20(3) . ?
 O14 C14 1.21(3) . ?
 O4 C4 1.30(4) . ?
 O11 C11 1.26(4) . ?
 O1W H1WA 0.8798 . ?
 O1W H1WB 0.8543 . ?
 O13 C14 1.34(3) . ?
 O3 C4 1.27(2) . ?
 O12 C11 1.21(2) . ?
 O2W H2WA 0.8500 . ?
 O2W H2WB 0.8499 . ?
 N13 H13A 0.8600 . ?
 N13 H13B 0.8600 . ?
 N13 H13C 0.9900 . ?
 N13 C13 1.43(4) . ?
 N3 H3A 0.8400 . ?
 N3 H3B 0.8900 . ?
 N3 H3C 0.8900 . ?
 N3 C3 1.48(3) . ?
 C4 C3 1.50(3) . ?
 C13 H13 0.9800 . ?
 C13 C12 1.53(2) . ?
 C13 C14 1.51(3) . ?
 C11 C12 1.54(3) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.56(3) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C1 1.53(6) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 116.3(18) . 2_766 ?
 O4 Zn1 O1 98.5(10) 2_656 . ?
 O4 Zn1 O14 100.9(16) 2_656 2_766 ?
 O4 Zn1 O11 107.7(16) 2_656 . ?
 O11 Zn1 O1 111(2) . . ?
 O11 Zn1 O14 119(2) . 2_766 ?
 C1 O1 Zn1 131(4) . . ?
 C14 O14 Zn1 111(3) . 2_766 ?
 C4 O4 Zn1 126.2(10) . 2_656 ?
 C11 O11 Zn1 129(2) . . ?
 H1WA O1W H1WB 103.9 . . ?
 H2WA O2W H2WB 104.5 . . ?
 H13A N13 H13B 113.0 . . ?
 H13A N13 H13C 102.0 . . ?
 H13B N13 H13C 101.0 . . ?
 C13 N13 H13A 116.0 . . ?
 C13 N13 H13B 114.0 . . ?
 C13 N13 H13C 109.5 . . ?
 H3A N3 H3B 113.0 . . ?
 H3A N3 H3C 111.0 . . ?
 H3B N3 H3C 107.0 . . ?
 C3 N3 H3A 114.0 . . ?
 C3 N3 H3B 105.0 . . ?
 C3 N3 H3C 106.0 . . ?
 O4 C4 C3 117.8(13) . . ?
 O3 C4 O4 122(3) . . ?
 O3 C4 C3 119.4(18) . . ?
 N13 C13 H13 107.2 . . ?
 N13 C13 C12 115(3) . . ?
 N13 C13 C14 109(4) . . ?
 C12 C13 H13 107.2 . . ?
 C14 C13 H13 107.2 . . ?
 C14 C13 C12 110.8(17) . . ?
 O11 C11 C12 112.5(13) . . ?
 O12 C11 O11 124(3) . . ?
 O12 C11 C12 122(2) . . ?
 C13 C12 C11 115(2) . . ?
 C13 C12 H12A 108.6 . . ?
 C13 C12 H12B 108.6 . . ?
 C11 C12 H12A 108.6 . . ?
 C11 C12 H12B 108.6 . . ?
 H12A C12 H12B 107.6 . . ?
 O14 C14 O13 117(4) . . ?
 O14 C14 C13 116(4) . . ?
 O13 C14 C13 126(3) . . ?
 N3 C3 C4 109(2) . . ?
 N3 C3 H3 108.0 . . ?
 N3 C3 C2 110(2) . . ?
 C4 C3 H3 108.0 . . ?
 C4 C3 C2 113.7(19) . . ?
 C2 C3 H3 108.0 . . ?
 C3 C2 H2A 109.3 . . ?
 C3 C2 H2B 109.3 . . ?
 H2A C2 H2B 107.9 . . ?
 C1 C2 C3 112(3) . . ?
 C1 C2 H2A 109.3 . . ?
 C1 C2 H2B 109.3 . . ?
 O1 C1 C2 117(3) . . ?
 O2 C1 O1 121(4) . . ?
 O2 C1 C2 122(3) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 18(3) . . . . ?
 Zn1 O14 C14 C13 175.6(15) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -169(3) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 167(4) . . . . ?
 O2 C1 C2 C3 26(3) . . . . ?
 O12 C11 C12 C13 150(6) . . . . ?
 N13 C13 C14 O13 14(3) . . . . ?
 N3 C3 C4 O3 -27(5) . . . . ?
 C11 C12 C13 N13 66(5) . . . . ?
 C11 C12 C13 C14 -58(4) . . . . ?
 C1 C2 C3 N3 -63(4) . . . . ?
 C1 C2 C3 C4 60(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_1_54GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972166'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_1_54GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.194 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_1_54GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.045 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
_vrf_PLAT417_zinc-aspartate_dihydrate_1_54GPa
;
PROBLEM: Short Inter D-H..H-D       H1WA     ..H2WA     .       2.05 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form

_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.594(4)
_cell_length_b                     9.235(3)
_cell_length_c                     9.6951(16)
_cell_angle_alpha                  111.39(2)
_cell_angle_beta                   104.94(2)
_cell_angle_gamma                  108.42(3)
_cell_volume                       616.2(4)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      314
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         1540000 
_cell_measurement_theta_max        26.694
_cell_measurement_theta_min        3.915
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.053
_exptl_absorpt_correction_T_max    0.902
_exptl_absorpt_correction_T_min    0.617
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 1.54(2) GPa
 (1540000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      1.971
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1148
_diffrn_reflns_av_unetI/netI       0.0835
_diffrn_reflns_Laue_measured_fraction_full  0.194
_diffrn_reflns_Laue_measured_fraction_max  0.175
_diffrn_reflns_limit_h_max         4
_diffrn_reflns_limit_h_min         -4
_diffrn_reflns_limit_k_max         9
_diffrn_reflns_limit_k_min         -9
_diffrn_reflns_limit_l_max         12
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              2559
_diffrn_reflns_point_group_measured_fraction_full  0.194
_diffrn_reflns_point_group_measured_fraction_max  0.175
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.694
_diffrn_reflns_theta_min           3.915
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.194
_diffrn_measured_fraction_theta_max  0.175
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  314
_reflns_number_total               458
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.248
_refine_diff_density_min           -0.263
_refine_diff_density_rms           0.067
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.119
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           458
_refine_ls_number_restraints       136
_refine_ls_R_factor_all            0.0874
_refine_ls_R_factor_gt             0.0491
_refine_ls_restrained_S_all        0.937
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0615P)²+3.7775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1078
_refine_ls_wR_factor_ref           0.1421
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C2-C1
 1.52 with sigma of 0.02
 C1-O2
 1.24 with sigma of 0.02
 C14-O14
 1.24 with sigma of 0.02
 C14-O13
 1.33 with sigma of 0.03
 C14-C13
 1.52 with sigma of 0.03
 C4-C2
 2.55 with sigma of 0.01
 C3-C1
 2.56 with sigma of 0.01
 C11-C13
 2.6 with sigma of 0.01
 C12-C14
 2.51 with sigma of 0.01
 C4-N3
 2.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O4) \\sim Ueq,
Uanis(O3) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq:
with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.7017(16) 0.3212(6) 0.5364(3) 0.036(3) Uani 1 1 d . U . . .
 O1 O 0.636(5) 0.342(2) 0.7185(14) 0.040(5) Uani 1 1 d . U . . .
 O2 O 0.580(4) 0.2784(18) 0.9021(13) 0.036(7) Uani 1 1 d D U . . .
 O14 O 1.087(6) 0.760(3) 0.4713(18) 0.038(7) Uani 1 1 d D U . . .
 O4 O 0.504(5) -0.1102(19) 0.6355(13) 0.036(5) Uani 1 1 d . U . . .
