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#$Date: 2022-06-28 11:11:00 +0300 (Tue, 28 Jun 2022) $
#$Revision: 276310 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/55/8105542.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8105542
loop_
_publ_author_name
'Xue, Li-ping'
_publ_section_title
;
 Crystal structure of
 catena-poly[tetraaqua(μ2-4-(1H-imidazol-1-yl)pyridine-κ2
 N:N′))zinc(II)] thiophene-2,5-dicarboxylate, C14H17N3O8ZnS
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für 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  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -20.00  26.00   1.00    5.00    --  -12.53 -99.00-180.00   46
  2  ω     -3.00  81.00   1.00    5.00    --   13.47  57.00  30.00   84
  3  ω    -54.00  40.00   1.00    5.00    --   13.47 -77.00 120.00   94
  4  ω     -3.00  81.00   1.00    5.00    --   13.47  57.00-120.00   84
  5  ω     -3.00  81.00   1.00    5.00    --   13.47  57.00 -60.00   84
  6  ω    -29.00  45.00   1.00    5.00    --  -12.53  57.00 -30.00   74
  7  ω    -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       'ω 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/[σ²(Fo²)+(0.0120P)²+1.4940P] where P=(Fo²+2Fc²)/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 > 2σ(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
_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.
;
_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)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Zn1 Zn 0.5000 0.5000 0.5000 0.02520(15) Uani 1 2 d S T P . .
Zn2 Zn 0.5000 0.5000 1.0000 0.02506(15) Uani 1 2 d S T P . .
O5 O 0.7031(4) 0.3207(4) 0.51899(11) 0.0292(5) Uani 1 1 d . . . . .
H1W H 0.7130 0.2572 0.4834 0.044 Uiso 1 1 d GR . . . .
H2W H 0.6467 0.2309 0.5452 0.044 Uiso 1 1 d GR . . . .
O6 O 0.7742(4) 0.7902(4) 0.53645(12) 0.0351(6) Uani 1 1 d . . . . .
H3W H 0.7283 0.8633 0.5618 0.053 Uiso 1 1 d GR . . . .
H4W H 0.8829 0.7683 0.5584 0.053 Uiso 1 1 d GR . . . .
O7 O 0.6560(4) 0.2833(4) 0.97156(11) 0.0302(6) Uani 1 1 d . . . . .
H5W H 0.5557 0.1706 0.9531 0.045 Uiso 1 1 d GR . . . .
H6W H 0.7114 0.2366 1.0040 0.045 Uiso 1 1 d GR . . . .
O8 O 0.2142(4) 0.2447(4) 1.01949(12) 0.0376(6) Uani 1 1 d . . . . .
H7W H 0.2162 0.1319 1.0018 0.056 Uiso 1 1 d GR . . . .
H8W H 0.2155 0.2370 1.0609 0.056 Uiso 1 1 d GR . . . .
N1 N 0.4211(5) 0.4627(4) 0.59765(13) 0.0261(6) Uani 1 1 d . . . . .
N2 N 0.2824(5) 0.4355(4) 0.79368(13) 0.0250(6) Uani 1 1 d . . . . .
N3 N 0.3416(5) 0.4556(4) 0.90277(12) 0.0271(6) Uani 1 1 d . . . . .
C7 C 0.2108(6) 0.3878(6) 0.61115(17) 0.0347(9) Uani 1 1 d . . . . .
H7 H 0.0936 0.3431 0.5760 0.042 Uiso 1 1 calc R . . . .
C8 C 0.1563(6) 0.3724(6) 0.67465(16) 0.0314(8) Uani 1 1 d . . . . .
H8 H 0.0061 0.3166 0.6818 0.038 Uiso 1 1 calc R . . . .
C9 C 0.3295(6) 0.4418(5) 0.72784(16) 0.0246(7) Uani 1 1 d . . . . .
C10 C 0.5500(6) 0.5177(5) 0.71469(16) 0.0283(8) Uani 1 1 d . . . . .
H10 H 0.6703 0.5630 0.7490 0.034 Uiso 1 1 calc R . . . .
C11 C 0.5877(6) 0.5247(6) 0.64961(16) 0.0308(8) Uani 1 1 d . . . . .
H11 H 0.7365 0.5751 0.6410 0.037 Uiso 1 1 calc R . . . .
