data_global

_audit_update_record
;
2020-06-09 # Formatted by IUCr publCIF

;
_publcif_datablock.id '{af904e04-2fdb-4e58-8fa3-f2c677137f9c}'

# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents

 section 
;
Introduction
; 
;

;
 section 
;
Experimental
; 
;

;
 subsection 
;
Synthesis and crystallization
; 
;

;
 subsection 
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1.
;

 section 
;
Results and discussion
; 
;

;
# publcif _publ_body_element loop end

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

_publ_contact_author
;
Muhammad Nawaz Tahir
University of Sargodha
Department of Physics
Sargodha
Pakistan
;
_publ_contact_author_phone       '0092 48 92 30 914'
_publ_contact_author_fax         '0092 48 32 22 121'
_publ_contact_author_email       'dmntahir_uos@yahoo.com'
_publ_requested_journal          ''
_journal_date_recd_electronic      2020-01-27

_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted     2020-05-14

_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?

_journal_coeditor_name            ?
_journal_coeditor_code      BM5124SUP1
_journal_paper_category      FA
_journal_coeditor_notes
;
;

_journal_techeditor_code      B200647
_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         ?
#==============================================================

 loop_
_publ_author_name
_publ_author_address

 'Muhammad Nawaz Tahir'
;
Department of Physics
University of Sargodha
Sargodha-40100
Pakistan
;

'Shafaat Hussain Mirza'
;
Department of Physics
University of Sargodha
Sargodha-40100
Pakistan
;

'Akbar Ali'
;
Department of Chemistry
University of Sargodha
Sargodha-40100
Pakistan
;

'Muhammad Khalid'
;
Department of Chemistry, 
Khwaja Fareed University of Engineering & Information Technology, 
Rahim Yar Khan-64200, 
Pakistan
;

'Muhammad Usman Khan'
;
Department of Applied Chemistry, 
Government College University, 
Faisalabad-38000, 
Pakistan
;

 ' Ataualpa Albert Carmo Braga'
;
Departamento de Quimica Fundamental, 
Instituto de Quimica, 
Universidade de Sao Paulo, 
Avenida Professor Lineu Prestes, 748, 
Sao Paulo 05508-000, 
Brazil
; 

_audit_creation_date             ?
_audit_creation_method           ?
#==============================================================================

# TEXT

_publ_section_title
;
Diaqua-bis(pyridine-2-carboxamide-N,O)-nickel(ii)
bis(2,6-pyridinedicarboxylato)-nickel(ii) 4.67-hydrate
;

_publ_section_abstract 
;

; 


_publ_section_exptl_refinement 
;

;

_publ_section_exptl_prep
;

;

_publ_section_related_literature
;
;

_publ_section_references
;
Bruker (2005). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison,
Wisconsin, USA.

Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.

Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.

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

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

Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;

_publ_section_figure_captions
;

;
_publ_section_acknowledgements
;
?
;

data_I
_publcif_datablock.id '{c0f4e083-065d-4891-8c57-d8e66a4a1f82}'
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_common     ?
_chemical_absolute_configuration   .
_chemical_name_systematic
;
Diaqua-bis(pyridine-2-carboxamide-N,O)-nickel(ii) 
bis(2,6-pyridinedicarboxylato)-nickel(ii) 4.67-hydrate
;
_chemical_formula_moiety  'C14 H6 N2 Ni O8, C12 H16 N4 Ni O4, 4.67(H2 O)'
_chemical_formula_sum       'C26 H31.34 N6 Ni2 O16.67'
_chemical_formula_iupac     'C26 H31.34 N6 Ni2 O16.67'
_chemical_formula_weight                     813.49 #811.97

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'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    10.1294(7)
_cell_length_b                    12.2011(9)
_cell_length_c                    14.2430(11)
_cell_angle_alpha                 82.035(4)
_cell_angle_beta                  74.232(3)
_cell_angle_gamma                 79.373(3)
_cell_volume                      1657.7(2)
_cell_formula_units_Z             2
_cell_measurement_reflns_used            5643
_cell_measurement_theta_min             2.159
_cell_measurement_theta_max            27.526 
_cell_measurement_temperature     296(2)
_exptl_crystal_description         prism 
_exptl_crystal_colour         'blue'
_exptl_crystal_size_max     0.38
_exptl_crystal_size_mid     0.20
_exptl_crystal_size_min     0.18
_exptl_crystal_density_diffrn     1.627 
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000                       839 
_exptl_absorpt_coefficient_mu       1.221
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Bruker, 2005)'
_exptl_absorpt_correction_T_min     0.640 
_exptl_absorpt_correction_T_max     0.840 
_exptl_special_details  
;
;


