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_7133590
_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         'C32 H12 B F24, C24 H27 Bi Cl '
_chemical_formula_sum            'C56 H39 B Bi Cl F24'
_chemical_formula_weight         1423.11
_chemical_name_systematic
'Chloro-tris(3,5-dimethylphenyl)bismuthonium tetrakis(3,5-bis(trifluoromethyl)phenyl)borate'
_chemical_properties_physical    none
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                15634
_audit_creation_date             2024-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-17 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.109(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1228(8)
_cell_length_b                   15.8254(6)
_cell_length_c                   20.0417(9)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.34
_cell_volume                     5522.3(4)
_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      150(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            179506
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.169
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.360
_exptl_absorpt_correction_T_max  0.83841
_exptl_absorpt_correction_T_min  0.47600
_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    1.712
_exptl_crystal_description       needle
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  dichloromethane, pentane'
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.083
_refine_diff_density_max         1.721
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         16869
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+11.5886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13456
_reflns_number_total             16869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03364g2.cif
_cod_data_source_block           15634sadabs
_cod_depositor_comments
'Adding full bibliography for 7133586--7133592.cif.'
_cod_database_code               7133590
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.331
_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. Uiso/Uaniso restraints and constraints
Uanis(F20A) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F19A) \\sim Ueq,
Uanis(C55A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F23A) \\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(F24A) \\sim Ueq,
Uanis(F22A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F8A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F7A) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(F14A) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F15A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F10A) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: F1A(0.6) F2A(0.6) F3A(0.6) F4A(0.6) F5A(0.6) F6A(0.6) F7A(0.6)
 F8A(0.6) F9A(0.6) F10A(0.6) F11A(0.6) F12A(0.6) F13A(0.6) F14A(0.6) F15A(0.6)
 F16A(0.6) F17A(0.6) F18A(0.6) F19A(0.7) F20A(0.7) F21A(0.7) F22A(0.6)
 F23A(0.6) F24A(0.6) C55A(0.7) C56A(0.6) F1B(0.2) F2B(0.2) F3B(0.2) F4B(0.2)
 F5B(0.2) F6B(0.2) F7B(0.4) F8B(0.4) F9B(0.4) F10B(0.2) F11B(0.2) F12B(0.2)
 F13B(0.2) F14B(0.2) F15B(0.2) F16B(0.2) F17B(0.2) F18B(0.2) F19B(0.3)
 F20B(0.3) F21B(0.3) F22B(0.2) F23B(0.2) F24B(0.2) C55B(0.3) C56B(0.2) F1C(0.2)
 F2C(0.2) F3C(0.2) F4C(0.2) F5C(0.2) F6C(0.2) F10C(0.2) F11C(0.2) F12C(0.2)
 F13C(0.2) F14C(0.2) F15C(0.2) F16C(0.2) F17C(0.2) F18C(0.2) F22C(0.2)
 F23C(0.2) F24C(0.2) C56C(0.2)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14), C18(H18), C20(H20),
 C22(H22), C26(H26), C28(H28), C30(H30), C34(H34), C36(H36), C38(H38), C42(H42),
  C44(H44), C46(H46), C50(H50), C52(H52), C54(H54)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              64555
_shelx_hkl_checksum              54764
_olex2_submission_special_instructions 'No special instructions were received'