C12 C 0.0748(6) 0.3913(6) 0.81494(17) 0.0332(8) Uani 1 1 d . . . . .
H12 H -0.0637 0.3595 0.7886 0.040 Uiso 1 1 calc R . . . .
C13 C 0.1124(6) 0.4034(6) 0.88154(17) 0.0333(8) Uani 1 1 d . . . . .
H13 H 0.0014 0.3803 0.9092 0.040 Uiso 1 1 calc R . . . .
C14 C 0.4376(6) 0.4733(6) 0.84949(16) 0.0315(8) Uani 1 1 d . . . . .
H14 H 0.5919 0.5072 0.8491 0.038 Uiso 1 1 calc R . . . .
S1 S 0.86112(14) 0.10859(13) 0.26641(4) 0.0243(2) Uani 1 1 d . . . . .
O1 O 0.7375(4) 0.0484(4) 0.07198(11) 0.0313(6) Uani 1 1 d . . . . .
O2 O 1.0640(4) 0.1782(4) 0.13995(11) 0.0357(6) Uani 1 1 d . . . . .
O3 O 0.4102(4) -0.0276(4) 0.38905(11) 0.0349(6) Uani 1 1 d . . . . .
O4 O 0.7843(4) 0.1399(4) 0.40980(11) 0.0391(6) Uani 1 1 d . . . . .
C1 C 0.8540(6) 0.1023(5) 0.12876(16) 0.0242(7) Uani 1 1 d . . . . .
C2 C 0.7241(5) 0.0717(5) 0.18644(15) 0.0208(7) Uani 1 1 d . . . . .
C3 C 0.4961(6) 0.0197(5) 0.18553(16) 0.0285(8) Uani 1 1 d . . . . .
H3 H 0.3940 -0.0042 0.1471 0.034 Uiso 1 1 calc R . . . .
C4 C 0.4349(6) 0.0066(5) 0.24949(16) 0.0258(7) Uani 1 1 d . . . . .
H4 H 0.2863 -0.0271 0.2576 0.031 Uiso 1 1 calc R . . . .
C5 C 0.6097(5) 0.0468(5) 0.29834(15) 0.0230(7) Uani 1 1 d . . . . .
C6 C 0.6025(6) 0.0521(5) 0.37171(16) 0.0277(8) Uani 1 1 d . . . . .
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'
S S 0.1246 0.1234 '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'
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
O5 Zn1 O5 180.0 . 2_666
O5 Zn1 O6 93.39(9) 2_666 2_666
O5 Zn1 O6 93.39(9) . .
O5 Zn1 O6 86.61(9) 2_666 .
O5 Zn1 O6 86.61(9) . 2_666
O6 Zn1 O6 180.0 2_666 .
N1 Zn1 O5 92.66(9) 2_666 .
N1 Zn1 O5 92.66(9) . 2_666
N1 Zn1 O5 87.34(9) . .
N1 Zn1 O5 87.34(9) 2_666 2_666
N1 Zn1 O6 89.30(10) 2_666 2_666
N1 Zn1 O6 90.70(10) 2_666 .
N1 Zn1 O6 90.70(10) . 2_666
N1 Zn1 O6 89.30(10) . .
N1 Zn1 N1 180.0 2_666 .
O7 Zn2 O7 180.0 . 2_667
O8 Zn2 O7 89.05(9) 2_667 2_667
O8 Zn2 O7 89.05(9) . .
O8 Zn2 O7 90.95(9) . 2_667
O8 Zn2 O7 90.95(9) 2_667 .
O8 Zn2 O8 180.0 . 2_667
N3 Zn2 O7 88.02(10) 2_667 2_667
N3 Zn2 O7 91.98(10) . 2_667
N3 Zn2 O7 91.98(10) 2_667 .
N3 Zn2 O7 88.02(10) . .
N3 Zn2 O8 92.93(10) . 2_667
N3 Zn2 O8 87.07(11) . .
N3 Zn2 O8 87.07(11) 2_667 2_667
N3 Zn2 O8 92.93(10) 2_667 .
N3 Zn2 N3 180.0 2_667 .
Zn1 O5 H1W 111.0 . .
Zn1 O5 H2W 110.6 . .
H1W O5 H2W 108.0 . .
Zn1 O6 H3W 110.1 . .
Zn1 O6 H4W 110.8 . .
H3W O6 H4W 108.2 . .
Zn2 O7 H5W 110.2 . .
