Binary interpnictogen compounds bearing diaryl bismuth fragments bound to all lighter pnictogens
Dunaj, Tobias; Dollberg, Kevin; von Hänisch, Carsten; Dalton Transactions  (2022) –; doi:10.1039/D2DT00472K

data_7710192
_publ_section_title
;
 Binary interpnictogen compounds bearing diaryl bismuth fragments bound to
 all lighter pnictogens
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00472K
_journal_year                    2022
_chemical_formula_moiety         'C25 H40 As Bi Si'
_chemical_formula_sum            'C25 H40 As Bi Si'
_chemical_formula_weight         652.56
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Light-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.745(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1538(3)
_cell_length_b                   8.4878(2)
_cell_length_c                   31.1727(10)
_cell_measurement_reflns_used    39217
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.03
_cell_volume                     2655.34(13)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'STOE IPDS 2T'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            15324
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.976
_diffrn_reflns_theta_min         2.029
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.930
_exptl_absorpt_correction_T_max  0.0148
_exptl_absorpt_correction_T_min  0.0081
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'LANA 1.83.8.0 (STOE, 2020)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_rad          0.1739
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6248
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+3.7667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5369
_reflns_number_total             6248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00472k2.cif
_cod_data_source_block           pcrx99
_cod_database_code               7710192
_shelx_shelxl_version_number     2018/3
_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
 Si1A-C21A \\sim Si1A-C22A \\sim Si1A-C20A
 with sigma of 0.02
 C23A-C3A \\sim C25A-C3A \\sim C3A-C24A
 with sigma of 0.02
 Si1B-C23B \\sim Si1B-C25B \\sim Si1B-C24B
 with sigma of 0.02
 C3B-C21B \\sim C3B-C22B \\sim C3B-C20B
 with sigma of 0.02
 As1B-C3B \\sim As1A-C3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3B) \\sim Ueq, Uanis(C3A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
Uanis(C21A) = Uanis(C22A) = Uanis(C20A)
Uanis(C23A) = Uanis(C25A) = Uanis(C24A)
Uanis(C23B) = Uanis(C25B) = Uanis(C24B)
Uanis(C21B) = Uanis(C22B) = Uanis(C20B)
4. Others
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C20B)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C25B)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C21B)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C3B)=Sof(Si1B)=Sof(As1B)=1-FVAR(1)
 Sof(Si1A)=Sof(C3A)=Sof(As1A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C25A)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=FVAR(1)
5.a Me refined with riding coordinates:
 C21B(H21A,H21B,H21C)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C10(H10), C12(H12)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C24A(H24A,H24B,
 H24C), C20B(H20A,H20B,H20C), C14(H14A,H14B,H14C), C23B(H23A,H23B,H23C),
 C25B(H25A,H25B,H25C), C22B(H22A,H22B,H22C), C18(H18A,H18B,H18C), C15(H15A,H15B,
 H15C), C21A(H21D,H21E,H21F), C20A(H20D,H20E,H20F), C22A(H22D,H22E,H22F),
 C23A(H23D,H23E,H23F), C25A(H25D,H25E,H25F), C24B(H24D,H24E,H24F)
;
_olex2_submission_special_instructions 'No special instructions were received'