 O11 O 0.711(6) 0.508(2) 0.4911(13) 0.032(5) Uani 1 1 d . U . . .
 O1W O 0.245(6) 0.029(2) 0.7768(14) 0.040(7) Uani 1 1 d . U . . .
 H1WA H 0.345785 0.121739 0.812882 0.060 Uiso 1 1 d G . . . .
 H1WB H 0.251170 -0.051045 0.702144 0.060 Uiso 1 1 d G . . . .
 O13 O 0.945(5) 0.506(3) 0.2532(18) 0.055(8) Uani 1 1 d D U . . .
 O3 O 0.514(5) -0.1650(18) 0.8437(13) 0.038(7) Uani 1 1 d . U . . .
 O12 O 0.834(5) 0.734(2) 0.7368(14) 0.040(7) Uani 1 1 d . U . . .
 O2W O 0.224(6) 0.321(2) 1.0072(15) 0.043(8) Uani 1 1 d . U . . .
 H2WA H 0.242281 0.236081 0.963754 0.065 Uiso 1 1 d G . . . .
 H2WB H 0.218624 0.329127 1.089515 0.065 Uiso 1 1 d G . . . .
 N13 N 0.641(8) 0.537(3) 0.2115(19) 0.033(7) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.790(6) 0.156(3) 1.0600(14) 0.038(7) Uani 1 1 d D U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C2 C 0.805(5) 0.213(3) 0.833(3) 0.040(9) Uani 1 1 d D U . . .
 H2A H 0.922178 0.312603 0.910182 0.048 Uiso 1 1 calc R . . . .
 H2B H 0.810741 0.162296 0.728518 0.048 Uiso 1 1 calc R . . . .
 C4 C 0.601(11) -0.085(4) 0.7873(18) 0.034(6) Uani 1 1 d D U . . .
 C14 C 0.945(4) 0.646(3) 0.353(2) 0.030(9) Uani 1 1 d D U . . .
 C11 C 0.765(8) 0.675(3) 0.590(2) 0.035(6) Uani 1 1 d D U . . .
 C12 C 0.787(5) 0.780(2) 0.5025(17) 0.027(6) Uani 1 1 d D U . . .
 H12A H 0.897622 0.888609 0.574246 0.033 Uiso 1 1 calc R . . . .
 H12B H 0.687663 0.810572 0.486762 0.033 Uiso 1 1 calc R . . . .
 C13 C 0.793(6) 0.697(3) 0.337(2) 0.035(9) Uani 1 1 d D U . . .
 H13 H 0.813820 0.781970 0.297877 0.042 Uiso 1 1 calc R . . . .
 C1 C 0.662(4) 0.277(3) 0.815(2) 0.022(7) Uani 1 1 d D U . . .
 C3 C 0.772(5) 0.078(2) 0.8915(18) 0.039(6) Uani 1 1 d D U . . .
 H3 H 0.868910 0.043949 0.893936 0.047 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.95(2) . ?
 Zn1 O14 2.18(6) 2_766 ?
 Zn1 O4 1.907(16) 2_656 ?
 Zn1 O11 1.91(4) . ?
 O1 C1 1.29(4) . ?
 O2 C1 1.23(2) . ?
 O14 C14 1.22(2) . ?
 O4 C4 1.38(5) . ?
 O11 C11 1.33(4) . ?
 O1W H1WA 0.8702 . ?
 O1W H1WB 0.8516 . ?
 O13 C14 1.30(3) . ?
 O3 C4 1.25(3) . ?
 O12 C11 1.22(2) . ?
 O2W H2WA 0.8293 . ?
 O2W H2WB 0.7900 . ?
 N13 H13A 0.8100 . ?
 N13 H13B 0.9200 . ?
 N13 H13C 0.9800 . ?
 N13 C13 1.42(3) . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8100 . ?
 N3 H3C 0.8600 . ?
 N3 C3 1.47(3) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C1 1.52(3) . ?
 C2 C3 1.53(2) . ?
 C4 C3 1.47(4) . ?
 C14 C13 1.52(4) . ?
 C11 C12 1.50(3) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.53(2) . ?
 C13 H13 0.9800 . ?
 C3 H3 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 116.4(16) . 2_766 ?
 O4 Zn1 O1 99.6(10) 2_656 . ?
 O4 Zn1 O14 99.6(15) 2_656 2_766 ?
 O4 Zn1 O11 109.1(15) 2_656 . ?
 O11 Zn1 O1 111.7(19) . . ?
 O11 Zn1 O14 117.7(19) . 2_766 ?
 C1 O1 Zn1 131(4) . . ?
 C14 O14 Zn1 108(3) . 2_766 ?
 C4 O4 Zn1 125.2(10) . 2_656 ?
 C11 O11 Zn1 131.3(14) . . ?
 H1WA O1W H1WB 104.0 . . ?
 H2WA O2W H2WB 109.0 . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 105.0 . . ?
 H13B N13 H13C 96.0 . . ?
 C13 N13 H13A 123.0 . . ?
 C13 N13 H13B 107.0 . . ?
 C13 N13 H13C 112.0 . . ?
 H3A N3 H3B 113.0 . . ?
 H3A N3 H3C 107.0 . . ?
 H3B N3 H3C 114.0 . . ?
 C3 N3 H3A 108.0 . . ?
 C3 N3 H3B 107.0 . . ?
 C3 N3 H3C 107.0 . . ?
 H2A C2 H2B 107.7 . . ?
 C1 C2 H2A 108.8 . . ?
 C1 C2 H2B 108.8 . . ?
 C1 C2 C3 113.9(17) . . ?
 C3 C2 H2A 108.8 . . ?
 C3 C2 H2B 108.8 . . ?
 O4 C4 C3 115.9(15) . . ?
 O3 C4 O4 117(5) . . ?
 O3 C4 C3 122.8(15) . . ?
 O14 C14 O13 119(4) . . ?
 O14 C14 C13 113(4) . . ?
 O13 C14 C13 128(3) . . ?
 O11 C11 C12 111.8(13) . . ?
 O12 C11 O11 119(3) . . ?
 O12 C11 C12 125.5(15) . . ?
 C11 C12 H12A 107.9 . . ?
 C11 C12 H12B 107.9 . . ?
 C11 C12 C13 118(2) . . ?
 H12A C12 H12B 107.2 . . ?
 C13 C12 H12A 107.9 . . ?
 C13 C12 H12B 107.9 . . ?
 N13 C13 C14 102(4) . . ?
 N13 C13 C12 118(3) . . ?
 N13 C13 H13 108.8 . . ?
 C14 C13 C12 110.6(18) . . ?
 C14 C13 H13 108.8 . . ?
 C12 C13 H13 108.8 . . ?
 O1 C1 C2 121(3) . . ?
 O2 C1 O1 120(4) . . ?
 O2 C1 C2 119(3) . . ?
 N3 C3 C2 111.0(18) . . ?
 N3 C3 C4 110(2) . . ?
 N3 C3 H3 106.3 . . ?
 C2 C3 H3 106.3 . . ?
 C4 C3 C2 116(2) . . ?
 C4 C3 H3 106.3 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 20(3) . . . . ?
 Zn1 O14 C14 C13 174.2(14) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -170(4) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 167(4) . . . . ?
 O2 C1 C2 C3 29(3) . . . . ?
 O12 C11 C12 C13 145(5) . . . . ?
 N13 C13 C14 O13 14(3) . . . . ?
 N3 C3 C4 O3 -18(10) . . . . ?
 C11 C12 C13 N13 59(5) . . . . ?
 C11 C12 C13 C14 -58(4) . . . . ?
 C1 C2 C3 N3 -67(4) . . . . ?
