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_1572323
_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         'C33 H56 Bi Ga N2 Si2'
_chemical_formula_sum            'C33 H56 Bi Ga N2 Si2'
_chemical_formula_weight         815.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-16 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3792(3)
_cell_length_b                   19.2881(2)
_cell_length_c                   20.2475(2)
_cell_measurement_reflns_used    19768
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      73.3790
_cell_measurement_theta_min      3.1320
_cell_volume                     7568.27(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.953
_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     11.00  40.00   0.50    0.05    --   60.21 -30.00  60.00   58
  2  \w     11.00  40.00   0.50    0.05    --   60.21 -30.00  90.00   58
  3  \w     35.00 104.00   0.50    0.05    --   78.50-125.00  60.00  138
  4  \w     48.00  96.00   0.50    0.05    --   78.50-112.00 -73.00   96
  5  \w     39.00  80.00   0.50    0.05    --   78.50 -95.00-120.00   82
  6  \w     11.00  39.00   0.50    0.05    --   60.21 -30.00-150.00   56
  7  \w     46.00  95.00   0.50    0.05    --   78.50  18.00 -87.00   98
  8  \w     78.00 118.00   0.50    0.05    --   73.83  30.00  30.00   80
  9  \w     90.00 128.00   0.50    0.05    --   78.50  30.00-180.00   76
 10  \w   -104.00 -30.00   0.50    0.05    --  -61.12 160.00-100.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0346462000
_diffrn_orient_matrix_UB_12      -0.0695471000
_diffrn_orient_matrix_UB_13      0.0174562000
_diffrn_orient_matrix_UB_21      0.0706540000
_diffrn_orient_matrix_UB_22      0.0362170000
_diffrn_orient_matrix_UB_23      0.0028714000
_diffrn_orient_matrix_UB_31      -0.0108370000
_diffrn_orient_matrix_UB_32      0.0150288000
_diffrn_orient_matrix_UB_33      0.0740937000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26333
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.674
_diffrn_reflns_theta_min         3.902
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.653
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
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 colourless'
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       plate
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.000018(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         7278
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+2.5797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6764
_reflns_number_total             7278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03926b3.cif
_cod_data_source_block           rs802_cua_abs
_cod_depositor_comments
'Adding full bibliography for 1572322--1572325.cif.'
_cod_database_code               1572323
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C33 H56 N2 Ga Bi Si2'
_shelx_estimated_absorpt_t_max   0.317
_shelx_estimated_absorpt_t_min   0.076
_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
 Ga1-H \\sim Ga1-HA
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C31(H31), C19(H19), C16(H16), C28(H28)
3.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C3(H3), C25(H25), C2(H2), C14(H14), C26(H26), C13(H13), C12(H12)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C33(H33A,H33B,H33C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C18(H18A,H18B,H18C),
 C5(H5A,H5B,H5C), C32(H32A,H32B,H32C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C),
 C20(H20A,H20B,H20C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              48222
_shelx_hkl_checksum              67457
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.455
_oxdiff_exptl_absorpt_empirical_full_min 0.622