##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section E. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section E, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     'SHELXL-2014/7'
_chemical_name_systematic
;
1,1-Dimethylhydrazinium tetraphoshonoatotrizincate(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     '2(C2 H9 N2 +), H4 O12 P4 Zn3 2-'
_chemical_formula_sum     'C4 H22 N4 O12 P4 Zn3'
_chemical_formula_iupac     '(C2 H9 N2)2 [Zn3 (H P O3)4]'
_chemical_formula_weight     638.24
_chemical_melting_point     ?
_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_name_H-M_alt     'C 2/c'
_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     15.1154(5)
_cell_length_b     8.7269(3)
_cell_length_c     16.1675(6)
_cell_angle_alpha     90
_cell_angle_beta     108.1560(10)
_cell_angle_gamma     90
_cell_volume     2026.48(12)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     6272
_cell_measurement_theta_min     2.64
_cell_measurement_theta_max     27.60
_cell_measurement_temperature     100(2)
_exptl_crystal_description     block
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.19
_exptl_crystal_size_mid     0.11
_exptl_crystal_size_min     0.05
_exptl_crystal_density_diffrn     2.092
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     1280
_exptl_absorpt_coefficient_mu     3.898
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2004)
;
_shelx_estimated_absorpt_T_min     0.525
_shelx_estimated_absorpt_T_max     0.829
_exptl_absorpt_correction_T_min     0.52654
_exptl_absorpt_correction_T_max     1.00000
_diffrn_ambient_temperature     100(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type     'Rigaku Mercury CCD'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     2273
_diffrn_reflns_av_R_equivalents     ?
_diffrn_reflns_theta_min     2.652
_diffrn_reflns_theta_max     27.508
_diffrn_reflns_theta_full     25.242
_diffrn_measured_fraction_theta_max     0.976
_diffrn_measured_fraction_theta_full     0.982
_diffrn_reflns_limit_h_min     -19
_diffrn_reflns_limit_h_max     18
_diffrn_reflns_limit_k_min     -11
_diffrn_reflns_limit_k_max     11
_diffrn_reflns_limit_l_min     -11
_diffrn_reflns_limit_l_max     20
_refine_special_details
;
Refined as a 2-component twin with components
rotated about (001) in reciprocal space
;
_reflns_number_total     2273
_reflns_number_gt     2169
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0792
_refine_ls_R_factor_gt     0.0679
_refine_ls_wR_factor_gt     0.1964
_refine_ls_wR_factor_ref     0.2392
_refine_ls_goodness_of_fit_ref     1.215
_refine_ls_restrained_S_all     1.215
_refine_ls_number_reflns     2273
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
             'w=1/[σ²(Fo²)+(0.1587P)²+13.6003P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     ?
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.507
_refine_diff_density_min     -1.243
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_extinction_coef     0.011(2)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
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'
    'P' 'P' 0.1023 0.0942
                         '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'
_computing_data_collection
;
CrysAlis PRO (Rigaku, 2015)
;
_computing_cell_refinement
;
CrysAlis PRO (Rigaku, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Shape Software,
2005)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Zn Zn1 0.0000 0.16565(13) 0.2500 0.0076(4) Uani d 1 . .
    Zn Zn2 0.36570(6) 0.37073(9) 0.48484(5) 0.0096(4) Uani d 1 . .
    P P1 0.15444(13) 0.3885(2) 0.37817(11) 0.0091(5) Uani d 1 . .
    H H1 0.1147 0.5248 0.3662 0.011 Uiso calc 1 . .
    P P2 -0.01597(13) -0.0917(2) 0.11747(11) 0.0088(5) Uani d 1 . .
    H H2 -0.0253 -0.1970 0.1728 0.011 Uiso calc 1 . .
    O O1 0.2557(4) 0.4152(7) 0.3858(3) 0.0193(12) Uani d 1 . .
    O O2 0.1393(5) 0.3246(6) 0.4592(3) 0.0180(12) Uani d 1 . .
    O O3 0.1081(4) 0.2975(7) 0.2948(3) 0.0160(11) Uani d 1 . .
    O O4 0.0428(4) 0.0362(6) 0.1728(3) 0.0146(11) Uani d 1 . .
    O O5 0.0321(4) -0.1690(6) 0.0604(4) 0.0169(12) Uani d 1 . .
