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_7133586
_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, C84 H126 Bi2 Cl3'
_chemical_formula_sum            'C116 H138 B Bi2 Cl3 F24'
_chemical_formula_weight         2523.38
_chemical_name_systematic
'(\^I1/4-chloro)-hexakis(3,5-di-t-butylphenyl)-difluoro-di-bismuth tetrakis(3,5-bis(trifluoromethyl)phenyl)borate'
_chemical_properties_physical    none
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                14974
_audit_block_doi                 10.5517/ccdc.csd.cc2h2zwg
_audit_creation_date             2023-03-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-22 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.812(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.1234(13)
_cell_length_b                   18.2693(7)
_cell_length_c                   19.4972(8)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3492
_cell_measurement_theta_min      2.1956
_cell_volume                     11505.5(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2022)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS Kappa K3-System'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Montel multilayer mirrors'
_diffrn_radiation_source         '1\mS Diamond'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            549469
_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         2.160
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.209
_exptl_absorpt_correction_T_max  0.8626
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             5088
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  DCM, hexane'
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         17558
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+43.6497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15018
_reflns_number_total             17558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03364g2.cif
_cod_data_source_block           14974sadabs
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133586--7133592.cif.
;
_cod_database_code               7133586
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.458
_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. Restrained distances
 C57-F8B
 1.36 with sigma of 0.02
 C57-F9B
 1.27 with sigma of 0.02
 F9B-C57
 1.38 with sigma of 0.001
 F8B-C57
 1.38 with sigma of 0.001
 C57-F7B
 1.38 with sigma of 0.001
 F10C-C58
 1.38 with sigma of 0.001
 F10B-C58
 1.38 with sigma of 0.001
 F11C-C58
 1.38 with sigma of 0.001
 F11B-C58
 1.38 with sigma of 0.001
 F12C-C58
 1.38 with sigma of 0.001
 F12B-C58
 1.38 with sigma of 0.001
 C57-F7B \\sim C57-F8B \\sim C57-F9B
 with sigma of 0.02
 F7B-F8B \\sim F8B-F9B \\sim F9B-F7B
 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(F7A) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F10A) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F11A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: F1A(0.6) F2A(0.6) F3A(0.6) F4A(0.5) F5A(0.5) F6A(0.5) F7A(0.7)
 F8A(0.7) F9A(0.7) F10A(0.5) F11A(0.5) F12A(0.5) C49A(0.6) F1B(0.4) F2B(0.4)
 F3B(0.4) F4B(0.25) F5B(0.25) F6B(0.25) F7B(0.3) F8B(0.3) F9B(0.3) F10B(0.25)
 F11B(0.25) F12B(0.25) C49B(0.4) F4C(0.25) F5C(0.25) F6C(0.25) F10C(0.25)
 F11C(0.25) F12C(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C16(H16), C18(H18), C20(H20), C30(H30), C32(H32),
 C34(H34), C44(H44), C46(H46), C48(H48), C52(H52), C54(H54), C56(H56)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'