 C1 C2 C3 C4 59(5) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_2_53GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972167'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_2_53GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.194 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_2_53GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.05 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.484(3)
_cell_length_b                     9.110(3)
_cell_length_c                     9.6213(14)
_cell_angle_alpha                  110.91(2)
_cell_angle_beta                   104.75(2)
_cell_angle_gamma                  108.76(3)
_cell_volume                       597.6(3)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      319
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         2530000 
_cell_measurement_theta_max        27.112
_cell_measurement_theta_min        3.984
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.117
_exptl_absorpt_correction_T_max    0.900
_exptl_absorpt_correction_T_min    0.608
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 2.53(2) GPa
 (2530000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.032
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1056
_diffrn_reflns_av_unetI/netI       0.0889
_diffrn_reflns_Laue_measured_fraction_full  0.194
_diffrn_reflns_Laue_measured_fraction_max  0.168
_diffrn_reflns_limit_h_max         4
_diffrn_reflns_limit_h_min         -4
_diffrn_reflns_limit_k_max         8
_diffrn_reflns_limit_k_min         -9
_diffrn_reflns_limit_l_max         12
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              2469
_diffrn_reflns_point_group_measured_fraction_full  0.194
_diffrn_reflns_point_group_measured_fraction_max  0.168
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.112
_diffrn_reflns_theta_min           3.984
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.194
_diffrn_measured_fraction_theta_max  0.168
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  319
_reflns_number_total               444
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.290
_refine_diff_density_min           -0.270
_refine_diff_density_rms           0.072
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.057
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           444
_refine_ls_number_restraints       134
_refine_ls_R_factor_all            0.0847
_refine_ls_R_factor_gt             0.0514
_refine_ls_restrained_S_all        0.894
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0740P)²+4.5648P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1124
_refine_ls_wR_factor_ref           0.1409
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C2-C1
 1.52 with sigma of 0.02
 C1-O2
 1.24 with sigma of 0.02
 C14-O14
 1.24 with sigma of 0.02
 C14-O13
 1.33 with sigma of 0.03
 C14-C13
 1.52 with sigma of 0.03
 C4-C2
 2.55 with sigma of 0.01
 C3-C1
 2.56 with sigma of 0.01
 C4-C1
 3.06 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Zn1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O4) \\sim Ueq,
Uanis(O3) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq:
with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?

loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.6989(18) 0.3200(8) 0.5311(3) 0.030(3) Uani 1 1 d . U . . .
 O1 O 0.644(5) 0.338(2) 0.7171(14) 0.034(5) Uani 1 1 d . U . . .
 O2 O 0.586(4) 0.281(2) 0.9072(13) 0.032(7) Uani 1 1 d D U . . .
 O14 O 1.108(7) 0.761(4) 0.480(2) 0.043(9) Uani 1 1 d D U . . .
 O4 O 0.525(5) -0.109(2) 0.6398(14) 0.029(5) Uani 1 1 d . U . . .
 O11 O 0.699(7) 0.511(3) 0.4876(14) 0.032(5) Uani 1 1 d . U . . .
 O1W O 0.237(6) 0.033(2) 0.7766(14) 0.029(7) Uani 1 1 d . U . . .
 H1WA H 0.348749 0.108103 0.811188 0.044 Uiso 1 1 d G . . . .
 H1WB H 0.205179 -0.031224 0.675390 0.044 Uiso 1 1 d G . . . .
 O13 O 0.953(5) 0.505(3) 0.2591(18) 0.048(8) Uani 1 1 d D U . . .
 O3 O 0.519(5) -0.167(2) 0.8465(13) 0.033(7) Uani 1 1 d . U . . .
 O12 O 0.834(5) 0.736(2) 0.7340(13) 0.031(7) Uani 1 1 d . U . . .
 O2W O 0.237(5) 0.319(3) 1.0099(15) 0.039(7) Uani 1 1 d . U . . .
 H2WA H 0.181869 0.210974 0.956312 0.058 Uiso 1 1 d G . . . .
 H2WB H 0.208858 0.346307 1.089051 0.058 Uiso 1 1 d G . . . .
 N13 N 0.628(2) 0.526(2) 0.215(17) 0.030(7) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.790(6) 0.156(3) 1.0600(14) 0.032(8) Uani 1 1 d . U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C2 C 0.815(5) 0.216(3) 0.831(3) 0.033(9) Uani 1 1 d D U . . .
 H2A H 0.935600 0.315171 0.903852 0.040 Uiso 1 1 calc R . . . .
 H2B H 0.813846 0.162494 0.723152 0.040 Uiso 1 1 calc R . . . .
 C4 C 0.599(7) -0.083(3) 0.787(2) 0.029(6) Uani 1 1 d D U . . .
 C14 C 0.954(6) 0.647(3) 0.359(3) 0.024(9) Uani 1 1 d D U . . .
 C11 C 0.775(8) 0.672(4) 0.586(2) 0.029(6) Uani 1 1 d . U . . .
 C12 C 0.805(7) 0.778(3) 0.4998(18) 0.028(6) Uani 1 1 d . U . . .
 H12A H 0.712606 0.819791 0.491530 0.033 Uiso 1 1 calc R . . . .
 H12B H 0.922565 0.881743 0.570380 0.033 Uiso 1 1 calc R . . . .
 C13 C 0.802(6) 0.703(4) 0.342(3) 0.026(9) Uani 1 1 d D U . . .
 H13 H 0.829338 0.793724 0.307141 0.031 Uiso 1 1 calc R . . . .
 C1 C 0.672(5) 0.283(3) 0.821(3) 0.026(8) Uani 1 1 d D U . . .
 C3 C 0.781(5) 0.078(3) 0.8938(18) 0.031(6) Uani 1 1 d D U . . .
 H3 H 0.874335 0.037145 0.888835 0.038 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.929(19) . ?
 Zn1 O14 2.01(7) 2_766 ?
 Zn1 O4 1.953(18) 2_656 ?
 Zn1 O11 1.93(5) . ?
 O1 C1 1.28(4) . ?
 O2 C1 1.24(2) . ?
 O14 C14 1.27(2) . ?
 O4 C4 1.29(3) . ?
 O11 C11 1.25(3) . ?
 O1W H1WA 0.8567 . ?
 O1W H1WB 0.8493 . ?
 O13 C14 1.30(3) . ?
 O3 C4 1.25(2) . ?
 O12 C11 1.22(2) . ?
 O2W H2WA 0.8221 . ?
 O2W H2WB 0.8340 . ?
 N13 H13A 0.8700 . ?
 N13 H13B 0.8700 . ?
 N13 H13C 0.8500 . ?
 N13 C13 1.46(4) . ?
 N3 H3A 0.8900 . ?
 N3 H3B 0.8000 . ?
 N3 H3C 0.8500 . ?
 N3 C3 1.44(2) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C1 1.52(3) . ?
 C2 C3 1.56(2) . ?
 C4 C3 1.50(3) . ?
 C14 C13 1.53(4) . ?
 C11 C12 1.48(3) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C12 C13 1.42(4) . ?
 C13 H13 0.9800 . ?
 C3 H3 0.9800 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 113.7(18) . 2_766 ?
 O1 Zn1 O4 98.6(9) . 2_656 ?
 O1 Zn1 O11 111(2) . . ?
 O4 Zn1 O14 102.1(16) 2_656 2_766 ?
 O11 Zn1 O14 121(2) . 2_766 ?
 O11 Zn1 O4 106.4(18) . 2_656 ?
 C1 O1 Zn1 136(4) . . ?
 C14 O14 Zn1 111(3) . 2_766 ?
 C4 O4 Zn1 123.2(10) . 2_656 ?
 C11 O11 Zn1 129(3) . . ?
 H1WA O1W H1WB 104.2 . . ?
 H2WA O2W H2WB 106.0 . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 111.0 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 105.0 . . ?
 C13 N13 H13C 112.0 . . ?
