Crystal structure of bis[triaqua-(μ2-1,2-di(4-pyridyl)ethylene-κ2N:N′)-(4-sulfonatobenzoato-κ2O,O′)zinc(II)], C13H15NO8SZn
Li, Xiao-Ling; Xin, Ling-Yun; Yu, Yue-Yi; Yang, Qing-Qing; Liu, Meng-Ke; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 169–170; doi:10.1515/ncrs-2019-0558

data_8105048
_publ_section_title
;
 Crystal structure of
 bis[triaqua-(\m2-1,2-di(4-pyridyl)ethylene-\k2N:N&#x2032;)-(4-sulfonatobenzoato-\k2O,O&#x2032;)zinc(II)],
 C13H15NO8SZn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              169
_journal_page_last               170
_journal_paper_doi               10.1515/ncrs-2019-0558
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C13 H15 N O8 S Zn'
_chemical_formula_sum            'C13 H15 N O8 S Zn'
_chemical_formula_weight         410.69
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 107.051(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3456(3)
_cell_length_b                   13.7680(4)
_cell_length_c                   19.9125(5)
_cell_measurement_reflns_used    5818
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0680
_cell_measurement_theta_min      4.2730
_cell_volume                     3235.84(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.854
_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  25.00   1.00    5.50    --  -13.80 -99.00  90.00   45
  2  \w    -30.00  54.00   1.00    5.50    --  -13.80  56.00  25.00   84
  3  \w     -2.00  82.00   1.00    5.50    --   14.82  57.00 -90.00   84
  4  \w     -4.00  84.00   1.00    5.50    --   14.82  38.00-150.00   88
  5  \w     -2.00  48.00   1.00    5.50    --   14.82  57.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0424202000
_diffrn_orient_matrix_UB_12      -0.0041151000
_diffrn_orient_matrix_UB_13      0.0173425000
_diffrn_orient_matrix_UB_21      -0.0275258000
_diffrn_orient_matrix_UB_22      0.0417172000
_diffrn_orient_matrix_UB_23      -0.0180815000
_diffrn_orient_matrix_UB_31      -0.0325157000
_diffrn_orient_matrix_UB_32      -0.0299271000
_diffrn_orient_matrix_UB_33      -0.0275823000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11762
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.399
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.686
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0385P)^2^+4.5684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3031
_reflns_number_total             3481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0558_suppl.cif
_cod_data_source_block           lxl-13
_cod_original_cell_volume        3235.85(14)
_cod_database_code               8105048
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.566
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13)
;