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_7129045
_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         'C96 H138 Bi4 Sn4, 2(C2 H5 O)'
_chemical_formula_sum            'C100 H148 Bi4 O2 Sn4'
_chemical_formula_weight         2692.86
_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   mixed
_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                78.431(2)
_cell_angle_beta                 80.056(2)
_cell_angle_gamma                75.059(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2666(9)
_cell_length_b                   16.4529(8)
_cell_length_c                   21.8940(12)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.65
_cell_volume                     5162.8(5)
_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      100.11
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1138
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            145026
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.585
_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    7.784
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1593 before and 0.0965 after correction.
The Ratio of minimum to maximum transmission is 0.3767.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       Block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.886
_refine_diff_density_min         -2.599
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         20225
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0380P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15377
_reflns_number_total             20225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02538d2.cif
_cod_data_source_block           rf1905a_1_0m
_cod_database_code               7129045
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.455
_shelx_estimated_absorpt_t_min   0.211
_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, All Sn(H) groups
2. Restrained distances
 Sn1-H \\sim Sn4-HA
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C61) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34), C43(H43), C46(H46),
 C55(H55), C58(H58), C67(H67), C70(H70), C79(H79), C82(H82), C91(H91), C94(H94)
4.b Secondary CH2 refined with riding coordinates:
 C98(H98A,H98B), C99(H99A,H99B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C39(H39), C40(H40), C41(H41), C51(H51), C52(H52), C53(H53), C63(H63),
  C64(H64), C65(H65), C75(H75), C76(H76), C77(H77), C87(H87), C88(H88), C89(H89)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), 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),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C100(H10A,H10B,H10C),
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              71245
_shelx_hkl_checksum              50700
_olex2_submission_special_instructions 'No special instructions were received'