    O O6 -0.1139(4) -0.0379(6) 0.0684(3) 0.0124(10) Uani d 1 . .
    C C1 0.1591(7) 0.2877(11) 0.0880(5) 0.028(2) Uani d 1 . .
    H H1A 0.1821 0.1825 0.1002 0.043 Uiso calc 1 . .
    H H1B 0.1847 0.3339 0.0452 0.043 Uiso calc 1 . .
    H H1C 0.0909 0.2867 0.0649 0.043 Uiso calc 1 . .
    C C2 0.1529(8) 0.5365(10) 0.1562(6) 0.029(2) Uani d 1 . .
    H H2A 0.1818 0.5963 0.2091 0.043 Uiso calc 1 . .
    H H2B 0.0852 0.5358 0.1439 0.043 Uiso calc 1 . .
    H H2C 0.1683 0.5827 0.1072 0.043 Uiso calc 1 . .
    N N1 0.2898(6) 0.3663(9) 0.2063(5) 0.0249(17) Uani d 1 . .
    H H1N 0.3067 0.3880 0.2642 0.030 Uiso d 1 . .
    H H2N 0.3170 0.4346 0.1793 0.030 Uiso d 1 . .
    N N2 0.1884(5) 0.3781(7) 0.1691(4) 0.0132(13) Uani d 1 . .
    H H3N 0.1608 0.3280 0.2110 0.016 Uiso calc 1 . .
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Zn1 O4 . 1.938(5) y
    Zn1 O4 2 1.938(5) y
    Zn1 O3 2 1.945(5) ?
    Zn1 O3 . 1.945(5) ?
    Zn2 O5 4 1.936(6) y
    Zn2 O2 7_556 1.943(5) y
    Zn2 O6 8_556 1.946(5) y
    Zn2 O1 . 1.954(6) y
    P1 O2 . 1.504(5) y
    P1 O1 . 1.515(6) y
    P1 O3 . 1.533(5) y
    P1 H1 . 1.3200 ?
    P2 O5 . 1.500(6) y
    P2 O6 . 1.520(5) y
    P2 O4 . 1.529(5) y
    P2 H2 . 1.3200 ?
    O2 Zn2 7_556 1.943(5) ?
    O5 Zn2 4_545 1.936(6) ?
    O6 Zn2 8_455 1.946(5) ?
    C1 N2 . 1.475(9) ?
    C1 H1A . 0.9800 ?
    C1 H1B . 0.9800 ?
    C1 H1C . 0.9800 ?
    C2 N2 . 1.474(10) ?
    C2 H2A . 0.9800 ?
    C2 H2B . 0.9800 ?
    C2 H2C . 0.9800 ?
    N1 N2 . 1.465(10) ?
    N1 H1N . 0.9100 ?
    N1 H2N . 0.9100 ?
    N2 H3N . 1.0000 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O4 Zn1 O4 . 2 108.7(3) ?
    O4 Zn1 O3 . 2 121.0(2) ?
    O4 Zn1 O3 2 2 100.0(2) ?
    O4 Zn1 O3 . . 100.0(2) ?
    O4 Zn1 O3 2 . 121.0(2) ?
    O3 Zn1 O3 2 . 107.4(4) ?
    O5 Zn2 O2 4 7_556 99.8(2) ?
    O5 Zn2 O6 4 8_556 115.1(2) ?
    O2 Zn2 O6 7_556 8_556 110.8(2) ?
    O5 Zn2 O1 4 . 107.5(3) ?
    O2 Zn2 O1 7_556 . 114.1(3) ?
    O6 Zn2 O1 8_556 . 109.3(2) ?
    O2 P1 O1 . . 114.2(3) ?
    O2 P1 O3 . . 115.0(3) ?
    O1 P1 O3 . . 108.9(3) ?
    O2 P1 H1 . . 106.0 ?
    O1 P1 H1 . . 106.0 ?
    O3 P1 H1 . . 106.0 ?
    O5 P2 O6 . . 113.4(3) ?
    O5 P2 O4 . . 112.6(3) ?
    O6 P2 O4 . . 111.9(3) ?
    O5 P2 H2 . . 106.1 ?
    O6 P2 H2 . . 106.1 ?