 H3A N3 H3B 113.0 . . ?
 H3A N3 H3C 107.0 . . ?
 H3B N3 H3C 114.0 . . ?
 C3 N3 H3A 111.0 . . ?
 C3 N3 H3B 105.0 . . ?
 C3 N3 H3C 107.0 . . ?
 H2A C2 H2B 107.9 . . ?
 C1 C2 H2A 109.2 . . ?
 C1 C2 H2B 109.2 . . ?
 C1 C2 C3 112.2(16) . . ?
 C3 C2 H2A 109.2 . . ?
 C3 C2 H2B 109.2 . . ?
 O4 C4 C3 114.8(13) . . ?
 O3 C4 O4 124(3) . . ?
 O3 C4 C3 120.3(17) . . ?
 O14 C14 O13 115(4) . . ?
 O14 C14 C13 116(4) . . ?
 O13 C14 C13 129(3) . . ?
 O11 C11 C12 111.0(14) . . ?
 O12 C11 O11 125(3) . . ?
 O12 C11 C12 123.9(18) . . ?
 C11 C12 H12A 107.2 . . ?
 C11 C12 H12B 107.2 . . ?
 H12A C12 H12B 106.8 . . ?
 C13 C12 C11 121(3) . . ?
 C13 C12 H12A 107.2 . . ?
 C13 C12 H12B 107.2 . . ?
 N13 C13 C14 106(4) . . ?
 N13 C13 H13 115.0 . . ?
 C14 C13 H13 108.9 . . ?
 C12 C13 N13 117(3) . . ?
 C12 C13 C14 107(4) . . ?
 C12 C13 H13 108.9 . . ?
 O1 C1 C2 116(3) . . ?
 O2 C1 O1 122(4) . . ?
 O2 C1 C2 122(3) . . ?
 N3 C3 C2 112.6(19) . . ?
 N3 C3 C4 108(3) . . ?
 N3 C3 H3 112.0 . . ?
 C2 C3 H3 106.2 . . ?
 C4 C3 C2 113.3(16) . . ?
 C4 C3 H3 106.2 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 15(3) . . . . ?
 Zn1 O14 C14 C13 173.0(18) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -174(3) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 157(5) . . . . ?
 O2 C1 C2 C3 25(3) . . . . ?
 O12 C11 C12 C13 154(6) . . . . ?
 N13 C13 C14 O13 14(4) . . . . ?
 N3 C3 C4 O3 -22(5) . . . . ?
 C11 C12 C13 N13 58(8) . . . . ?
 C11 C12 C13 C14 -60(5) . . . . ?
 C1 C2 C3 N3 -61(4) . . . . ?
 C1 C2 C3 C4 60(2) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_3_05GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972168'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_3_05GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.194 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_3_05GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04167 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.415(4)
_cell_length_b                     9.033(4)
_cell_length_c                     9.5778(17)
_cell_angle_alpha                  110.49(3)
_cell_angle_beta                   104.77(3)
_cell_angle_gamma                  108.92(5)
_cell_volume                       586.8(5)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      327
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         3050000 
_cell_measurement_theta_max        27.414
_cell_measurement_theta_min        4.025
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.156
_exptl_absorpt_correction_T_max    0.900
_exptl_absorpt_correction_T_min    0.608
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 3.05(2) GPa
 (3050000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.069
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0645
_diffrn_reflns_av_unetI/netI       0.0618
_diffrn_reflns_Laue_measured_fraction_full  0.194
_diffrn_reflns_Laue_measured_fraction_max  0.164
_diffrn_reflns_limit_h_max         4
_diffrn_reflns_limit_h_min         -4
_diffrn_reflns_limit_k_max         8
_diffrn_reflns_limit_k_min         -8
_diffrn_reflns_limit_l_max         12
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              2377
_diffrn_reflns_point_group_measured_fraction_full  0.194
_diffrn_reflns_point_group_measured_fraction_max  0.164
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.414
_diffrn_reflns_theta_min           4.025
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.194
_diffrn_measured_fraction_theta_max  0.164
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  327
_reflns_number_total               440
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.207
_refine_diff_density_min           -0.152
_refine_diff_density_rms           0.043
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.071
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           440
_refine_ls_number_restraints       126
_refine_ls_R_factor_all            0.0665
_refine_ls_R_factor_gt             0.0360
_refine_ls_restrained_S_all        0.906
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0544P)²+0.3153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0736
_refine_ls_wR_factor_ref           0.0850
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C14-C13
 1.55 with sigma of 0.03
 C2-C1
 1.51 with sigma of 0.03
 C4-C2
 2.55 with sigma of 0.01
 C3-C1
 2.56 with sigma of 0.01
 C4-C1
 3.06 with sigma of 0.01
 C4-N3
 2.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.6965(14) 0.3198(7) 0.5275(2) 0.043(13) Uani 1 1 d . . . . .
 O1 O 0.634(3) 0.3435(17) 0.7156(9) 0.039(4) Uani 1 1 d . U . . .
 O2 O 0.584(3) 0.2830(17) 0.9065(9) 0.036(6) Uani 1 1 d . U . . .
 O14 O 1.109(8) 0.759(4) 0.4868(19) 0.053(8) Uani 1 1 d . U . . .
 O4 O 0.527(3) -0.1049(16) 0.6418(8) 0.033(4) Uani 1 1 d . U . . .
 O11 O 0.701(5) 0.509(3) 0.4835(9) 0.031(5) Uani 1 1 d . U . . .
 O1W O 0.241(4) 0.0350(18) 0.7780(9) 0.032(6) Uani 1 1 d . U . . .
 H1WA H 0.352455 0.107109 0.808728 0.047 Uiso 1 1 d G . . . .
 H1WB H 0.213022 -0.047092 0.684478 0.047 Uiso 1 1 d G . . . .
 O13 O 0.942(4) 0.508(2) 0.2613(12) 0.043(7) Uani 1 1 d . U . . .
 O3 O 0.513(3) -0.1641(15) 0.8470(8) 0.037(6) Uani 1 1 d . U . . .
 O12 O 0.825(4) 0.737(2) 0.7302(9) 0.038(6) Uani 1 1 d . U . . .
 O2W O 0.232(3) 0.3211(17) 1.0127(9) 0.038(6) Uani 1 1 d . U . . .
 H2WA H 0.204770 0.223193 0.933353 0.057 Uiso 1 1 d G . . . .
 H2WB H 0.254475 0.304054 1.095837 0.057 Uiso 1 1 d G . . . .
 N13 N 0.628(2) 0.526(2) 0.215(17) 0.0290(3) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.802(5) 0.1559(19) 1.0631(10) 0.038(7) Uani 1 1 d D U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C4 C 0.603(5) -0.083(2) 0.7892(12) 0.029(5) Uani 1 1 d D U . . .
 C13 C 0.811(6) 0.701(3) 0.3404(19) 0.026(8) Uani 1 1 d D U . . .
 H13 H 0.842274 0.790701 0.303282 0.031 Uiso 1 1 calc R . . . .
 C11 C 0.768(5) 0.676(3) 0.5814(13) 0.030(5) Uani 1 1 d . U . . .
 C12 C 0.800(5) 0.783(2) 0.4960(12) 0.029(5) Uani 1 1 d . U . . .
 H12A H 0.702236 0.817163 0.477437 0.035 Uiso 1 1 calc R . . . .
 H12B H 0.914931 0.890891 0.568785 0.035 Uiso 1 1 calc R . . . .
 C14 C 0.967(6) 0.643(3) 0.361(2) 0.025(8) Uani 1 1 d D U . . .
 C3 C 0.783(4) 0.081(2) 0.8977(12) 0.032(5) Uani 1 1 d D U . . .
 H3 H 0.879972 0.043506 0.897901 0.038 Uiso 1 1 calc R . . . .