Zn2 O7 H6W 114.2 . .
H5W O7 H6W 99.2 . .
Zn2 O8 H7W 110.2 . .
Zn2 O8 H8W 110.6 . .
H7W O8 H8W 108.3 . .
C7 N1 Zn1 122.7(2) . .
C7 N1 C11 117.0(3) . .
C11 N1 Zn1 120.2(2) . .
C12 N2 C9 127.3(3) . .
C14 N2 C9 126.1(3) . .
C14 N2 C12 106.5(3) . .
C13 N3 Zn2 127.2(2) . .
C14 N3 Zn2 126.9(2) . .
C14 N3 C13 105.9(3) . .
N1 C7 H7 118.3 . .
N1 C7 C8 123.4(3) . .
C8 C7 H7 118.3 . .
C7 C8 H8 120.5 . .
C7 C8 C9 119.0(3) . .
C9 C8 H8 120.5 . .
C8 C9 N2 121.2(3) . .
C10 C9 N2 120.4(3) . .
C10 C9 C8 118.4(3) . .
C9 C10 H10 120.8 . .
C11 C10 C9 118.4(3) . .
C11 C10 H10 120.8 . .
N1 C11 C10 123.8(3) . .
N1 C11 H11 118.1 . .
C10 C11 H11 118.1 . .
N2 C12 H12 126.9 . .
C13 C12 N2 106.3(3) . .
C13 C12 H12 126.9 . .
N3 C13 H13 125.0 . .
C12 C13 N3 109.9(3) . .
C12 C13 H13 125.0 . .
N2 C14 H14 124.3 . .
N3 C14 N2 111.4(3) . .
N3 C14 H14 124.3 . .
C5 S1 C2 91.58(15) . .
O1 C1 C2 116.1(3) . .
O2 C1 O1 125.5(3) . .
O2 C1 C2 118.4(3) . .
C1 C2 S1 120.8(2) . .
C3 C2 S1 111.3(2) . .
C3 C2 C1 127.9(3) . .
C2 C3 H3 124.0 . .
C2 C3 C4 111.9(3) . .
C4 C3 H3 124.0 . .
C3 C4 H4 122.8 . .
C5 C4 C3 114.4(3) . .
C5 C4 H4 122.8 . .
C4 C5 S1 110.8(2) . .
C4 C5 C6 127.6(3) . .
C6 C5 S1 121.5(3) . .
O3 C6 C5 115.8(3) . .
O4 C6 O3 125.9(3) . .
O4 C6 C5 118.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O5 2.118(2) .
Zn1 O5 2.118(2) 2_666
Zn1 O6 2.171(2) 2_666
Zn1 O6 2.171(2) .
Zn1 N1 2.117(3) 2_666
Zn1 N1 2.117(3) .
Zn2 O7 2.169(2) 2_667
Zn2 O7 2.169(2) .
Zn2 O8 2.135(2) .
Zn2 O8 2.135(2) 2_667
Zn2 N3 2.081(3) 2_667
Zn2 N3 2.081(3) .
O5 H1W 0.8499 .
O5 H2W 0.8500 .
O6 H3W 0.8502 .
O6 H4W 0.8499 .
O7 H5W 0.8499 .
O7 H6W 0.8501 .
O8 H7W 0.8500 .
O8 H8W 0.8499 .
N1 C7 1.324(4) .
N1 C11 1.349(4) .
N2 C9 1.409(4) .
N2 C12 1.377(4) .
N2 C14 1.373(4) .
N3 C13 1.390(4) .
N3 C14 1.297(4) .
C7 H7 0.9300 .
C7 C8 1.379(5) .
C8 H8 0.9300 .
C8 C9 1.391(5) .
C9 C10 1.381(5) .
C10 H10 0.9300 .
C10 C11 1.377(5) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C12 C13 1.348(5) .
C13 H13 0.9300 .
C14 H14 0.9300 .
S1 C2 1.726(3) .
S1 C5 1.721(3) .
O1 C1 1.266(4) .
O2 C1 1.244(4) .
O3 C6 1.255(4) .
O4 C6 1.253(4) .
C1 C2 1.497(4) .
C2 C3 1.369(4) .
C3 H3 0.9300 .
C3 C4 1.403(4) .
C4 H4 0.9300 .
C4 C5 1.351(5) .
C5 C6 1.503(4) .