_diffrn_ambient_temperature     296(2)
_diffrn_radiation_type      MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type 'Bruker Kappa APEXII CCD'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean  0.76
_diffrn_reflns_number             20962
_diffrn_reflns_av_unetI/netI      0.0601
_diffrn_reflns_av_R_equivalents   0.0472
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.159
_diffrn_reflns_theta_max          27.526
_diffrn_reflns_theta_full         27.526 
_diffrn_measured_fraction_theta_max   0.993 
_diffrn_measured_fraction_theta_full  0.993
_diffrn_standards_number     0
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?

_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 >
σ(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.
;
_reflns_number_total              7584
_reflns_number_gt                 5642
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all           0.0612
_refine_ls_R_factor_gt            0.0406
_refine_ls_wR_factor_ref          0.1126
_refine_ls_wR_factor_gt           0.1015
_refine_ls_goodness_of_fit_ref    1.025
_refine_ls_restrained_S_all       1.025
_refine_ls_number_reflns          7584
_refine_ls_number_parameters      515
_refine_ls_number_restraints      18
_refine_ls_hydrogen_treatment    mixed 
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0540P)²+0.0685P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max       0.001
_refine_ls_shift/su_mean      0.000
_computing_data_collection     'APEX2 (Bruker, 2007)'
_computing_cell_refinement     'SAINT (Bruker, 2007)'
_computing_data_reduction      'SAINT (Bruker, 2007)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL-2014/6  (Sheldrick, 2015)'
_computing_molecular_graphics     
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material   
;
WinGX (Farrugia, 1999) and PLATON (Spek, 2009)
;