 C2 C 0.820(5) 0.221(2) 0.838(2) 0.034(7) Uani 1 1 d D U . . .
 H2A H 0.937743 0.322825 0.915356 0.041 Uiso 1 1 calc R . . . .
 H2B H 0.827963 0.171389 0.733532 0.041 Uiso 1 1 calc R . . . .
 C1 C 0.670(4) 0.282(2) 0.817(2) 0.022(6) Uani 1 1 d D U . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.962(15) . ?
 Zn1 O14 2.01(7) 2_766 ?
 Zn1 O4 1.954(11) 2_656 ?
 Zn1 O11 1.89(4) . ?
 O1 C1 1.30(3) . ?
 O2 C1 1.26(3) . ?
 O14 C14 1.25(3) . ?
 O4 C4 1.31(2) . ?
 O11 C11 1.29(3) . ?
 O1W H1WA 0.8502 . ?
 O1W H1WB 0.8504 . ?
 O13 C14 1.17(4) . ?
 O3 C4 1.249(18) . ?
 O12 C11 1.224(13) . ?
 O2W H2WA 0.8492 . ?
 O2W H2WB 0.8499 . ?
 N13 H13A 0.8700 . ?
 N13 H13B 0.8600 . ?
 N13 H13C 0.8400 . ?
 N13 C13 1.48(3) . ?
 N3 H3A 0.9700 . ?
 N3 H3B 0.7300 . ?
 N3 H3C 0.8400 . ?
 N3 C3 1.431(19) . ?
 C4 C3 1.493(18) . ?
 C13 H13 0.9800 . ?
 C13 C12 1.45(3) . ?
 C13 C14 1.56(4) . ?
 C11 C12 1.476(19) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.54(2) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C1 1.53(4) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O14 117.2(12) . 2_766 ?
 O4 Zn1 O1 98.4(7) 2_656 . ?
 O4 Zn1 O14 101.3(13) 2_656 2_766 ?
 O11 Zn1 O1 109.6(17) . . ?
 O11 Zn1 O14 119.3(18) . 2_766 ?
 O11 Zn1 O4 108.0(13) . 2_656 ?
 C1 O1 Zn1 130(2) . . ?
 C14 O14 Zn1 105(4) . 2_766 ?
 C4 O4 Zn1 122.0(6) . 2_656 ?
 C11 O11 Zn1 130.6(13) . . ?
 H1WA O1W H1WB 104.4 . . ?
 H2WA O2W H2WB 104.6 . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 109.5 . . ?
 C13 N13 H13B 107.0 . . ?
 C13 N13 H13C 111.0 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 100.0 . . ?
 H3B N3 H3C 122.0 . . ?
 C3 N3 H3A 106.0 . . ?
 C3 N3 H3B 109.5 . . ?
 C3 N3 H3C 108.0 . . ?
 O4 C4 C3 114.8(9) . . ?
 O3 C4 O4 122(2) . . ?
 O3 C4 C3 121.2(9) . . ?
 N13 C13 H13 114.0 . . ?
 N13 C13 C14 107(3) . . ?
 C12 C13 N13 115(3) . . ?
 C12 C13 H13 107.7 . . ?
 C12 C13 C14 111(3) . . ?
 C14 C13 H13 107.7 . . ?
 O11 C11 C12 111.7(10) . . ?
 O12 C11 O11 123(2) . . ?
 O12 C11 C12 124.5(13) . . ?
 C13 C12 C11 117(3) . . ?
 C13 C12 H12A 108.0 . . ?
 C13 C12 H12B 108.0 . . ?
 C11 C12 H12A 108.0 . . ?
 C11 C12 H12B 108.0 . . ?
 H12A C12 H12B 107.2 . . ?
 O14 C14 C13 111(4) . . ?
 O13 C14 O14 129(6) . . ?
 O13 C14 C13 120(3) . . ?
 N3 C3 C4 111.0(14) . . ?
 N3 C3 H3 106.5 . . ?
 N3 C3 C2 111.5(16) . . ?
 C4 C3 H3 106.5 . . ?
 C4 C3 C2 114.4(12) . . ?
 C2 C3 H3 106.5 . . ?
 C3 C2 H2A 109.0 . . ?
 C3 C2 H2B 109.0 . . ?
 H2A C2 H2B 107.8 . . ?
 C1 C2 C3 113.0(18) . . ?
 C1 C2 H2A 109.0 . . ?
 C1 C2 H2B 109.0 . . ?
 O1 C1 C2 123(2) . . ?
 O2 C1 O1 117(4) . . ?
 O2 C1 C2 120(3) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 18.1(19) . . . . ?
 Zn1 O14 C14 C13 170.9(12) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -174(2) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 160(4) . . . . ?
 O2 C1 C2 C3 30(2) . . . . ?
 O12 C11 C12 C13 150(4) . . . . ?
 N13 C13 C14 O13 20(6) . . . . ?
 N3 C3 C4 O3 -18(4) . . . . ?
 C11 C12 C13 N13 64(5) . . . . ?
 C11 C12 C13 C14 -58(3) . . . . ?
 C1 C2 C3 N3 -69(3) . . . . ?
 C1 C2 C3 C4 58(2) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_3_53GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972169'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_3_53GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.188 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_3_53GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.06667 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.386(5)
_cell_length_b                     8.983(3)
_cell_length_c                     9.5498(19)
_cell_angle_alpha                  110.18(2)
_cell_angle_beta                   104.73(3)
_cell_angle_gamma                  109.15(4)
_cell_volume                       580.5(5)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      284
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         3530000 
_cell_measurement_theta_max        27.366
_cell_measurement_theta_min        4.055
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.180
_exptl_absorpt_correction_T_max    0.897
_exptl_absorpt_correction_T_min    0.599
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 3.53(2) GPa
 (3530000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.092
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0842
_diffrn_reflns_av_unetI/netI       0.0866
_diffrn_reflns_Laue_measured_fraction_full  0.188
_diffrn_reflns_Laue_measured_fraction_max  0.160
_diffrn_reflns_limit_h_max         4
_diffrn_reflns_limit_h_min         -5
_diffrn_reflns_limit_k_max         8
_diffrn_reflns_limit_k_min         -8
_diffrn_reflns_limit_l_max         11
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              2344
_diffrn_reflns_point_group_measured_fraction_full  0.188
_diffrn_reflns_point_group_measured_fraction_max  0.160
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.366
_diffrn_reflns_theta_min           4.055
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.188
_diffrn_measured_fraction_theta_max  0.160
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  284
_reflns_number_total               421
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.426
_refine_diff_density_min           -0.288
_refine_diff_density_rms           0.071
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.134
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       198
_refine_ls_number_reflns           421
_refine_ls_number_restraints       126
_refine_ls_R_factor_all            0.0952
_refine_ls_R_factor_gt             0.0536
_refine_ls_restrained_S_all        0.949
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.1189P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1339
_refine_ls_wR_factor_ref           0.1625
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C14-C13
 1.55 with sigma of 0.03
 C2-C1
 1.51 with sigma of 0.03
 C4-C2
 2.55 with sigma of 0.01
 C3-C1
 2.56 with sigma of 0.01
 C4-C1
 3.06 with sigma of 0.01
 C4-N3
 2.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.d Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.6859(17) 0.3227(10) 0.5251(4) 0.066(17) Uani 1 1 d . . . . .
 O1 O 0.636(5) 0.345(3) 0.7162(15) 0.042(5) Uani 1 1 d . U . . .
 O2 O 0.598(5) 0.282(3) 0.9093(14) 0.039(8) Uani 1 1 d . U . . .
 O14 O 1.125(9) 0.746(5) 0.486(2) 0.021(7) Uani 1 1 d . U . . .
 O4 O 0.536(6) -0.104(3) 0.6453(14) 0.031(5) Uani 1 1 d . U . . .
