Crystal structure of catena-poly[tetraaqua(μ2-4-(1H-imidazol-1-yl)pyridine-κ2 N:N′))zinc(II)] thiophene-2,5-dicarboxylate, C14H17N3O8ZnS
Xue, Li-ping; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 61–63; doi:10.1515/ncrs-2018-0155

data_8105542
_publ_section_title
;
 Crystal structure of
 catena-poly[tetraaqua(\m2-4-(1H-imidazol-1-yl)pyridine-\k2
 N:N&#x2032;))zinc(II)] thiophene-2,5-dicarboxylate, C14H17N3O8ZnS
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              61
_journal_page_last               63
_journal_paper_doi               10.1515/ncrs-2018-0155
_journal_volume                  234
_journal_year                    2018
_chemical_formula_moiety         'C8 H15 N3 O4 Zn, C6 H2 O4 S'
_chemical_formula_sum            'C14 H17 N3 O8 S Zn'
_chemical_formula_weight         452.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                93.040(8)
_cell_angle_beta                 96.337(7)
_cell_angle_gamma                110.970(8)
_cell_formula_units_Z            2
_cell_length_a                   6.3962(5)
_cell_length_b                   6.9439(7)
_cell_length_c                   20.4208(19)
_cell_measurement_reflns_used    4674
_cell_measurement_temperature    288.23(10)
_cell_measurement_theta_max      27.3240
_cell_measurement_theta_min      3.9130
_cell_volume                     837.54(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_environment      air
_diffrn_ambient_temperature      288.23(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -20.00  26.00   1.00    5.00    --  -12.53 -99.00-180.00   46
  2  \w     -3.00  81.00   1.00    5.00    --   13.47  57.00  30.00   84
  3  \w    -54.00  40.00   1.00    5.00    --   13.47 -77.00 120.00   94
  4  \w     -3.00  81.00   1.00    5.00    --   13.47  57.00-120.00   84
  5  \w     -3.00  81.00   1.00    5.00    --   13.47  57.00 -60.00   84
  6  \w    -29.00  45.00   1.00    5.00    --  -12.53  57.00 -30.00   74
  7  \w    -85.00 -34.00   1.00    5.00    --  -12.53 178.00 150.00   51
;
_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      0.1145507000
_diffrn_orient_matrix_UB_12      0.0523957000
_diffrn_orient_matrix_UB_13      -0.0042215000
_diffrn_orient_matrix_UB_21      0.0354699000
_diffrn_orient_matrix_UB_22      -0.0348392000
_diffrn_orient_matrix_UB_23      0.0297328000
_diffrn_orient_matrix_UB_31      -0.0007271000
_diffrn_orient_matrix_UB_32      -0.0901551000
_diffrn_orient_matrix_UB_33      -0.0182139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8683
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0120P)^2^+1.4940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2757
_reflns_number_total             2935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0155_suppl.cif
_cod_data_source_block           x
_cod_original_cell_volume        837.54(13)
_cod_database_code               8105542
_reflns_odcompleteness_completeness 99.82
_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 O(H,H) groups
2.a Rotating group:
 O5(H1W,H2W), O6(H3W,H4W), O7(H5W,H6W), O8(H7W,H8W)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C3(H3),
 C4(H4)
;