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
Ni1 Ni 0.26869(3) 0.49927(3) 0.25271(2) 0.02749(10) Uani 1 1 d . . . . .
O1 O 0.15048(19) 0.36721(16) 0.32202(14) 0.0360(4) Uani 1 1 d . . . . .
O2 O 0.0623(2) 0.28291(17) 0.46869(14) 0.0427(5) Uani 1 1 d . . . . .
O3 O 0.36664(19) 0.64061(16) 0.24888(14) 0.0382(5) Uani 1 1 d . . . . .
O4 O 0.3919(2) 0.75572(18) 0.35097(16) 0.0519(6) Uani 1 1 d . . . . .
O5 O 0.45482(19) 0.38287(17) 0.21684(15) 0.0414(5) Uani 1 1 d . . . . .
O6 O 0.5781(2) 0.27569(19) 0.09867(18) 0.0541(6) Uani 1 1 d . . . . .
O7 O 0.09136(18) 0.61167(15) 0.22332(13) 0.0344(4) Uani 1 1 d . . . . .
O8 O -0.0027(2) 0.68393(18) 0.09874(15) 0.0453(5) Uani 1 1 d . . . . .
N1 N 0.2475(2) 0.50913(17) 0.39231(15) 0.0281(5) Uani 1 1 d . . . . .
N2 N 0.2832(2) 0.47969(17) 0.11548(15) 0.0279(5) Uani 1 1 d . . . . .
C1 C 0.1276(3) 0.3538(2) 0.4139(2) 0.0316(6) Uani 1 1 d . . . . .
C2 C 0.1858(3) 0.4340(2) 0.45899(18) 0.0293(6) Uani 1 1 d . . . . .
C3 C 0.1804(3) 0.4343(3) 0.5567(2) 0.0445(7) Uani 1 1 d . . . . .
H3 H 0.1372 0.3820 0.6031 0.053 Uiso 1 1 calc R U . . .
C4 C 0.2403(4) 0.5138(3) 0.5845(2) 0.0535(9) Uani 1 1 d . . . . .
H4 H 0.2392 0.5146 0.6499 0.064 Uiso 1 1 calc R U . . .
C5 C 0.3016(3) 0.5917(3) 0.5144(2) 0.0439(7) Uani 1 1 d . . . . .
H5 H 0.3420 0.6457 0.5319 0.053 Uiso 1 1 calc R U . . .
C6 C 0.3021(3) 0.5883(2) 0.4189(2) 0.0315(6) Uani 1 1 d . . . . .
C7 C 0.3592(3) 0.6686(2) 0.3325(2) 0.0365(6) Uani 1 1 d . . . . .
C8 C 0.4823(3) 0.3496(2) 0.1330(2) 0.0372(6) Uani 1 1 d . . . . .
C9 C 0.3845(3) 0.4048(2) 0.0699(2) 0.0331(6) Uani 1 1 d . . . . .
C10 C 0.3945(3) 0.3837(3) -0.0244(2) 0.0476(8) Uani 1 1 d . . . . .
H10 H 0.4662 0.3318 -0.0562 0.057 Uiso 1 1 calc R U . . .
C11 C 0.2948(3) 0.4421(3) -0.0708(2) 0.0530(8) Uani 1 1 d . . . . .
H11 H 0.2995 0.4298 -0.1347 0.064 Uiso 1 1 calc R U . . .
C12 C 0.1884(3) 0.5184(3) -0.0218(2) 0.0436(7) Uani 1 1 d . . . . .
H12 H 0.1199 0.5568 -0.0515 0.052 Uiso 1 1 calc R U . . .
C13 C 0.1866(3) 0.5360(2) 0.07185(19) 0.0293(5) Uani 1 1 d . . . . .
C14 C 0.0821(3) 0.6173(2) 0.1356(2) 0.0328(6) Uani 1 1 d . . . . .
Ni2 Ni 0.09828(3) 0.07788(3) 0.71413(2) 0.02964(10) Uani 1 1 d . . . . .
O9 O 0.1893(2) -0.06232(17) 0.78693(16) 0.0446(5) Uani 1 1 d . . . . .
O10 O 0.04663(18) -0.03287(16) 0.63522(15) 0.0395(5) Uani 1 1 d . . . . .
O11 O 0.1795(2) 0.1826(2) 0.77421(17) 0.0455(5) Uani 1 1 d D . . . .
H11A H 0.2523(19) 0.166(3) 0.790(2) 0.055 Uiso 1 1 d D U . . .
