Synthesis and characterization of chlorotriarylbismuthonium salts.
Kuziola, Jennifer; Nöthling, Nils; Leutzsch, Markus; Cornella, Josep; Chemical communications (Cambridge, England) 60 (2024) 10532–10535; doi:10.1039/d4cc03364g

data_7133587
_publ_section_title
;
 Synthesis and characterization of chlorotriarylbismuthonium salts.
;
_journal_issue                   76
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10532
_journal_page_last               10535
_journal_paper_doi               10.1039/d4cc03364g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C24 H27 Bi Cl2'
_chemical_formula_sum            'C24 H27 Bi Cl2'
_chemical_formula_weight         595.33
_chemical_name_systematic
;
tris(3,5-diemthylphenyl)bimuth dichloride
;
_chemical_properties_physical    none
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
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_audit_update_record
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2024-05-17 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9412(6)
_cell_length_b                   10.4632(4)
_cell_length_c                   13.6006(5)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.59
_cell_measurement_theta_min      2.33
_cell_volume                     2268.53(15)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX3 (Bruker AXS, 2005-2017)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2014)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         1\mS
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            85206
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.958
_diffrn_reflns_theta_min         2.328
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
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_exptl_absorpt_coefficient_mu    8.014
_exptl_absorpt_correction_T_max  0.83538
_exptl_absorpt_correction_T_min  0.52512
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  dichloromethane, pentane'
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0163
_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^)+(0.0095P)^2^+2.0990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0291
_refine_ls_wR_factor_ref         0.0330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3558
_reflns_number_total             4976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03364g2.cif
_cod_data_source_block           15527sadabs
_cod_depositor_comments
'Adding full bibliography for 7133586--7133592.cif.'
_cod_database_code               7133587
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.724
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_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:
 C2(H2), C4(H4), C6(H6), C10(H10), C13(H13)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              2381
_shelx_hkl_checksum              21071
_olex2_submission_special_instructions 'No special instructions were received'