The crystal structure of 2-bromo-1,3-phenylene bis(4-methylbenzenesulfonate), C20H17BrO6S2
Chen, Jue-Yuan; Zou, Long-Sheng; Lai, Ni; Yin, Zi-Yi; Yuan, Lin; Li, Zhong-Yan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 503–505; doi:10.1515/ncrs-2023-0056

data_8107479
_publ_section_title
;
 The crystal structure of 2-bromo-1,3-phenylene
 bis(4-methylbenzenesulfonate), C20H17BrO6S2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              503
_journal_page_last               505
_journal_paper_doi               10.1515/ncrs-2023-0056
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C20 H17 Br O6 S2'
_chemical_formula_sum            'C20 H17 Br O6 S2'
_chemical_formula_weight         497.36
_chemical_name_systematic
;
2-bromo-1,3-phenylene bis(4-methylbenzenesulfonate)
;
_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   geom
_cell_angle_alpha                89.947(3)
_cell_angle_beta                 83.105(3)
_cell_angle_gamma                72.077(3)
_cell_formula_units_Z            2
_cell_length_a                   8.173(2)
_cell_length_b                   8.256(2)
_cell_length_c                   16.514(5)
_cell_measurement_reflns_used    5485
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.49
_cell_volume                     1051.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10043
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.243
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1304 before and 0.0445 after correction.
The Ratio of minimum to maximum transmission is 0.5660.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.066(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0365P)^2^+0.6166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3105
_reflns_number_total             3690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0056_suppl_001.cif
_cod_data_source_block           123
_cod_database_code               8107479
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C12(H12), C11(H11), C16(H16), C15(H15), C4(H4), C5(H5),
 C6(H6), C8(H8), C9(H9)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              53414
_shelx_hkl_checksum              99663
_olex2_submission_special_instructions 'No special instructions were received'