H11B H 0.130(3) 0.223(2) 0.814(2) 0.055 Uiso 1 1 d D U . . .
O12 O -0.02329(19) 0.21512(16) 0.66076(15) 0.0340(4) Uani 1 1 d D . . . .
H12A H -0.034(3) 0.2682(17) 0.691(2) 0.041 Uiso 1 1 d D U . . .
H12B H 0.007(3) 0.239(2) 0.6049(10) 0.041 Uiso 1 1 d D U . . .
N3 N -0.0662(2) 0.05063(18) 0.83220(16) 0.0313(5) Uani 1 1 d . . . . .
N4 N 0.2550(2) 0.08274(18) 0.58697(16) 0.0302(5) Uani 1 1 d . . . . .
N5 N 0.1445(3) -0.1874(2) 0.9188(2) 0.0483(7) Uani 1 1 d D . . . .
H5A H 0.2309(14) -0.218(3) 0.905(2) 0.058 Uiso 1 1 d D U . . .
H5B H 0.079(2) -0.213(3) 0.9649(18) 0.058 Uiso 1 1 d D U . . .
N6 N 0.1393(3) -0.1384(2) 0.5094(2) 0.0451(6) Uani 1 1 d D . . . .
H6A H 0.074(2) -0.178(2) 0.528(2) 0.054 Uiso 1 1 d D U . . .
H6B H 0.210(2) -0.151(3) 0.4611(17) 0.054 Uiso 1 1 d D U . . .
C15 C 0.1056(3) -0.0996(2) 0.8623(2) 0.0370(6) Uani 1 1 d . . . . .
C16 C -0.0417(3) -0.0418(2) 0.8900(2) 0.0344(6) Uani 1 1 d . . . . .
C17 C -0.1426(3) -0.0800(3) 0.9671(2) 0.0503(8) Uani 1 1 d . . . . .
H17 H -0.1223 -0.1454 1.0061 0.060 Uiso 1 1 calc R U . . .
C18 C -0.2759(3) -0.0187(3) 0.9856(2) 0.0562(9) Uani 1 1 d . . . . .
H18 H -0.3465 -0.0425 1.0370 0.067 Uiso 1 1 calc R U . . .
C19 C -0.3013(3) 0.0774(3) 0.9264(2) 0.0495(8) Uani 1 1 d . . . . .
H19 H -0.3890 0.1206 0.9381 0.059 Uiso 1 1 calc R U . . .
C20 C -0.1964(3) 0.1089(3) 0.8504(2) 0.0424(7) Uani 1 1 d . . . . .
H20 H -0.2150 0.1729 0.8095 0.051 Uiso 1 1 calc R U . . .
C21 C 0.1374(3) -0.0550(2) 0.5581(2) 0.0326(6) Uani 1 1 d . . . . .
C22 C 0.2481(3) 0.0183(2) 0.5200(2) 0.0325(6) Uani 1 1 d . . . . .
C23 C 0.3319(3) 0.0229(3) 0.4265(2) 0.0457(7) Uani 1 1 d . . . . .
H23 H 0.3247 -0.0229 0.3817 0.055 Uiso 1 1 calc R U . . .
C24 C 0.4278(3) 0.0969(3) 0.3997(2) 0.0526(8) Uani 1 1 d . . . . .
H24 H 0.4853 0.1021 0.3365 0.063 Uiso 1 1 calc R U . . .
C25 C 0.4358(3) 0.1621(3) 0.4682(2) 0.0482(8) Uani 1 1 d . . . . .
H25 H 0.4994 0.2121 0.4522 0.058 Uiso 1 1 calc R U . . .
C26 C 0.3492(3) 0.1532(2) 0.5608(2) 0.0392(7) Uani 1 1 d . . . . .
H26 H 0.3559 0.1974 0.6070 0.047 Uiso 1 1 calc R U . . .
O13 O 0.6818(3) 0.2837(3) 0.3017(2) 0.0702(8) Uani 1 1 d D . . . .
H13A H 0.610(2) 0.305(4) 0.285(3) 0.084 Uiso 1 1 d D U . . .
H13B H 0.700(4) 0.229(2) 0.271(3) 0.070 Uiso 1 1 d D U . . .
O14 O 0.4502(3) 0.0784(3) 0.1621(3) 0.0875(9) Uani 1 1 d D . . . .
H14A H 0.3648(13) 0.095(4) 0.184(3) 0.105 Uiso 1 1 d D U . . .
H14B H 0.494(4) 0.129(3) 0.135(3) 0.105 Uiso 1 1 d D U . . .
O15 O 0.9395(6) 0.3782(6) 0.2050(4) 0.107(3) Uani 0.670(8) 1 d D . P . .
