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_1572324
_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 B Bi N2 Si2'
_chemical_formula_sum            'C33 H56 B Bi N2 Si2'
_chemical_formula_weight         756.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-06-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.900(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0837(3)
_cell_length_b                   10.2928(2)
_cell_length_c                   40.2707(12)
_cell_measurement_reflns_used    44696
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      35.7140
_cell_measurement_theta_min      2.2300
_cell_volume                     7491.5(3)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     -1.00  28.26   0.38    3.04    --    0.15  19.00-150.00   77
  2  \w    -13.00  40.20   0.38    3.04    --    0.15  19.00-120.00  140
  3  \w    -46.00  27.72   0.38    3.04    --    0.15 -19.00 -60.00  194
  4  \w    -48.00  -8.86   0.38    3.04    --    0.15 -19.00-120.00  103
  5  \w     -6.00  19.08   0.38    3.04    --    0.15 -19.00-120.00   66
  6  \w    -48.00  23.06   0.38    3.04    --    0.15 -19.00-180.00  187
  7  \w    -48.00  25.72   0.38    3.04    --    0.15 -19.00   0.00  194
  8  \w     -3.00  30.06   0.38    3.04    --    0.15 -19.00  30.00   87
  9  \w    -43.00 -11.84   0.38    3.04    --    0.15 -19.00  30.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            92561
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         2.222
_exptl_absorpt_coefficient_mu    4.793
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.453
_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 light yellow'
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       plate
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.778
_refine_diff_density_min         -1.762
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         13330
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+23.4480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11815
_reflns_number_total             13330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03926b3.cif
_cod_data_source_block           rs922_moa_abs
_cod_depositor_comments
'Adding full bibliography for 1572322--1572325.cif.'
_cod_database_code               1572324
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.318
_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
 B19-H19A = B19-H19B
 1.1 with sigma of 0.02
 B2-H2B = B2-H2A
 1.1 with sigma of 0.02
 B1-H1A = B1-H1B
 1.1 with sigma of 0.02
 H2B-H2A
 1.9 with sigma of 0.04
 H2B-C40
 2.2 with sigma of 0.04
 H2A-C40
 2.2 with sigma of 0.04
 H19B-H19A
 1.9 with sigma of 0.04
 H19B-C40
 2.2 with sigma of 0.04
 H19A-C40
 2.2 with sigma of 0.04
 H1B-H1A
 1.9 with sigma of 0.04
 H1A-C18
 2.2 with sigma of 0.04
 H1B-C18
 2.2 with sigma of 0.04
 H19A-Bi3
 2.9 with sigma of 0.04
 H19B-Bi3
 2.9 with sigma of 0.04
 Bi2-B2 \\sim Bi3-B19
 with sigma of 0.02
 C40-B19 \\sim C40-B2
 with sigma of 0.02
 Bi2-Si3 \\sim Bi2-Si3A
 with sigma of 0.02
 Si3-C54 \\sim Si3A-C54A
 with sigma of 0.02
 Si3-C33 \\sim Si3A-C33A
 with sigma of 0.02
 Si3-C57 \\sim Si3A-C57A
 with sigma of 0.02
 Si3-Bi3 \\sim Si3A-Bi3
 with sigma of 0.02
 Bi2-C54 \\sim Bi2-C54A
 with sigma of 0.04
 Bi2-C33 \\sim Bi2-C33A
 with sigma of 0.04
 Bi2-C57 \\sim Bi2-C57A
 with sigma of 0.04
 C54-C33 \\sim C54A-C33A
 with sigma of 0.04
 C54-C57 \\sim C54A-C57A
 with sigma of 0.04
 C54-Bi3 \\sim C54A-Bi3
 with sigma of 0.04
 C33-C57 \\sim C33A-C57A
 with sigma of 0.04
 C33-Bi3 \\sim C33A-Bi3
 with sigma of 0.04
 C57-Bi3 \\sim C57A-Bi3
 with sigma of 0.04
 Bi2-Si2 \\sim Bi2-Si2A
 with sigma of 0.02
 Si2-C7 \\sim Si2A-C7A
 with sigma of 0.02
 Si2-C61 \\sim Si2A-C61A
 with sigma of 0.02
 Si2-C65 \\sim Si2A-C65A
 with sigma of 0.02
 Bi2-C7 \\sim Bi2-C7A
 with sigma of 0.04
 Bi2-C61 \\sim Bi2-C61A
 with sigma of 0.04
 Bi2-C65 \\sim Bi2-C65A
 with sigma of 0.04
 Si2-Bi3 \\sim Si2A-Bi3
 with sigma of 0.04
 C7-C61 \\sim C7A-C61A
 with sigma of 0.04
 C7-C65 \\sim C7A-C65A
 with sigma of 0.04
 C7-Bi3 \\sim C7A-Bi3
 with sigma of 0.04
 C61-C65 \\sim C61A-C65A
 with sigma of 0.04
 C61-Bi3 \\sim C61A-Bi3
 with sigma of 0.04
 C65-Bi3 \\sim C65A-Bi3
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Si2 \\sim C7 \\sim C61 \\sim C65 \\sim Si2A \\sim C61A \\sim C65A \\sim C7A
\\sim Si3 \\sim C54 \\sim C33 \\sim C57 \\sim Si3A \\sim C57A \\sim C54A \\sim
C33A: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2.5A
B2 \\sim B19: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(B19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(Bi3)=Sof(B19)=Sof(Si3A)=Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C54A)=
 Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 Sof(Si2A)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C65A)=Sof(H65D)=
 Sof(H65E)=Sof(H65F)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(H19A)=Sof(H19B)=
 1-FVAR(1)
 Sof(Bi2)=Sof(Si2)=Sof(Si3)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(B2)=
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(H2A)=Sof(H2B)=FVAR(1)
 Sof(Bi4)=1-FVAR(2)
 Sof(Bi1)=FVAR(2)
 Fixed Uiso: H19A(0.04) H19B(0.04) H1A(0.04) H2A(0.04) H1B(0.04) H2B(0.04)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C30(H30), C32(H32), C38(H38), C46(H46), C48(H48), C66(H66), C51(H51)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C28(H28), C34(H34), C42(H42), C44(H44), C56(H56), C58(H58), C62(H62),
 C17(H17), C35(H35), C19(H19), C39(H39), C5(H5), C21(H21), C43(H43), C11(H11)
5.c Idealised Me refined with riding coordinates:
 C65A(H65D,H65E,H65F)
5.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C60(H60A,H60B,
 H60C), C33(H33A,H33B,H33C), C9(H9A,H9B,H9C), C37(H37A,H37B,H37C), C41(H41A,
 H41B,H41C), C45(H45A,H45B,H45C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C),
 C3(H3A,H3B,H3C), C49(H49A,H49B,H49C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C),
  C53(H53A,H53B,H53C), C27(H27A,H27B,H27C), C55(H55A,H55B,H55C), C7(H7A,H7B,
 H7C), C57(H57A,H57B,H57C), C29(H29A,H29B,H29C), C59(H59A,H59B,H59C), C15(H15A,
 H15B,H15C), C61(H61A,H61B,H61C), C31(H31A,H31B,H31C), C63(H63A,H63B,H63C),
 C2(H2C,H2D,H2E), C65(H65A,H65B,H65C), C57A(H57D,H57E,H57F), C54A(H54D,H54E,
 H54F), C33A(H33D,H33E,H33F), C61A(H61D,H61E,H61F), C7A(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              89409
_shelx_hkl_checksum              63296
_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
;