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_7129046
_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 H101 Bi2 Sn4, C4 H9 O2'
_chemical_formula_sum            'C76 H110 Bi2 O2 Sn4'
_chemical_formula_weight         1948.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1893(5)
_cell_length_b                   14.1893(5)
_cell_length_c                   37.5042(15)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.17
_cell_volume                     7551.0(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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0681
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            192012
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.086
_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    5.989
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1187 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.5380.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.591
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Flack x determined using 6536 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         16239
_refine_ls_number_restraints     469
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0553P)^2^+120.0653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15314
_reflns_number_total             16239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02538d2.cif
_cod_data_source_block           rf1964b_0m
_cod_original_cell_volume        7551.0(6)
_cod_database_code               7129046
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9005(11)
 0.0995(11)
2. 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
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C76) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.016
Uanis(C20) \\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), C70(H70), C67(H67),
 C58(H58), C55(H55), C46(H46), C43(H43)
4.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C75(H75A,H75B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28), C29(H29),
 C65(H65), C64(H64), C63(H63), C53(H53), C52(H52), C51(H51), C41(H41), C40(H40),
  C39(H39), C3(H3)
4.d X=CH2 refined with riding coordinates:
 C12(H12A,H12B), C76(H76A,H76B)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), 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), C72(H72A,
 H72B,H72C), C71(H71A,H71B,H71C), C69(H69A,H69B,H69C), C68(H68A,H68B,H68C),
 C60(H60A,H60B,H60C), C59(H59A,H59B,H59C), C57(H57A,H57B,H57C), C56(H56A,H56B,
 H56C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C), C44(H44A,
 H44B,H44C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              63579
_shelx_hkl_checksum              38629
_olex2_submission_special_instructions 'No special instructions were received'