 O11 O 0.710(8) 0.507(4) 0.4821(15) 0.041(6) Uani 1 1 d . U . . .
 O1W O 0.239(6) 0.036(3) 0.7777(16) 0.043(8) Uani 1 1 d . U . . .
 H1WA H 0.354154 0.103369 0.817840 0.065 Uiso 1 1 d G . . . .
 H1WB H 0.213955 -0.037761 0.681240 0.065 Uiso 1 1 d G . . . .
 O13 O 0.944(7) 0.506(4) 0.2630(19) 0.045(8) Uani 1 1 d . U . . .
 O3 O 0.523(5) -0.166(3) 0.8474(13) 0.042(8) Uani 1 1 d . U . . .
 O12 O 0.836(6) 0.732(4) 0.7292(15) 0.042(8) Uani 1 1 d . U . . .
 O2W O 0.226(5) 0.324(3) 1.0150(15) 0.040(8) Uani 1 1 d . U . . .
 H2WA H 0.240072 0.236654 0.969367 0.061 Uiso 1 1 d G . . . .
 H2WB H 0.233859 0.333204 1.106321 0.061 Uiso 1 1 d G . . . .
 N13 N 0.6283(2) 0.526(2) 0.216(2) 0.035(7) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.7820(2) 0.15150(18) 1.05345(17) 0.041(7) Uani 1 1 d DU . . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C4 C 0.600(6) -0.082(3) 0.7879(18) 0.031(6) Uani 1 1 d D U . . .
 C13 C 0.820(10) 0.703(5) 0.341(3) 0.025(10) Uani 1 1 d D U . . .
 H13 H 0.858374 0.792701 0.304345 0.030 Uiso 1 1 calc R . . . .
 C11 C 0.762(8) 0.680(5) 0.581(2) 0.031(6) Uani 1 1 d . U . . .
 C12 C 0.802(8) 0.788(4) 0.4936(19) 0.031(6) Uani 1 1 d . U . . .
 H12A H 0.702412 0.820892 0.468608 0.037 Uiso 1 1 calc R . . . .
 H12B H 0.915326 0.897887 0.568166 0.037 Uiso 1 1 calc R . . . .
 C14 C 0.970(10) 0.638(6) 0.364(4) 0.043(14) Uani 1 1 d D U . . .
 C3 C 0.785(6) 0.083(4) 0.8984(19) 0.034(6) Uani 1 1 d D U . . .
 H3 H 0.878002 0.040906 0.889884 0.041 Uiso 1 1 calc R . . . .
 C2 C 0.822(7) 0.223(4) 0.836(3) 0.036(11) Uani 1 1 d D U . . .
 H2A H 0.942306 0.324716 0.911152 0.043 Uiso 1 1 calc R . . . .
 H2B H 0.826625 0.171181 0.729821 0.043 Uiso 1 1 calc R . . . .
 C1 C 0.671(7) 0.286(3) 0.818(3) 0.031(11) Uani 1 1 d D U . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.93(2) . ?
 Zn1 O14 1.89(10) 2_766 ?
 Zn1 O4 1.955(15) 2_656 ?
 Zn1 O11 1.80(5) . ?
 O1 C1 1.28(5) . ?
 O2 C1 1.18(4) . ?
 O14 C14 1.27(6) . ?
 O4 C4 1.25(3) . ?
 O11 C11 1.35(6) . ?
 O1W H1WA 0.8444 . ?
 O1W H1WB 0.8495 . ?
 O13 C14 1.15(7) . ?
 O3 C4 1.21(2) . ?
 O12 C11 1.22(3) . ?
 O2W H2WA 0.8165 . ?
 O2W H2WB 0.8293 . ?
 N13 H13A 0.8900 . ?
 N13 H13B 0.8600 . ?
 N13 H13C 0.8300 . ?
 N13 C13 1.61(6) . ?
 N3 H3A 0.8500 . ?
 N3 H3B 0.8500 . ?
 N3 H3C 0.8400 . ?
 N3 C3 1.37(3) . ?
 C4 C3 1.52(3) . ?
 C13 H13 0.9800 . ?
 C13 C12 1.47(6) . ?
 C13 C14 1.55(4) . ?
 C11 C12 1.50(4) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.55(3) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C1 1.55(4) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O4 100.6(9) . 2_656 ?
 O14 Zn1 O1 114(2) 2_766 . ?
 O14 Zn1 O4 101.6(19) 2_766 2_656 ?
 O11 Zn1 O1 114(2) . . ?
 O11 Zn1 O14 113(3) . 2_766 ?
 O11 Zn1 O4 111.2(18) . 2_656 ?
 C1 O1 Zn1 133(4) . . ?
 C14 O14 Zn1 113(5) . 2_766 ?
 C4 O4 Zn1 120.6(10) . 2_656 ?
 C11 O11 Zn1 131.2(15) . . ?
 H1WA O1W H1WB 104.4 . . ?
 H2WA O2W H2WB 106.9 . . ?
 H13A N13 H13B 108.0 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 111.0 . . ?
 C13 N13 H13A 107.0 . . ?
 C13 N13 H13B 109.5 . . ?
 C13 N13 H13C 112.0 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 107.0 . . ?
 C3 N3 H3A 117.0 . . ?
 C3 N3 H3B 104.0 . . ?
 C3 N3 H3C 109.5 . . ?
 O4 C4 C3 113.5(14) . . ?
 O3 C4 O4 127(3) . . ?
 O3 C4 C3 119.0(15) . . ?
 N13 C13 H13 116.0 . . ?
 N13 C13 C14 105(3) . . ?
 C12 C13 N13 111(5) . . ?
 C12 C13 H13 107.3 . . ?
 C12 C13 C14 113(5) . . ?
 C14 C13 H13 107.3 . . ?
 O11 C11 C12 110(2) . . ?
 O12 C11 O11 117(5) . . ?
 O12 C11 C12 126.3(17) . . ?
 C13 C12 C11 116(5) . . ?
 C13 C12 H12A 108.2 . . ?
 C13 C12 H12B 108.2 . . ?
 C11 C12 H12A 108.2 . . ?
 C11 C12 H12B 108.2 . . ?
 H12A C12 H12B 107.3 . . ?
 O14 C14 C13 117(6) . . ?
 O13 C14 O14 123(9) . . ?
 O13 C14 C13 119(6) . . ?
 N3 C3 C4 106(3) . . ?
 N3 C3 H3 117.0 . . ?
 N3 C3 C2 115(3) . . ?
 C4 C3 H3 104.6 . . ?
 C4 C3 C2 113.3(16) . . ?
 C2 C3 H3 104.6 . . ?
 C3 C2 H2A 109.3 . . ?
 C3 C2 H2B 109.3 . . ?
 H2A C2 H2B 107.9 . . ?
 C1 C2 C3 112(2) . . ?
 C1 C2 H2A 109.3 . . ?
 C1 C2 H2B 109.3 . . ?
 O1 C1 C2 120(4) . . ?
 O2 C1 O1 124(6) . . ?
 O2 C1 C2 116(4) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Zn1 O1 C1 C2 19(3) . . . . ?
 Zn1 O14 C14 C13 166(2) . 2_766 2_766 2_766 ?
 Zn1 O4 C4 C3 -173(3) . 2_656 2_656 2_656 ?
 Zn1 O11 C11 C12 167(6) . . . . ?
 O2 C1 C2 C3 29(3) . . . . ?
 O12 C11 C12 C13 136(8) . . . . ?
 N13 C13 C14 O13 25(6) . . . . ?
 N3 C3 C4 O3 -29(5) . . . . ?
 C11 C12 C13 N13 60(6) . . . . ?
 C11 C12 C13 C14 -56(5) . . . . ?
 C1 C2 C3 N3 -61(4) . . . . ?