    O4 P2 H2 . . 106.1 ?
    P1 O1 Zn2 . . 128.0(3) y
    P1 O2 Zn2 . 7_556 140.3(3) y
    P1 O3 Zn1 . . 137.2(3) y
    P2 O4 Zn1 . . 123.6(3) y
    P2 O5 Zn2 . 4_545 138.4(4) y
    P2 O6 Zn2 . 8_455 120.8(3) y
    N2 C1 H1A . . 109.5 ?
    N2 C1 H1B . . 109.5 ?
    H1A C1 H1B . . 109.5 ?
    N2 C1 H1C . . 109.5 ?
    H1A C1 H1C . . 109.5 ?
    H1B C1 H1C . . 109.5 ?
    N2 C2 H2A . . 109.5 ?
    N2 C2 H2B . . 109.5 ?
    H2A C2 H2B . . 109.5 ?
    N2 C2 H2C . . 109.5 ?
    H2A C2 H2C . . 109.5 ?
    H2B C2 H2C . . 109.5 ?
    N2 N1 H1N . . 109.3 ?
    N2 N1 H2N . . 109.2 ?
    H1N N1 H2N . . 109.5 ?
    N1 N2 C2 . . 114.3(7) ?
    N1 N2 C1 . . 108.3(6) ?
    C2 N2 C1 . . 112.4(7) ?
    N1 N2 H3N . . 107.2 ?
    C2 N2 H3N . . 107.2 ?
    C1 N2 H3N . . 107.2 ?
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_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    O2 P1 O1 Zn2 . . . . 2.2(6) ?
    O3 P1 O1 Zn2 . . . . -127.8(4) ?
    O1 P1 O2 Zn2 . . . 7_556 -86.8(7) ?
    O3 P1 O2 Zn2 . . . 7_556 40.2(8) ?
    O2 P1 O3 Zn1 . . . . 28.0(7) ?
    O1 P1 O3 Zn1 . . . . 157.6(5) ?
    O5 P2 O4 Zn1 . . . . 177.2(3) ?
    O6 P2 O4 Zn1 . . . . 48.1(4) ?
    O6 P2 O5 Zn2 . . . 4_545 110.4(6) ?
    O4 P2 O5 Zn2 . . . 4_545 -18.0(7) ?
    O5 P2 O6 Zn2 . . . 8_455 -68.4(4) ?
    O4 P2 O6 Zn2 . . . 8_455 60.3(4) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    N1 H1N O1 . 0.91 2.34 3.130(9) 146
    N1 H2N O6 3 0.91 2.35 3.133(9) 144
    N2 H3N O3 . 1.00 1.79 2.762(8) 163
    C1 H1A O1 4_545 0.98 2.50 3.474(11) 173
    C1 H1C O5 5 0.98 2.50 3.295(11) 138
    C2 H2C O2 6_565 0.98 2.43 3.355(9) 157
data_global
_journal_date_recd_electronic     2017-04-14
_journal_date_accepted     2017-04-16
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2017
_journal_volume     73
_journal_issue      5
_journal_page_first     759
_journal_page_last     762
_journal_paper_category     GM
_journal_paper_doi     10.1107/S2056989017005758
_journal_coeditor_code     SJ5526
_publ_contact_author_name     'William T A Harrison'
_publ_contact_author_address
;
Department of Chemistry
University of Aberdeen
Meston Walk
Aberdeen AB24 3UE
Scotland
;
_publ_contact_author_email     w.harrison@abdn.ac.uk
_publ_contact_author_fax     ?
_publ_contact_author_phone     ?
_publ_section_title
;
The crystal structure of (C₂H₉N₂)₂[Zn₃(HPO₃)₄], a
three-dimensional zincophosphite framework containing 16-membered rings
templated by the unsymmetrical dimethyl hydrazinium cation
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Katinaitė, Judita' .
;
Department of Chemistry
University of Aberdeen
Meston Walk
Aberdeen AB24 3UE
Scotland
;
    'Harrison, William T. A.' .
;
Department of Chemistry
University of Aberdeen
Meston Walk
Aberdeen AB24 3UE
Scotland
;
_publ_section_synopsis
;
The title open framework contains 16-ring pores templated by pairs of
side-by-side unsymmetrical dimethyl hydrazinium cations.
;