H15A H 0.984(8) 0.332(6) 0.235(6) 0.129 Uiso 0.670(8) 1 d D U P . .
H15B H 0.864(4) 0.358(7) 0.224(6) 0.129 Uiso 0.670(8) 1 d D U P . .
O16 O 0.4325(2) 0.1375(2) 0.8005(2) 0.0620(7) Uani 1 1 d D . . . .
H16A H 0.468(4) 0.0721(13) 0.804(3) 0.074 Uiso 1 1 d D U . . .
H16B H 0.493(3) 0.166(3) 0.760(2) 0.074 Uiso 1 1 d D U . . .
O17 O 0.1736(3) 0.1601(3) 0.2442(3) 0.0897(10) Uani 1 1 d D . . . .
H17A H 0.122(4) 0.121(4) 0.283(3) 0.108 Uiso 1 1 d D U . . .
H17B H 0.172(5) 0.2251(16) 0.254(4) 0.108 Uiso 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
Ni1 N1 1.959(2) . ?
Ni1 N2 1.964(2) . ?
Ni1 O5 2.1266(19) . ?
Ni1 O3 2.1301(18) . ?
Ni1 O7 2.1502(17) . ?
Ni1 O1 2.1524(17) . ?
O1 C1 1.257(3) . ?
O2 C1 1.240(3) . ?
O3 C7 1.263(3) . ?
O4 C7 1.250(3) . ?
O5 C8 1.257(4) . ?
O6 C8 1.239(3) . ?
O7 C14 1.269(3) . ?
O8 C14 1.243(3) . ?
N1 C2 1.334(3) . ?
N1 C6 1.340(3) . ?
N2 C9 1.328(3) . ?
N2 C13 1.335(3) . ?
C1 C2 1.521(3) . ?
C2 C3 1.377(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.380(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.365(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.516(4) . ?
C8 C9 1.520(4) . ?
C9 C10 1.376(4) . ?
C10 C11 1.390(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.375(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.507(4) . ?
Ni2 O11 2.029(2) . ?
Ni2 N3 2.059(2) . ?
Ni2 N4 2.061(2) . ?
Ni2 O12 2.0721(19) . ?
Ni2 O9 2.073(2) . ?
Ni2 O10 2.089(2) . ?
O9 C15 1.261(3) . ?
O10 C21 1.251(3) . ?
O11 H11A 0.807(10) . ?
O11 H11B 0.805(10) . ?
O12 H12A 0.806(10) . ?
O12 H12B 0.805(10) . ?
N3 C16 1.327(3) . ?
N3 C20 1.353(3) . ?
N4 C22 1.340(3) . ?
N4 C26 1.345(3) . ?
N5 C15 1.314(4) . ?
N5 H5A 0.866(10) . ?
N5 H5B 0.867(10) . ?
N6 C21 1.304(4) . ?
N6 H6A 0.850(10) . ?
N6 H6B 0.853(10) . ?
C15 C16 1.500(4) . ?
C16 C17 1.376(4) . ?
C17 C18 1.393(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.373(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.363(4) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.501(4) . ?
C22 C23 1.371(4) . ?
C23 C24 1.390(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.369(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.373(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
O13 H13A 0.810(10) . ?
O13 H13B 0.810(10) . ?
O14 H14A 0.831(10) . ?
O14 H14B 0.821(10) . ?
O15 H15A 0.813(10) . ?
O15 H15B 0.812(10) . ?
O16 H16A 0.814(10) . ?
O16 H16B 0.809(10) . ?
O17 H17A 0.821(10) . ?
O17 H17B 0.819(10) . ?
 