 C1 C2 C3 C4 59(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# and

#==============================================================================

data_Zn-aspartate_dihydrate_4_02GPa 
_database_code_depnum_ccdc_archive 'CCDC 1972170'

_audit_creation_date               2019-09-16
# start Validation Reply Form
_vrf_PLAT029_zinc-aspartate_dihydrate_4_02GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.194 Why?  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT232_zinc-aspartate_dihydrate_4_02GPa
;
PROBLEM: Hirshfeld Test Diff (M-X)  Zn1      --O14_b    .       12.4 s.u.  
RESPONSE: Due to the specificity of the applied measuring 
technique and use of a diamond-anvil cell limiting the access 
of the X-ray radiation to the measured sample, and therefore 
lowering the measured fraction of the theta angle.
;
_vrf_PLAT341_zinc-aspartate_dihydrate_4_02GPa
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.06667 Ang.  
RESPONSE: Low precision of bond length due to limited access 
to reciprocal lattice due to the specificity of the applied 
measuring technique and use of a diamond-anvil cell.
;
# end Validation Reply Form
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_audit_contact_author_email       katran@amu.edu.pl
_audit_contact_author_name         'Katrusiak, Andrzej'
_audit_contact_author_phone        ?

_publ_contact_author_address      
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
loop_
_publ_contact_author_email       
katran@amu.edu.pl
kinga.roszak@amu.edu.pl
loop_
_publ_contact_author_name        
'Katrusiak, Andrzej'
'Roszak, Kinga'
_publ_contact_author_phone        ?

loop_
_publ_author_name
   'Katrusiak, Andrzej'
   'Roszak, Kinga'
loop_
_publ_author_footnote
; Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_author_address
;Faculty of Chemistry,
Adam Mickiewicz University in Ponzan,
Uniwersytetu Poznanskiego 8, 61-614  Poznan
Poland
;
_publ_contact_author_id_orcid      0000-0002-1439-7278
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              
; 
zinc-aspartate dihydrate 
;  
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H24 N4 O16 Zn2, 4(H2 O)'
_chemical_formula_sum              'C16 H32 N4 O20 Zn2'
_chemical_formula_weight           731.19
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     8.343(7)
_cell_length_b                     8.947(6)
_cell_length_c                     9.537(3)
_cell_angle_alpha                  110.02(4)
_cell_angle_beta                   104.76(4)
_cell_angle_gamma                  109.16(7)
_cell_volume                       575.2(7)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      253
_cell_measurement_temperature      296(2)
_cell_measurement_pressure         4020000 
_cell_measurement_theta_max        27.309
_cell_measurement_theta_min        4.074
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.200
_exptl_absorpt_correction_T_max    0.896
_exptl_absorpt_correction_T_min    0.596
_exptl_absorpt_correction_type     'integration'
_exptl_absorpt_process_details    
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (2015).
; 
_exptl_special_details 
; 
Data were collected at room temperature and pressure of 4.02(2) GPa
 (4020000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique. Pressure was determined by monitoring 
the shift of the ruby R1-fluorescence line.
;             
_exptl_crystal_colour              colourless
_exptl_crystal_density_diffrn      2.111
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         plate
_exptl_crystal_F_000               376
_exptl_crystal_size_max            0.25
_exptl_crystal_size_mid            0.20
_exptl_crystal_size_min            0.05
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1240
_diffrn_reflns_av_unetI/netI       0.1047
_diffrn_reflns_Laue_measured_fraction_full  0.194
_diffrn_reflns_Laue_measured_fraction_max  0.166
_diffrn_reflns_limit_h_max         5
_diffrn_reflns_limit_h_min         -5
_diffrn_reflns_limit_k_max         7
_diffrn_reflns_limit_k_min         -7
_diffrn_reflns_limit_l_max         11
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              2352
_diffrn_reflns_point_group_measured_fraction_full  0.194
_diffrn_reflns_point_group_measured_fraction_max  0.166
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.309
_diffrn_reflns_theta_min           4.074
_diffrn_ambient_temperature        296(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.194
_diffrn_measured_fraction_theta_max  0.166
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'omega scan'
_diffrn_standards_number           12
_diffrn_standards_interval_count   84
_diffrn_standards_interval_time    2
_diffrn_standards_decay_%          0
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed x-ray tube'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  253
_reflns_number_total               430
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max           0.218
_refine_diff_density_min           -0.198
_refine_diff_density_rms           0.056
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.149
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       204
_refine_ls_number_reflns           430
_refine_ls_number_restraints       134
_refine_ls_R_factor_all            0.1168
_refine_ls_R_factor_gt             0.0519
_refine_ls_restrained_S_all        0.948
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0827P)²+0.5519P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1136
_refine_ls_wR_factor_ref           0.1560
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C14-C13
 1.55 with sigma of 0.03
 C2-C1
 1.51 with sigma of 0.03
 C4-C2
 2.55 with sigma of 0.01
 C3-C1
 2.56 with sigma of 0.01
 C4-C1
 3.06 with sigma of 0.01
 C4-N3
 2.4 with sigma of 0.01
 O1W-H1WB
 0.85 with sigma of 0.01
 O1W-H1WA
 0.85 with sigma of 0.01
 H1WA-O2
 1.8 with sigma of 0.05
 H1WB_$1-O14
 1.8 with sigma of 0.05
 O2W-H2WB
 0.85 with sigma of 0.05
 O2W-H2WA
 0.85 with sigma of 0.05
 H2WA-O1W
 2 with sigma of 0.05
 H2WB_$4-O12
 2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
4.a Ternary CH refined with riding coordinates:
 C13(H13), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.c Idealised Me refined as rotating group:
 N13(H13A,H13B,H13C), N3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Zn1 Zn 0.6860(14) 0.3227(9) 0.5241(4) 0.107(18) Uani 1 1 d . . . . .
 O1 O 0.646(5) 0.339(4) 0.7158(17) 0.057(6) Uani 1 1 d . U . . .
 O2 O 0.593(6) 0.284(4) 0.9096(16) 0.049(8) Uani 1 1 d D U . . .
 O14 O 1.144(9) 0.748(7) 0.492(2) 0.046(10) Uani 1 1 d D U . . .
 O4 O 0.530(5) -0.103(4) 0.6444(16) 0.041(6) Uani 1 1 d . U . . .
 O11 O 0.723(7) 0.491(4) 0.4783(18) 0.060(7) Uani 1 1 d . U . . .
 O1W O 0.239(5) 0.035(4) 0.7770(18) 0.049(8) Uani 1 1 d D U . . .
 H1WA H 0.356(8) 0.10(2) 0.81(2) 0.073 Uiso 1 1 d DR . . . .
 H1WB H 0.20(3) -0.054(18) 0.682(13) 0.073 Uiso 1 1 d DR . . . .
 O13 O 0.934(7) 0.511(5) 0.265(2) 0.054(9) Uani 1 1 d . U . . .
 O3 O 0.521(5) -0.166(3) 0.8511(15) 0.042(8) Uani 1 1 d . U . . .
 O12 O 0.815(6) 0.741(5) 0.7274(18) 0.052(8) Uani 1 1 d D U . . .
 O2W O 0.235(4) 0.320(3) 1.0140(15) 0.043(8) Uani 1 1 d D U . . .
 H2WA H 0.21(4) 0.211(14) 0.96(2) 0.064 Uiso 1 1 d DR . . . .
 H2WB H 0.24(7) 0.35(4) 1.114(11) 0.064 Uiso 1 1 d DR . . . .
 N13 N 0.628(18) 0.526(19) 0.215(17) 0.047(9) Uani 1 1 d . U . . .
 H13A H 0.636167 0.482799 0.121891 0.035 Uiso 1 1 calc GR . . . .
