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_7710191
_publ_section_title
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 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 Bi P Si'
_chemical_formula_sum            'C25 H40 Bi P Si'
_chemical_formula_weight         608.61
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-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                 98.857(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1342(10)
_cell_length_b                   8.4111(10)
_cell_length_c                   31.257(3)
_cell_measurement_reflns_used    32598
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.687
_cell_measurement_theta_min      2.034
_cell_volume                     2632.6(5)
_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_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            31860
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.687
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    6.812
_exptl_absorpt_correction_T_max  0.0377
_exptl_absorpt_correction_T_min  0.0178
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   '1.83.8.0 (STOE, 2020)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_rad          0.1573
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5563
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4625
_reflns_number_total             5563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00472k2.cif
_cod_data_source_block           tdx026
_cod_database_code               7710191
_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
 Si1B-C20B \\sim Si1B-C22B \\sim Si1B-C21B
 with sigma of 0.02
 C24A-Si1B \\sim C20B-Si1B
 with sigma of 0.02
 C23A-Si1B \\sim C22B-Si1B
 with sigma of 0.02
 C25A-Si1B \\sim C21B-Si1B
 with sigma of 0.02
 C3A-C24A \\sim C3A-C20B
 with sigma of 0.02
 C3A-C23A \\sim C3A-C22B
 with sigma of 0.02
 C3A-C25A \\sim C3A-C21B
 with sigma of 0.02
 C24A-C3A \\sim C23A-C3A \\sim C25A-C3A
 with sigma of 0.02
 P1B-Si1B \\sim P1A-Si1A
 with sigma of 0.02
 Si1A-C20A \\sim Si1A-C21A \\sim Si1A-C22A
 with sigma of 0.02
 Si1A-C20A \\sim Si1A-C25B
 with sigma of 0.02
 Si1A-C22A \\sim Si1A-C23B
 with sigma of 0.02
 Si1A-C21A \\sim Si1A-C24B
 with sigma of 0.02
 C20A-C3B \\sim C25B-C3B
 with sigma of 0.02
 C22A-C3B \\sim C23B-C3B
 with sigma of 0.02
 C21A-C3B \\sim C24B-C3B
 with sigma of 0.02
 C25B-C3B \\sim C24B-C3B \\sim C23B-C3B
 with sigma of 0.02
 P1A-C3A \\sim P1B-C3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C20B)
Uanis(C24B) = Uanis(C21A)
Uanis(C25B) = Uanis(C20A)
Uanis(C22A) = Uanis(C23B)
Uanis(Si1A) = Uanis(C3B)
4. Others
 Sof(P1B)=Sof(Si1B)=Sof(C3B)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C22B)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=
 Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(Si1A)=Sof(C3A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C23A)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(P1A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C12(H12), C5(H5)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C24A(H24A,H24B,H24C), C23A(H23A,
 H23B,H23C), C20A(H20A,H20B,H20C), C25A(H25A,H25B,H25C), C19(H19A,H19B,H19C),
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C22A(H22A,H22B,
 H22C), C21A(H21A,H21B,H21C), C20B(H20D,H20E,H20F), C22B(H22D,H22E,H22F),
 C21B(H21D,H21E,H21F), C25B(H25D,H25E,H25F), C24B(H24D,H24E,H24F), C23B(H23D,
 H23E,H23F)
;
_olex2_submission_special_instructions 'No special instructions were received'