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
N1 Ni1 N2 175.84(8) . . ?
N1 Ni1 O5 101.70(8) . . ?
N2 Ni1 O5 77.93(8) . . ?
N1 Ni1 O3 78.20(8) . . ?
N2 Ni1 O3 105.96(8) . . ?
O5 Ni1 O3 96.18(8) . . ?
N1 Ni1 O7 103.04(8) . . ?
N2 Ni1 O7 77.40(8) . . ?
O5 Ni1 O7 155.26(8) . . ?
O3 Ni1 O7 88.89(7) . . ?
N1 Ni1 O1 77.24(8) . . ?
N2 Ni1 O1 98.61(8) . . ?
O5 Ni1 O1 91.61(8) . . ?
O3 Ni1 O1 155.27(7) . . ?
O7 Ni1 O1 93.79(7) . . ?
C1 O1 Ni1 114.82(16) . . ?
C7 O3 Ni1 113.96(16) . . ?
C8 O5 Ni1 114.53(17) . . ?
C14 O7 Ni1 114.18(16) . . ?
C2 N1 C6 120.9(2) . . ?
C2 N1 Ni1 119.94(17) . . ?
C6 N1 Ni1 119.04(17) . . ?
C9 N2 C13 121.2(2) . . ?
C9 N2 Ni1 119.00(18) . . ?
C13 N2 Ni1 119.67(17) . . ?
O2 C1 O1 125.9(2) . . ?
O2 C1 C2 118.8(2) . . ?
O1 C1 C2 115.2(2) . . ?
N1 C2 C3 120.6(2) . . ?
N1 C2 C1 112.5(2) . . ?
C3 C2 C1 126.9(2) . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
N1 C6 C5 121.1(2) . . ?
N1 C6 C7 112.1(2) . . ?
C5 C6 C7 126.8(2) . . ?
O4 C7 O3 126.9(3) . . ?
O4 C7 C6 117.2(3) . . ?
O3 C7 C6 115.9(2) . . ?
O6 C8 O5 126.5(3) . . ?
O6 C8 C9 117.9(3) . . ?
O5 C8 C9 115.6(2) . . ?
N2 C9 C10 121.1(3) . . ?
N2 C9 C8 112.6(2) . . ?
C10 C9 C8 126.2(3) . . ?
C9 C10 C11 118.3(3) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 118.3(3) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
N2 C13 C12 121.1(2) . . ?
N2 C13 C14 112.8(2) . . ?
C12 C13 C14 126.1(2) . . ?
O8 C14 O7 126.0(3) . . ?
O8 C14 C13 118.4(2) . . ?
O7 C14 C13 115.6(2) . . ?
O11 Ni2 N3 97.61(9) . . ?
O11 Ni2 N4 91.83(9) . . ?
N3 Ni2 N4 170.32(9) . . ?
O11 Ni2 O12 89.37(9) . . ?
N3 Ni2 O12 90.22(8) . . ?
N4 Ni2 O12 92.02(8) . . ?
O11 Ni2 O9 92.10(9) . . ?
N3 Ni2 O9 79.87(8) . . ?
N4 Ni2 O9 97.73(8) . . ?
O12 Ni2 O9 170.09(8) . . ?
O11 Ni2 O10 170.45(8) . . ?
N3 Ni2 O10 91.54(8) . . ?
N4 Ni2 O10 78.94(8) . . ?
O12 Ni2 O10 93.35(8) . . ?
O9 Ni2 O10 86.80(8) . . ?
C15 O9 Ni2 112.71(17) . . ?
C21 O10 Ni2 113.37(16) . . ?
Ni2 O11 H11A 124(2) . . ?
Ni2 O11 H11B 120(2) . . ?
H11A O11 H11B 106(3) . . ?
Ni2 O12 H12A 112(2) . . ?
Ni2 O12 H12B 116(2) . . ?
H12A O12 H12B 104(3) . . ?
C16 N3 C20 118.0(2) . . ?
C16 N3 Ni2 114.15(17) . . ?
C20 N3 Ni2 127.43(18) . . ?
C22 N4 C26 118.1(2) . . ?
C22 N4 Ni2 114.60(16) . . ?
C26 N4 Ni2 126.64(19) . . ?
C15 N5 H5A 119(2) . . ?
C15 N5 H5B 116(2) . . ?
H5A N5 H5B 125(3) . . ?
C21 N6 H6A 120(2) . . ?
C21 N6 H6B 116(2) . . ?
H6A N6 H6B 124(3) . . ?
O9 C15 N5 121.7(3) . . ?
O9 C15 C16 119.7(2) . . ?
N5 C15 C16 118.6(3) . . ?
N3 C16 C17 122.8(3) . . ?
N3 C16 C15 113.3(2) . . ?
C17 C16 C15 123.9(3) . . ?
C16 C17 C18 118.5(3) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C19 C18 C17 118.8(3) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C20 C19 C18 119.2(3) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
