The crystal structure of poly[(m4-4-bromoisophthalato-κ4O: O′:O′′:O′′′)zinc(II)], C8H3BrO4Zn
Chang, Xin-Hong; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 3–4; doi:10.1515/ncrs-2019-0397

data_8104996
_publ_section_title
;
 The crystal structure of poly[(m4-4-bromoisophthalato-\k4O:
 O&#x2032;:O&#x2032;&#x2032;:O&#x2032;&#x2032;&#x2032;)zinc(II)],
 C8H3BrO4Zn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              3
_journal_page_last               4
_journal_paper_doi               10.1515/ncrs-2019-0397
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C8 H3 Br O4 Zn'
_chemical_formula_sum            'C8 H3 Br O4 Zn'
_chemical_formula_weight         308.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 98.942(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.7134(4)
_cell_length_b                   15.4354(13)
_cell_length_c                   12.0064(9)
_cell_measurement_reflns_used    1718
_cell_measurement_temperature    292.67(10)
_cell_measurement_theta_max      27.4140
_cell_measurement_theta_min      4.3110
_cell_volume                     862.89(12)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.67(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9983
_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    -74.00  45.00   1.00    4.58    --  -16.00   0.00-150.00  119
  2  \w    -88.00 -63.00   1.00    4.58    --  -16.00-178.00  30.00   25
  3  \w     -1.00  56.00   1.00    4.58    --   16.93 -99.00-150.00   57
;
_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      0.0475689000
_diffrn_orient_matrix_UB_12      -0.0429211000
_diffrn_orient_matrix_UB_13      -0.0076039000
_diffrn_orient_matrix_UB_21      0.1374984000
_diffrn_orient_matrix_UB_22      0.0107607000
_diffrn_orient_matrix_UB_23      0.0296976000
_diffrn_orient_matrix_UB_31      -0.0448786000
_diffrn_orient_matrix_UB_32      -0.0125370000
_diffrn_orient_matrix_UB_33      0.0513312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3504
_diffrn_reflns_theta_full        26.3639
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41277
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.3738
_exptl_crystal_description       plate
_exptl_crystal_F_000             592.5123
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.9929
_refine_diff_density_min         -1.3800
_refine_diff_density_rms         0.1945
_refine_ls_d_res_high            0.8002
_refine_ls_d_res_low             5.9302
_refine_ls_goodness_of_fit_ref   1.0371
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0371
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+1.5821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1491
_reflns_number_total             1754
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2019-0397_suppl.cif
_cod_data_source_block           1
_cod_database_code               8104996
_chemical_oxdiff_formula         C1H1N1O1Zn1
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C2(H2)
;