 H13B H 0.539355 0.554456 0.201408 0.035 Uiso 1 1 calc GR . . . .
 H13C H 0.608602 0.450977 0.249310 0.035 Uiso 1 1 calc GR . . . .
 N3 N 0.7820(2) 0.15150(18) 1.05345(17) 0.051(9) Uani 1 1 d D U . . .
 H3A H 0.711687 0.201226 1.064078 0.038 Uiso 1 1 calc GR . . . .
 H3B H 0.894515 0.228842 1.117093 0.038 Uiso 1 1 calc GR . . . .
 H3C H 0.756227 0.072026 1.082374 0.038 Uiso 1 1 calc GR . . . .
 C4 C 0.598(7) -0.079(4) 0.793(2) 0.046(8) Uani 1 1 d D U . . .
 C13 C 0.826(7) 0.702(4) 0.344(3) 0.018(8) Uani 1 1 d D U . . .
 H13 H 0.863461 0.788300 0.303468 0.022 Uiso 1 1 calc R . . . .
 C11 C 0.770(9) 0.677(6) 0.584(3) 0.047(8) Uani 1 1 d . U . . .
 C12 C 0.797(7) 0.797(5) 0.494(2) 0.038(7) Uani 1 1 d . U . . .
 H12A H 0.688426 0.815858 0.460999 0.046 Uiso 1 1 calc R . . . .
 H12B H 0.904842 0.913151 0.567116 0.046 Uiso 1 1 calc R . . . .
 C14 C 0.980(8) 0.641(6) 0.368(5) 0.068(15) Uani 1 1 d D U . . .
 C3 C 0.786(7) 0.087(5) 0.899(2) 0.041(8) Uani 1 1 d D U . . .
 H3 H 0.879375 0.045357 0.890037 0.049 Uiso 1 1 calc R . . . .
 C2 C 0.822(7) 0.227(4) 0.841(3) 0.041(11) Uani 1 1 d D U . . .
 H2A H 0.834414 0.180227 0.739043 0.050 Uiso 1 1 calc R . . . .
 H2B H 0.939081 0.330951 0.921215 0.050 Uiso 1 1 calc R . . . .
 C1 C 0.670(8) 0.288(4) 0.814(3) 0.026(9) Uani 1 1 d D U . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Zn1 O1 1.908(18) . ?
 Zn1 O14 1.75(10) 2_766 ?
 Zn1 O4 1.932(14) 2_656 ?
 Zn1 O11 1.66(4) . ?
 Zn1 C14 2.57(7) 2_766 ?
 O1 C1 1.18(5) . ?
 O2 C1 1.24(4) . ?
 O14 C14 1.31(6) . ?
 O4 C4 1.29(3) . ?
 O11 C11 1.47(7) . ?
 O1W H1WA 0.851(14) . ?
 O1W H1WB 0.86(2) . ?
 O13 C14 1.09(6) . ?
 O3 C4 1.22(2) . ?
 O12 C11 1.18(3) . ?
 O2W H2WA 0.87(6) . ?
 O2W H2WB 0.88(12) . ?
 N13 H13A 0.8700 . ?
 N13 H13B 0.8500 . ?
 N13 H13C 0.8300 . ?
 N13 C13 1.50(4) . ?
 N3 H3A 0.8500 . ?
 N3 H3B 0.8500 . ?
 N3 H3C 0.8300 . ?
 N3 C3 1.40(3) . ?
 C4 C3 1.52(3) . ?
 C13 H13 0.9800 . ?
 C13 C12 1.51(6) . ?
 C13 C14 1.55(4) . ?
 C11 C12 1.59(5) . ?
 C12 H12A 0.9700 . ?
 C12 H12B 0.9700 . ?
 C3 H3 0.9800 . ?
 C3 C2 1.51(3) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C2 C1 1.53(4) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O1 Zn1 O4 101.5(7) . 2_656 ?
 O1 Zn1 C14 96.5(17) . 2_766 ?
 O14 Zn1 O1 112(2) 2_766 . ?
 O14 Zn1 O4 98(2) 2_766 2_656 ?
 O14 Zn1 C14 27.8(11) 2_766 2_766 ?
 O4 Zn1 C14 125(2) 2_656 2_766 ?
 O11 Zn1 O1 121(2) . . ?
 O11 Zn1 O14 108(3) . 2_766 ?
 O11 Zn1 O4 113.2(16) . 2_656 ?
 O11 Zn1 C14 100(2) . 2_766 ?
 C1 O1 Zn1 141(5) . . ?
 C14 O14 Zn1 114(5) . 2_766 ?
 C4 O4 Zn1 120.6(13) . 2_656 ?
 C11 O11 Zn1 128.4(16) . . ?
 H1WA O1W H1WB 109(10) . . ?
 H2WA O2W H2WB 114 . . ?
 H13A N13 H13B 109.5 . . ?
 H13A N13 H13C 109.5 . . ?
 H13B N13 H13C 109.5 . . ?
 C13 N13 H13A 107.0 . . ?
 C13 N13 H13B 111.0 . . ?
 C13 N13 H13C 109.5 . . ?
 H3A N3 H3B 109.5 . . ?
 H3A N3 H3C 109.5 . . ?
 H3B N3 H3C 107.0 . . ?
 C3 N3 H3A 116.0 . . ?
 C3 N3 H3B 103.0 . . ?
 C3 N3 H3C 111.0 . . ?
 O4 C4 C3 112.4(16) . . ?
 O3 C4 O4 126(3) . . ?
 O3 C4 C3 121.0(17) . . ?
 N13 C13 H13 113.0 . . ?
 N13 C13 C12 114(4) . . ?
 N13 C13 C14 107(5) . . ?
 C12 C13 H13 105.4 . . ?
 C12 C13 C14 118(4) . . ?
 C14 C13 H13 105.4 . . ?
 O11 C11 C12 113(3) . . ?
 O12 C11 O11 125(6) . . ?
 O12 C11 C12 121(4) . . ?
 C13 C12 C11 108(5) . . ?
 C13 C12 H12A 110.1 . . ?
 C13 C12 H12B 110.0 . . ?
 C11 C12 H12A 110.1 . . ?
 C11 C12 H12B 110.1 . . ?
 H12A C12 H12B 108.4 . . ?
 O14 C14 Zn1 39(4) . 2_766 ?
 O14 C14 C13 120(6) . . ?
 O13 C14 Zn1 91(6) . 2_766 ?
 O13 C14 O14 130(9) . . ?
 O13 C14 C13 110(6) . . ?
 C13 C14 Zn1 157(3) . 2_766 ?
 N3 C3 C4 103(4) . . ?
 N3 C3 H3 116.0 . . ?
 N3 C3 C2 114(3) . . ?
 C4 C3 H3 105.4 . . ?
 C2 C3 C4 114.9(16) . . ?
 C2 C3 H3 105.4 . . ?
 C3 C2 H2A 108.6 . . ?
 C3 C2 H2B 108.6 . . ?
 C3 C2 C1 115(2) . . ?
 H2A C2 H2B 107.5 . . ?
 C1 C2 H2A 108.5 . . ?
 C1 C2 H2B 108.6 . . ?
 O1 C1 O2 128(7) . . ?
 O1 C1 C2 119(5) . . ?
 O2 C1 C2 113(4) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O2 C1 C2 C3 32(3) . . . . ?
 O12 C11 C12 C13 150(8) . . . . ?
 N13 C13 C14 O13 21(8) . . . . ?
 N3 C3 C4 O3 -30(6) . . . . ?
 C11 C12 C13 N13 74(6) . . . . ?
 C11 C12 C13 C14 -53(4) . . . . ?
 C1 C2 C3 N3 -64(4) . . . . ?
 C1 C2 C3 C4 54(3) . . . . ?


_olex2_submission_special_instructions  'No special instructions were received'
# end