N3 C20 C19 122.6(3) . . ?
N3 C20 H20 118.7 . . ?
C19 C20 H20 118.7 . . ?
O10 C21 N6 122.8(2) . . ?
O10 C21 C22 118.5(2) . . ?
N6 C21 C22 118.8(3) . . ?
N4 C22 C23 122.4(2) . . ?
N4 C22 C21 112.7(2) . . ?
C23 C22 C21 124.8(3) . . ?
C22 C23 C24 119.1(3) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C25 C24 C23 118.5(3) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C24 C25 C26 119.5(3) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
N4 C26 C25 122.3(3) . . ?
N4 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
H13A O13 H13B 92(4) . . ?
H14A O14 H14B 118(5) . . ?
H15A O15 H15B 101(8) . . ?
H16A O16 H16B 102(4) . . ?
H17A O17 H17B 120(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
Ni1 O1 C1 O2 -179.8(2) . . . . ?
Ni1 O1 C1 C2 0.8(3) . . . . ?
C6 N1 C2 C3 -1.8(4) . . . . ?
Ni1 N1 C2 C3 174.6(2) . . . . ?
C6 N1 C2 C1 178.4(2) . . . . ?
Ni1 N1 C2 C1 -5.1(3) . . . . ?
O2 C1 C2 N1 -176.9(2) . . . . ?
O1 C1 C2 N1 2.6(3) . . . . ?
O2 C1 C2 C3 3.4(4) . . . . ?
O1 C1 C2 C3 -177.1(3) . . . . ?
N1 C2 C3 C4 -0.2(5) . . . . ?
C1 C2 C3 C4 179.5(3) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C2 N1 C6 C5 2.8(4) . . . . ?
Ni1 N1 C6 C5 -173.6(2) . . . . ?
C2 N1 C6 C7 -176.7(2) . . . . ?
Ni1 N1 C6 C7 6.9(3) . . . . ?
C4 C5 C6 N1 -1.8(5) . . . . ?
C4 C5 C6 C7 177.6(3) . . . . ?
Ni1 O3 C7 O4 -170.3(2) . . . . ?
Ni1 O3 C7 C6 8.6(3) . . . . ?
N1 C6 C7 O4 168.7(2) . . . . ?
C5 C6 C7 O4 -10.7(4) . . . . ?
N1 C6 C7 O3 -10.3(3) . . . . ?
C5 C6 C7 O3 170.3(3) . . . . ?
Ni1 O5 C8 O6 -173.8(2) . . . . ?
Ni1 O5 C8 C9 4.5(3) . . . . ?
C13 N2 C9 C10 0.9(4) . . . . ?
Ni1 N2 C9 C10 176.4(2) . . . . ?
C13 N2 C9 C8 -179.4(2) . . . . ?
Ni1 N2 C9 C8 -3.9(3) . . . . ?
O6 C8 C9 N2 177.7(2) . . . . ?
O5 C8 C9 N2 -0.8(4) . . . . ?
O6 C8 C9 C10 -2.6(4) . . . . ?
O5 C8 C9 C10 178.9(3) . . . . ?
N2 C9 C10 C11 -0.7(5) . . . . ?
C8 C9 C10 C11 179.7(3) . . . . ?
C9 C10 C11 C12 -0.5(5) . . . . ?
C10 C11 C12 C13 1.4(5) . . . . ?
C9 N2 C13 C12 0.0(4) . . . . ?
Ni1 N2 C13 C12 -175.5(2) . . . . ?
C9 N2 C13 C14 -179.5(2) . . . . ?
Ni1 N2 C13 C14 5.0(3) . . . . ?
C11 C12 C13 N2 -1.2(4) . . . . ?
C11 C12 C13 C14 178.3(3) . . . . ?
Ni1 O7 C14 O8 -172.5(2) . . . . ?
Ni1 O7 C14 C13 6.4(3) . . . . ?
N2 C13 C14 O8 171.4(2) . . . . ?
C12 C13 C14 O8 -8.1(4) . . . . ?
N2 C13 C14 O7 -7.6(3) . . . . ?
C12 C13 C14 O7 172.9(3) . . . . ?
Ni2 O9 C15 N5 -179.3(2) . . . . ?
Ni2 O9 C15 C16 -0.3(3) . . . . ?
C20 N3 C16 C17 -0.2(4) . . . . ?
Ni2 N3 C16 C17 -173.7(2) . . . . ?
C20 N3 C16 C15 179.6(2) . . . . ?
Ni2 N3 C16 C15 6.1(3) . . . . ?
O9 C15 C16 N3 -4.0(4) . . . . ?
N5 C15 C16 N3 175.0(3) . . . . ?
O9 C15 C16 C17 175.8(3) . . . . ?
N5 C15 C16 C17 -5.2(4) . . . . ?
N3 C16 C17 C18 -0.3(5) . . . . ?
C15 C16 C17 C18 179.9(3) . . . . ?
C16 C17 C18 C19 -0.2(5) . . . . ?
