From organotin hydrides to heteronuclear main group metal compounds: isolation of the first neutral bismuth/tin clusters.
Steller, Beate G.; Flock, Michaela; Fischer, Roland C.; Chemical communications (Cambridge, England) 57 (2021) 10095–10098; doi:10.1039/d1cc02538d

data_7129044
_publ_section_title
;
 From organotin hydrides to heteronuclear main group metal compounds:
 isolation of the first neutral bismuth/tin clusters.
;
_journal_issue                   78
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10095
_journal_page_last               10098
_journal_paper_doi               10.1039/d1cc02538d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C72 H102 Bi8 Sn3, 2(C4 H10 O2)'
_chemical_formula_sum            'C80 H122 Bi8 O4 Sn3'
_chemical_formula_weight         3175.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.630(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7205(9)
_cell_length_b                   16.5280(6)
_cell_length_c                   23.0120(9)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    100.14
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.68
_cell_volume                     9093.7(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.14
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            91234
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.999
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.904
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.269
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1476 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.4334.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_description       Block
_exptl_crystal_F_000             5792
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.253
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9928
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0297P)^2^+126.7436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8542
_reflns_number_total             9928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02538d2.cif
_cod_data_source_block           rf1966_0m_a
_cod_database_code               7129044
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.194
_shelx_estimated_absorpt_t_min   0.112
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34)
3.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C38(H38A,H38B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C5(H5), C16(H16), C15(H15), C17(H17), C27(H27), C28(H28),
 C29(H29)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C40(H40A,H40B,H40C), C37(H37A,H37B,H37C), C9(H9A,H9B,H9C),
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              18404
_shelx_hkl_checksum              88918
_olex2_submission_special_instructions 'No special instructions were received'