Methylbismuth: an Organometallic Bismuthinidene Biradical
Mukhopadhyay, Deb Pratim; Schleier, Domenik; Wirsing, Sara; Ramler, Jacqueline; Kaiser, Dustin; Reusch, Engelbert; Hemberger, Patrick; Preitschopf, Tobias; Krummenacher, Ivo; Engels, Bernd; Fischer, Ingo; Lichtenberg, Crispin; Chemical Science  (2020) –; doi:10.1039/D0SC02410D

data_1558171
_publ_section_title
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 Methylbismuth: an Organometallic Bismuthinidene Biradical
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02410D
_journal_year                    2020
_chemical_formula_moiety         'C13 H13 Bi S2'
_chemical_formula_sum            'C13 H13 Bi S2'
_chemical_formula_weight         442.33
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-22 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                108.600(4)
_cell_angle_beta                 94.491(4)
_cell_angle_gamma                90.019(4)
_cell_formula_units_Z            2
_cell_length_a                   4.0972(12)
_cell_length_b                   10.591(3)
_cell_length_c                   16.590(5)
_cell_measurement_reflns_used    6503
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      2.60
_cell_volume                     680.0(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10552
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.939
_diffrn_reflns_theta_min         2.600
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.243
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0842 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.6775.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_description       needle
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.593
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.503
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2944
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0212P)^2^+0.8399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2706
_reflns_number_total             2944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02410d2.cif
_cod_data_source_block           Compound_8
_cod_original_cell_volume        679.9(3)
_cod_database_code               1558171
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.047
_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. Uiso/Uaniso restraints and constraints
Uanis(C10A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.008
Uanis(C11) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C5A) = Uanis(C5)
Uanis(C11) = Uanis(C11A)
3. Others
 Sof(S1A)=Sof(S2A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C8A)=Sof(C13A)=
 Sof(H13A)=Sof(C12A)=Sof(H12A)=Sof(C9A)=Sof(H9A)=Sof(C11A)=Sof(H11A)=Sof(C10A)=
 Sof(H10A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=Sof(C11)=Sof(H11)=1-FVAR(1)
 Sof(S1)=Sof(S2)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C2)=Sof(C5A)=
 Sof(H5A)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C13A(H13A), C12A(H12A), C9A(H9A),
 C11A(H11A), C10A(H10A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A),
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
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_olex2_submission_special_instructions 'No special instructions were received'