Isolable monoatomic monovalent bismuth complexes with a redox non-innocent bis-silylenyl carborane ligand
Xu, Jian; Yao, Shenglai; Postils, Verònica; Matito, Eduard; Lorent, Christian; Driess, Matthias; Chemical Science 16 (2025) 10826–10832; doi:10.1039/D5SC02644J

data_1574671
_publ_section_title
;
 Isolable monoatomic monovalent bismuth complexes with a redox
 non-innocent bis-silylenyl carborane ligand
;
_journal_issue                   24
_journal_name_full               'Chemical Science'
_journal_page_first              10826
_journal_page_last               10832
_journal_paper_doi               10.1039/D5SC02644J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C32 H56 B10 Bi N4 Si2, C F3 O3 S'
_chemical_formula_sum            'C33 H56 B10 Bi F3 N4 O3 S Si2'
_chemical_formula_weight         1019.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-01 deposited with the CCDC.	2025-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.66060(10)
_cell_length_b                   10.19510(10)
_cell_length_c                   27.7238(2)
_cell_measurement_reflns_used    23392
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      72.5890
_cell_measurement_theta_min      3.1140
_cell_volume                     4417.21(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.15
_diffrn_detector_area_resol_mean 10.5435
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -29.00  65.00   1.00   10.00    --   41.50 -57.00 120.00   94
  2  \w     71.00  96.00   1.00   10.00    --   41.50-125.00 -90.00   25
  3  \w    -33.00  66.00   1.00   10.00    --   41.50 -38.00 -30.00   99
  4  \w     18.00 110.00   1.00   10.00    --   41.50  57.00 -90.00   92
  5  \w     35.00  76.00   1.00   10.00    --   41.50 -99.00  30.00   41
  6  \w     44.00 136.00   1.00   12.50    --  103.94 -77.00  30.00   92
  7  \w     67.00 107.00   1.00   12.50    --  103.94-111.00-180.00   40
  8  \w     22.00  80.00   1.00   12.50    --  103.94 -94.00-150.00   58
  9  \w     30.00  81.00   1.00   12.50    --  103.94-111.00  30.00   51
 10  \w     79.00 134.00   1.00   12.50    --  103.94  61.00 -30.00   55
 11  \w     78.00 135.00   1.00   12.50    --  103.94  45.00 -90.00   57
 12  \w     85.00 151.00   1.00   12.50    --  103.94 111.00   0.00   66
 13  \w     85.00 150.00   1.00   12.50    --  103.94  77.00  90.00   65
 14  \w     85.00 158.00   1.00   12.50    --  103.94  45.00-180.00   73
 15  \w     60.00 108.00   1.00   12.50    --  103.94-111.00 -90.00   48
 16  \w     29.00 107.00   1.00   12.50    --  103.94 -94.00 -60.00   78
 17  \w     30.00  56.00   1.00   12.50    --  103.94-111.00  60.00   26
 18  \w     79.00 108.00   1.00   12.50    --  103.94-111.00  60.00   29
 19  \w     87.00 121.00   1.00   12.50    --  103.94  77.00 120.00   34
 20  \w     90.00 152.00   1.00   12.50    --  103.94 111.00-150.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31319
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.661
_diffrn_reflns_theta_min         3.157
_exptl_absorpt_coefficient_mu    9.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       needle
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         8661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+1.8558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8289
_reflns_number_total             8661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02644j2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 1574669--1574673.cif.'
_cod_database_code               1574671
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.608
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C28(H28), C24(H24), C25(H25), C10(H10), C27(H27), C26(H26), C13(H13),
 C11(H11), C12(H12)
1.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C15(H15A,H15B,
 H15C), C32(H32A,H32B,H32C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C20(H20A,
 H20B,H20C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C6(H6A,H6B,H6C), C31(H31A,
 H31B,H31C)
1.c Boron cage BH refined with riding coordinates:
 B8(H8), B2(H2), B9(H9A), B3(H3), B5(H5), B7(H7), B10(H10A), B1(H1), B4(H4),
 B6(H6)
;
_shelx_res_checksum              10601
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;