Crystal structure of poly[bis(1-methyl-[4,4′-bipyridin]-1-ium-κN)-tetrakis(μ3-sulfato-κ3 O:O′:O′′)trizinc(II)], C22H22Zn3N4O16S4
Fu, Hong-Ru; Wang, Kai-Lu; Zhao, Xiao-Xiao; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 349–351; doi:10.1515/ncrs-2017-0177

data_8106149
_publ_section_title
;
 Crystal structure of
 poly[bis(1-methyl-[4,4&#x2032;-bipyridin]-1-ium-\kN)-tetrakis(\m3-sulfato-\k3
 O:O&#x2032;:O&#x2032;&#x2032;)trizinc(II)], C22H22Zn3N4O16S4
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              349
_journal_page_last               351
_journal_paper_doi               10.1515/ncrs-2017-0177
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C22 H22 N4 O16 S4 Zn3'
_chemical_formula_sum            'C22 H22 N4 O16 S4 Zn3'
_chemical_formula_weight         922.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 98.924(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2909(2)
_cell_length_b                   16.8888(4)
_cell_length_c                   19.3547(6)
_cell_measurement_reflns_used    5881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6510
_cell_measurement_theta_min      3.7700
_cell_volume                     3000.22(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      5.00  73.00   1.00    8.00    --   13.55  19.00 -30.00   68
  2  \w    -16.00  61.00   1.00    8.00    --   13.55  19.00 120.00   77
  3  \w    -20.00  13.00   1.00    8.00    --  -12.53 -99.00  60.00   33
  4  \w     58.00  83.00   1.00    8.00    --   13.55 178.00  60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0315670000
_diffrn_orient_matrix_UB_12      -0.0362333000
_diffrn_orient_matrix_UB_13      0.0132895000
_diffrn_orient_matrix_UB_21      -0.0203095000
_diffrn_orient_matrix_UB_22      -0.0177320000
_diffrn_orient_matrix_UB_23      -0.0332868000
_diffrn_orient_matrix_UB_31      0.0676179000
_diffrn_orient_matrix_UB_32      0.0116002000
_diffrn_orient_matrix_UB_33      -0.0095683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11771
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.743
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.791
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         5230
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0401
_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/[\s^2^(Fo^2^)+(0.0320P)^2^+11.2650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4664
_reflns_number_total             5267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0177_suppl.cif
_cod_data_source_block           1
_cod_database_code               8106149
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.653
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(S007) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C12(H12), C1(H1), C9(H9), C7(H7), C4(H4), C16(H16), C6(H6), C10(H10),
 C15(H15), C13(H13), C2(H2), C21(H21), C18(H18), C20(H20), C19(H19)
3.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C11(H11a,H11b,H11c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.170
_oxdiff_exptl_absorpt_empirical_full_min 0.825