#------------------------------------------------------------------------------
#$Date: 2024-10-06 07:29:34 +0200 (Sun 06 de Oct de 2024) $
#$Revision: 295116 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/35/7133592.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133592
loop_
_publ_author_name
'Kuziola, Jennifer'
'Nöthling, Nils'
'Leutzsch, Markus'
'Cornella, Josep'
_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         'C36 H30 Bi2 Cl3, C32 H12 B F24'
_chemical_formula_sum            'C68 H42 B Bi2 Cl3 F24'
_chemical_formula_weight         1850.13
_chemical_name_systematic
'(μ-chloro)-hexakisphenyl-dichloro-di-bismuth tetrakis(3,5-bis(trifluoromethyl)phenyl)borate'
_chemical_properties_physical    none
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                14943
_audit_block_doi                 10.5517/ccdc.csd.cc2gv7sc
_audit_creation_date             2023-08-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-08-17 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                108.297(6)
_cell_angle_beta                 98.848(7)
_cell_angle_gamma                94.297(7)
_cell_formula_units_Z            2
_cell_length_a                   12.9043(18)
_cell_length_b                   14.639(2)
_cell_length_c                   20.359(3)
_cell_measurement_reflns_used    9444
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4830
_cell_measurement_theta_min      2.3887
_cell_volume                     3576.8(9)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-AXS Kappa K3-System'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  'Incoatec Montel multilayer mirrors'
_diffrn_radiation_source         '1\mS Diamond'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            453473
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.760
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.126
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.4447
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.4630.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  pentane, DCM'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.173
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         16412
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0142P)²+8.1699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15218
_reflns_number_total             16412
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03364g2.cif
_cod_data_source_block           14943sadabs
_cod_depositor_comments
'Adding full bibliography for 7133586--7133592.cif.'
_cod_original_cell_volume        3576.9(9)
_cod_database_code               7133592
_shelx_shelxl_version_number     2019/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.471
_shelx_estimated_absorpt_t_min   0.424
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F19C-C71
 1.38 with sigma of 0.001
 F20B-C71
 1.38 with sigma of 0.001
 F21C-C71
 1.38 with sigma of 0.001
 F19B-C71
 1.38 with sigma of 0.001
 F21B-C71
 1.38 with sigma of 0.001
 F20C-C71
 1.38 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4) \\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
Uanis(F19A) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F20A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F15A) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F3A) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: F1A(0.5) F1B(0.25) F1C(0.25) F2A(0.5) F2B(0.25) F2C(0.25) F3A(0.5)
 F3B(0.25) F3C(0.25) F7A(0.5) F7B(0.25) F7C(0.25) F8A(0.5) F8B(0.25) F8C(0.25)
 F9A(0.5) F9B(0.25) F9C(0.25) F10A(0.5) F10B(0.25) F10C(0.25) F11A(0.5)
 F11B(0.25) F11C(0.25) F12A(0.5) F12B(0.25) F12C(0.25) F13A(0.5) F13B(0.25)
 F13C(0.25) F14A(0.5) F14C(0.25) F15A(0.5) F15B(0.25) F15C(0.25) F16A(0.5)
 F16B(0.25) F16C(0.25) F17A(0.5) F17B(0.25) F17C(0.25) F18A(0.5) F18B(0.25)
 F18C(0.25) F19A(0.5) F19B(0.25) F19C(0.25) F20A(0.5) F20B(0.25) F20C(0.25)
 F21A(0.5) F21B(0.25) F21C(0.25) F22A(0.5) F22B(0.25) F22C(0.25) F23A(0.5)
 F23B(0.25) F23C(0.25) F24A(0.5) F24B(0.25) F24C(0.25) F40(0.25) C20A(0.7)
 H20A(0.7) C20B(0.3) H20B(0.3) C21A(0.7) H21A(0.7) C21B(0.3) H21B(0.3) H22(0.7)
 H22A(0.3) C23A(0.7) H23A(0.7) C23B(0.3) H23B(0.3) C24A(0.7) H24A(0.7)
 C24B(0.3) H24B(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20A(H20A),
 C20B(H20B), C21A(H21A), C21B(H21B), C22(H22), C22(H22A), C23A(H23A),
 C23B(H23B), C24A(H24A), C24B(H24B), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C44(H44),
  C46(H46), C50(H50), C52(H52), C54(H54), C58(H58), C60(H60), C62(H62),
 C66(H66), C68(H68), C70(H70)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