C17 C18 C19 C20 1.3(5) . . . . ?
C16 N3 C20 C19 1.3(5) . . . . ?
Ni2 N3 C20 C19 173.8(2) . . . . ?
C18 C19 C20 N3 -1.9(5) . . . . ?
Ni2 O10 C21 N6 165.6(2) . . . . ?
Ni2 O10 C21 C22 -14.9(3) . . . . ?
C26 N4 C22 C23 -0.8(4) . . . . ?
Ni2 N4 C22 C23 170.8(2) . . . . ?
C26 N4 C22 C21 -179.1(2) . . . . ?
Ni2 N4 C22 C21 -7.5(3) . . . . ?
O10 C21 C22 N4 15.4(4) . . . . ?
N6 C21 C22 N4 -165.0(3) . . . . ?
O10 C21 C22 C23 -162.9(3) . . . . ?
N6 C21 C22 C23 16.6(4) . . . . ?
N4 C22 C23 C24 0.0(5) . . . . ?
C21 C22 C23 C24 178.1(3) . . . . ?
C22 C23 C24 C25 0.6(5) . . . . ?
C23 C24 C25 C26 -0.3(5) . . . . ?
C22 N4 C26 C25 1.0(4) . . . . ?
Ni2 N4 C26 C25 -169.4(2) . . . . ?
C24 C25 C26 N4 -0.5(5) . . . . ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C5 H5 O13  0.93 2.57 3.261(4) 131.8 2_666
C12 H12 O15  0.93 2.41 3.225(6) 145.6 2_665
O11 H11A O16  0.807(10) 1.839(12) 2.637(3) 169(3) .
O11 H11B O8  0.805(10) 1.865(11) 2.667(3) 175(3) 2_566
O12 H12A O7  0.806(10) 1.938(12) 2.735(3) 170(3) 2_566
O12 H12B O2  0.805(10) 1.897(11) 2.696(3) 172(3) .
N5 H5A O6  0.866(10) 1.922(13) 2.775(3) 168(3) 2_656
N5 H5B O8  0.867(10) 2.181(17) 2.988(3) 155(3) 1_546
N6 H6A O2  0.850(10) 2.039(14) 2.864(3) 164(3) 2_556
N6 H6B O4  0.853(10) 2.303(15) 3.123(4) 161(3) 1_545
C17 H17 O8  0.93 2.59 3.501(4) 165.6 1_546
C20 H20 O12  0.93 2.52 3.057(3) 117.0 .
C25 H25 O13  0.93 2.59 3.348(4) 139.3 .
C26 H26 O11  0.93 2.57 3.092(4) 116.2 .
O13 H13A O5  0.810(10) 2.086(15) 2.879(3) 166(4) .
O13 H13B O9  0.810(10) 2.281(17) 3.057(4) 161(4) 2_656
O14 H14A O17  0.831(10) 1.961(15) 2.779(4) 168(5) .
O14 H14B O6  0.821(10) 2.060(16) 2.864(4) 166(5) .
O15 H15A O1  0.813(10) 2.46(7) 3.022(5) 127(8) 1_655
O15 H15A O17  0.813(10) 2.58(5) 3.316(8) 152(9) 1_655
O15 H15B O13  0.812(10) 2.16(2) 2.959(6) 167(8) .
O16 H16A O14  0.814(10) 1.923(14) 2.726(4) 169(4) 2_656
O16 H16B O4  0.809(10) 1.943(13) 2.740(3) 168(4) 2_666
O17 H17A O10  0.821(10) 2.159(15) 2.965(3) 167(5) 2_556
O17 H17B O1  0.819(10) 2.052(19) 2.844(4) 162(5) .
 
_refine_diff_density_max    0.643
_refine_diff_density_min   -0.344
_refine_diff_density_rms    0.071



_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n

loop_
_publcif_info_cif.paper_type
 CB

loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
"{af904e04-2fdb-4e58-8fa3-f2c677137f9c}" "_publcif_info_datablock.publ_exptl"
"{c0f4e083-065d-4891-8c57-d8e66a4a1f82}" "_geom_hbond_atom_site_label_D"

loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
'{c0f4e083-065d-4891-8c57-d8e66a4a1f82}' y y y
'{af904e04-2fdb-4e58-8fa3-f2c677137f9c}' ? ? ?

loop_
_publcif_info_exptl_table_extra_item
F000
Specimen_density
Cell_measurement_reflections
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
Datablock_name



_publcif_funding_html
;
;
