Synthesis of bismuthanyl-substituted monomeric triel hydrides.
Szlosek, Robert; Marquardt, Christian; Hegen, Oliver; Balázs, Gábor; Riesinger, Christoph; Timoshkin, Alexey Y.; Scheer, Manfred; Chemical science 15 (2024) 14837–14843; doi:10.1039/d4sc03926b

data_1572322
_publ_section_title
;
 Synthesis of bismuthanyl-substituted monomeric triel hydrides.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              14837
_journal_page_last               14843
_journal_paper_doi               10.1039/d4sc03926b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C13 H32 B Bi N2 Si2'
_chemical_formula_sum            'C13 H32 B Bi N2 Si2'
_chemical_formula_weight         492.37
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5219)
;
_audit_update_record
;
2024-03-16 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                97.044(4)
_cell_angle_beta                 108.604(4)
_cell_angle_gamma                101.577(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5403(4)
_cell_length_b                   9.8557(6)
_cell_length_c                   12.1971(4)
_cell_measurement_reflns_used    3828
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.6730
_cell_measurement_theta_min      4.6570
_cell_volume                     1043.07(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
  1 omega  -69.00   17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.9004   57.0000   30.0000 86

  2 omega  -69.00   24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.9004   57.0000 -120.0000 93

  3 omega -114.00  -22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.9004  -57.0000   90.0000 92

  4 omega   89.00  126.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -120.0000 37

  5 omega   98.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -180.0000 75

  6 omega   47.00  135.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000    0.0000 88

  7 omega   47.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  150.0000 77

  8 omega   38.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000    0.0000 83

  9 omega   41.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -120.0000 27

 10 omega   26.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000 -180.0000 83

 11 omega   28.00  141.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -15.0000    0.0000 113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  GV50
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0675277000
_diffrn_orient_matrix_UB_12      0.0789797000
_diffrn_orient_matrix_UB_13      0.1298065000
_diffrn_orient_matrix_UB_21      -0.0351167000
_diffrn_orient_matrix_UB_22      0.1359587000
_diffrn_orient_matrix_UB_23      -0.0393431000
_diffrn_orient_matrix_UB_31      -0.1589176000
_diffrn_orient_matrix_UB_32      -0.0425279000
_diffrn_orient_matrix_UB_33      0.0105381000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6314
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.073
_diffrn_reflns_theta_min         3.904
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.605
_exptl_absorpt_correction_T_max  0.341
_exptl_absorpt_correction_T_min  0.163
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.1943
_exptl_crystal_size_mid          0.1258
_exptl_crystal_size_min          0.1168
_refine_diff_density_max         1.572
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0512P)^2^+0.5687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3703
_reflns_number_total             3974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03926b3.cif
_cod_data_source_block           p-12
_cod_depositor_comments
'Adding full bibliography for 1572322--1572325.cif.'
_cod_database_code               1572322
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C13 N2 Si2 B Bi H32'
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C2(H2A,H2B,H2C),
 C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C),
 C11(H11A,H11B,H11C), C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'