The crystal structure of poly[diaqua-bis(μ 3-5-bromobenzene-1,3-dicarboxylato-κ 3 O,O,O′)-(μ 2-1,3-bis-(4-pyridyl)-propane-κ 2 N,N′)-dizinc(II))] – 5-bromobenzene-1,3-dicarboxylic acid [2/1], C37H29Br3N2O14Zn2
Shi, Xiao-Ming; Fu, Yu-Jia; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 499–501; doi:10.1515/ncrs-2023-0055

data_8107478
_publ_section_title
;
 The crystal structure of poly[diaqua-bis(\m
 3-5-bromobenzene-1,3-dicarboxylato-\k 3 O,O,O&#x2032;)-(\m
 2-1,3-bis-(4-pyridyl)-propane-\k 2 N,N&#x2032;)-dizinc(II))] --
 5-bromobenzene-1,3-dicarboxylic acid [2/1], C37H29Br3N2O14Zn2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              499
_journal_page_last               501
_journal_paper_doi               10.1515/ncrs-2023-0055
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C29 H24 Br2 N2 O10 Zn2, C8 H5 Br O4'
_chemical_formula_sum            'C37 H29 Br3 N2 O14 Zn2'
_chemical_formula_weight         1096.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 112.069(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2047(6)
_cell_length_b                   28.6129(13)
_cell_length_c                   8.8721(7)
_cell_measurement_reflns_used    3301
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      73.5370
_cell_measurement_theta_min      3.0510
_cell_volume                     1930.2(3)
_computing_cell_refinement
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015) [1]'
_computing_data_collection
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015) [1]'
_computing_data_reduction
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015) [1]'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)  [3]'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015) [4]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_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    -73.00 -12.00   1.00    1.00    --  -40.73  77.00  30.00   61
  2  \w   -107.00 -60.00   1.00    1.00    --  -40.73 -38.00-180.00   47
  3  \w   -114.00 -21.00   1.00    1.00    --  -40.73 -38.00  90.00   93
  4  \w    -56.00 -21.00   1.00    1.00    --  -40.73 -38.00-180.00   35
  5  \w     43.00 139.00   1.00    1.00    --  107.58 -77.00  30.00   96
  6  \w     92.00 135.00   1.00    1.00    --  107.58 -30.00 120.00   43
  7  \w    111.00 177.00   1.00    1.00    --  107.58  45.00   0.00   66
  8  \w    125.00 168.00   1.00    1.00    --  107.58 125.00 -30.00   43
  9  \w     32.00  57.00   1.00    1.00    --  107.58 -30.00 120.00   25
 10  \w     46.00 109.00   1.00    1.00    --  107.58-125.00 -60.00   63
 11  \w     48.00 137.00   1.00    1.00    --  107.58 -61.00-120.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0757981000
_diffrn_orient_matrix_UB_12      0.0007543000
_diffrn_orient_matrix_UB_13      0.1874494000
_diffrn_orient_matrix_UB_21      0.0623852000
_diffrn_orient_matrix_UB_22      -0.0508691000
_diffrn_orient_matrix_UB_23      0.0025426000
_diffrn_orient_matrix_UB_31      0.1772079000
_diffrn_orient_matrix_UB_32      0.0176151000
_diffrn_orient_matrix_UB_33      -0.0003980000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7278
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.076
_diffrn_reflns_theta_min         3.089
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.795
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (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    1.886
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.373
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0762P)^2^+5.8138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3196
_reflns_number_total             3722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0055_suppl_001.cif
_cod_data_source_block           z05
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               8107478
_shelx_estimated_absorpt_t_max   0.595
_shelx_estimated_absorpt_t_min   0.390
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C17(H17),
 C20(H20)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              14713
_shelx_hkl_checksum              23152
_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 2.096
_oxdiff_exptl_absorpt_empirical_full_min 0.522