Bismuthanylstibanes.
Marczenko, Katherine M.; Chitnis, Saurabh S.; Chemical communications (Cambridge, England) 56 (2020) 8015–8018; doi:10.1039/d0cc00254b

data_7125896
_publ_section_title
;
 Bismuthanylstibanes.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8015
_journal_page_last               8018
_journal_paper_doi               10.1039/d0cc00254b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C44 H72 Bi N4 Sb Si4, C3 H3'
_chemical_formula_sum            'C47 H75 Bi N4 Sb Si4'
_chemical_formula_weight         1139.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-07 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.486(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7148(10)
_cell_length_b                   24.8374(17)
_cell_length_c                   17.6977(10)
_cell_measurement_reflns_used    9393
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      63.47
_cell_measurement_theta_min      4.37
_cell_volume                     5093.0(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        63.501
_diffrn_reflns_theta_max         63.501
_diffrn_reflns_theta_min         3.089
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.067
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1659 before and 0.0922 after correction.
The Ratio of minimum to maximum transmission is 0.6785.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       plate
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.1225
_exptl_crystal_size_mid          0.0894
_exptl_crystal_size_min          0.0606
_refine_diff_density_max         1.773
_refine_diff_density_min         -2.083
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         8285
_refine_ls_number_restraints     601
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+79.8086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8105
_reflns_number_total             8285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00254b2.cif
_cod_data_source_block           final2
_cod_depositor_comments
'Adding full bibliography for 7125895--7125899.cif.'
_cod_database_code               7125896
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.528
_shelx_estimated_absorpt_t_min   0.320
_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
 Si05-N00A \\sim Si-N00A
 with sigma of 0.02
 Si05-C01B \\sim Si-C1AA
 with sigma of 0.02
 Si05-C01H \\sim Si-C0AA
 with sigma of 0.02
 Si05-C12 \\sim Si-C12A
 with sigma of 0.02
 N00A-C01B \\sim N00A-C1AA
 with sigma of 0.04
 N00A-C01H \\sim N00A-C0AA
 with sigma of 0.04
 N00A-C12 \\sim N00A-C12A
 with sigma of 0.04
 C01B-C01H \\sim C1AA-C0AA
 with sigma of 0.04
 C01B-C12 \\sim C1AA-C12A
 with sigma of 0.04
 C01H-C12 \\sim C0AA-C12A
 with sigma of 0.04
 Si06-N009 \\sim Si1-N009
 with sigma of 0.02
 Si06-C01F \\sim Si1-C2AA
 with sigma of 0.02
 Si06-C6 \\sim Si1-C6A
 with sigma of 0.02
 Si06-C7 \\sim Si1-C7A
 with sigma of 0.02
 N009-C01F \\sim N009-C2AA
 with sigma of 0.04
 N009-C6 \\sim N009-C6A
 with sigma of 0.04
 N009-C7 \\sim N009-C7A
 with sigma of 0.04
 C01F-C6 \\sim C2AA-C6A
 with sigma of 0.04
 C01F-C7 \\sim C2AA-C7A
 with sigma of 0.04
 C6-C7 \\sim C6A-C7A
 with sigma of 0.04
 C00F-C010 \\sim C00F-C3
 with sigma of 0.02
 C00G-C019 \\sim C00G-C0
 with sigma of 0.02
 C00L-C00N \\sim C00L-C3AA
 with sigma of 0.02
 C00N-C00S \\sim C3AA-C4AA
 with sigma of 0.02
 C00N-C016 \\sim C3AA-C2
 with sigma of 0.02
 C00S-C01C \\sim C4AA-C5AA
 with sigma of 0.02
 C010-C01C \\sim C3-C5AA
 with sigma of 0.02
 C016-C018 \\sim C2-C1
 with sigma of 0.02
 C018-C019 \\sim C1-C0
 with sigma of 0.02
 C00F-C01C \\sim C00F-C5AA
 with sigma of 0.04
 C00G-C018 \\sim C00G-C1
 with sigma of 0.04
 C00L-C00S \\sim C00L-C4AA
 with sigma of 0.04
 C00L-C016 \\sim C00L-C2
 with sigma of 0.04
 C00N-C018 \\sim C3AA-C1
 with sigma of 0.04
 C00N-C01C \\sim C3AA-C5AA
 with sigma of 0.04
 C00S-C010 \\sim C4AA-C3
 with sigma of 0.04
 C00S-C016 \\sim C4AA-C2
 with sigma of 0.04
 C016-C019 \\sim C2-C0
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C2AA) = Uanis(C6A) = Uanis(C12A) = Uanis(C7) = Uanis(C01F) = Uanis(C0AA)
= Uanis(C1AA)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(Si)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=
 Sof(H0AC)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(Si05)=Sof(C01B)=Sof(H01J)=Sof(H01K)=Sof(H01L)=Sof(C01H)=Sof(H01Z)=Sof(H)=
 Sof(HA)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(Si1)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(H7AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(2)
 Sof(Si06)=Sof(C01F)=Sof(H01T)=Sof(H01U)=Sof(H01V)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(2)
 Sof(C0)=Sof(H0)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3AA)=Sof(C4AA)=Sof(H4AA)=
 Sof(C5AA)=Sof(H5AA)=Sof(C3)=Sof(H3)=1-FVAR(3)
 Sof(C00N)=Sof(C00S)=Sof(H00S)=Sof(C010)=Sof(H010)=Sof(C016)=Sof(H016)=
 Sof(C018)=Sof(H018)=Sof(C019)=Sof(H019)=Sof(C01C)=Sof(H01M)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00O(H00O), C00Q(H00Q), C00U(H00U), C00Y(H00Y), C013(H013)
6.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00P(H00Z), C00S(H00S), C00V(H00), C00W(H00W),
 C00X(H00X), C010(H010), C011(H011), C012(H012), C015(H015), C016(H016),
 C018(H018), C019(H019), C01C(H01M), C0(H0), C1(H1), C2(H2), C4AA(H4AA),
 C5AA(H5AA), C3(H3)
6.c Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00C), C00M(H00D,H00E,H00F), C00R(H00G,H00K,H00L), C00T(H00M,
 H00N,H00P), C00Z(H00R,H00T,H00V), C014(H01A,H01B,H01C), C017(H01D,H01E,H01F),
 C01A(H01G,H01H,H01I), C01B(H01J,H01K,H01L), C01D(H01N,H01O,H01P), C01E(H01Q,
 H01R,H01S), C01F(H01T,H01U,H01V), C01G(H01W,H01X,H01Y), C01H(H01Z,H,HA),
 C01I(H01,HB,HC), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
 C12A(H12D,H12E,H12F), C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C2AA(H2AA,
 H2AB,H2AC), C7A(H7AA,H7AB,H7AC), C6A(H6AA,H6AB,H6AC)
;
_shelx_res_checksum              8093
_olex2_submission_special_instructions 'No special instructions were received'