The crystal structure of (C~2~H~9~N~2~)~2~[Zn~3~(HPO~3~)~4~], a three-dimensional zincophosphite framework containing 16-membered rings templated by the unsymmetrical dimethyl hydrazinium cation
Katinaitė, Judita; Harrison, William T. A.; Acta Crystallographica Section E 73 (2017) 759–762; doi:10.1107/S2056989017005758

data_2242168
_publ_section_title
;
 The crystal structure of (C~2~H~9~N~2~)~2~[Zn~3~(HPO~3~)~4~], a
 three-dimensional zincophosphite framework containing 16-membered rings
 templated by the unsymmetrical dimethyl hydrazinium cation
;
_journal_coeditor_code           SJ5526
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              759
_journal_page_last               762
_journal_paper_doi               10.1107/S2056989017005758
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '(C2 H9 N2)2 [Zn3 (H P O3)4]'
_chemical_formula_moiety         '2(C2 H9 N2 +), H4 O12 P4 Zn3 2-'
_chemical_formula_sum            'C4 H22 N4 O12 P4 Zn3'
_chemical_formula_weight         638.24
_chemical_name_systematic
;
1,1-Dimethylhydrazinium tetraphoshonoatotrizincate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.1560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1154(5)
_cell_length_b                   8.7269(3)
_cell_length_c                   16.1675(6)
_cell_measurement_reflns_used    6272
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.64
_cell_volume                     2026.48(12)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Shape Software,
2005)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2273
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.652
_exptl_absorpt_coefficient_mu    3.898
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.243
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0679
_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/[\s^2^(Fo^2^)+(0.1587P)^2^+13.6003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2392
_reflns_number_gt                2169
_reflns_number_total             2273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5526sup1.cif
_cod_data_source_block           I
_cod_database_code               2242168
_shelx_estimated_absorpt_t_min   0.525
_shelx_estimated_absorpt_t_max   0.829
_shelx_hkl_checksum              24757
_shelx_res_checksum              86084
_cod_database_fobs_code 2242168