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_7129047
_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         '0.5(C120 H186 Bi4 Sn4)'
_chemical_formula_sum            'C60 H93 Bi2 Sn2'
_chemical_formula_weight         1469.68
_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     dual
_audit_creation_date             2020-10-21
_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                78.826(2)
_cell_angle_beta                 89.605(2)
_cell_angle_gamma                81.323(2)
_cell_formula_units_Z            4
_cell_length_a                   14.1148(5)
_cell_length_b                   14.1612(5)
_cell_length_c                   31.9318(11)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.17
_cell_volume                     6188.3(4)
_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      100.01
_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  0.1346
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            189677
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         0.650
_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    6.501
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1574 before and 0.0986 after correction.
The Ratio of minimum to maximum transmission is 0.5052.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             2876
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.748
_refine_diff_density_min         -2.500
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1373
_refine_ls_number_reflns         26972
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0015P)^2^+123.5326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18522
_reflns_number_total             26972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02538d2.cif
_cod_data_source_block           rf1909_2_0m
_cod_database_code               7129047
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.263
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H99A,H99B,H99C} of C99, {H25D,H25E,H25F} of C256, {H56A,
  H56B,H56C} of C56, All Sn(H) groups
 At 1.5 times of:
  {H69A,H69B,H69C} of C69, {H86A,H86B,H86C} of C86, {H71A,H71B,H71C} of C71,
  {H24A,H24B,H24C} of C24, {H27A,H27B,H27C} of C27, {H68A,H68B,H68C} of C68,
  {H39A,H39B,H39C} of C39, {H12A,H12B,H12C} of C120, {H26A,H26B,H26C} of C26,
  {H75A,H75B,H75C} of C75, {H38A,H38B,H38C} of C38, {H11J,H11K,H11L} of C117,
  {H53A,H53B,H53C} of C53, {H11G,H11H,H11I} of C116, {H89A,H89B,H89C} of C89,
  {H21D,H21E,H21F} of C212, {H11P,H11Q,H11R} of C11, {H60A,H60B,H60C} of C60,
  {H10G,H10H,H10I} of C104, {H9A,H9B,H9C} of C9, {H14A,H14B,H14C} of C14, {H10A,
  H10B,H10C} of C101, {H72A,H72B,H72C} of C72, {H20D,H20E,H20F} of C209, {H41A,
  H41B,H41C} of C41, {H29A,H29B,H29C} of C29, {H45A,H45B,H45C} of C45, {H21J,
  H21K,H21L} of C215, {H11D,H11E,H11F} of C114, {H10D,H10E,H10F} of C102, {H98A,
  H98B,H98C} of C98, {H90A,H90B,H90C} of C90, {H84A,H84B,H84C} of C84, {H42A,
  H42B,H42C} of C42, {H21G,H21H,H21I} of C214, {H74A,H74B,H74C} of C74, {H25A,
  H25B,H25C} of C257, {H20A,H20B,H20C} of C208, {H44A,H44B,H44C} of C44, {H15A,
  H15B,H15C} of C15, {H21A,H21B,H21C} of C211, {H11M,H11N,H11O} of C119, {H11A,
  H11B,H11C} of C113, {H87A,H87B,H87C} of C87, {H83A,H83B,H83C} of C83, {H59A,
  H59B,H59C} of C59, {H23A,H23B,H23C} of C23, {H54A,H54B,H54C} of C54, {H10J,
  H10K,H10L} of C105, {H12D,H12E,H12F} of C12, {H8A,H8B,H8C} of C8, {H57A,H57B,
  H57C} of C57, {H30A,H30B,H30C} of C30
2. Restrained distances
 C1-C4 \\sim C2-C5 \\sim C3-C6 \\sim C201-C204 \\sim C202-C205 \\sim C203-C206
 with sigma of 0.01
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C1
 with sigma of 0.01
 C201-C202 \\sim C202-C203 \\sim C203-C204 \\sim C204-C205 \\sim C205-C206
\\sim C206-C201
 with sigma of 0.01
 C10-C11 \\sim C10-C12 \\sim C7-C8 \\sim C7-C9 \\sim C13-C14 \\sim C13-C15
\\sim C213-C214 \\sim C213-C215
 with sigma of 0.01
 C55-C56 \\sim C55-C57 \\sim C255-C256 \\sim C255-C257
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim
C15 \\sim C207 \\sim C208 \\sim C209 \\sim C210 \\sim C211 \\sim C212 \\sim
C213: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C55 \\sim C56 \\sim C57 \\sim C255 \\sim C256 \\sim C257: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C255)
\\sim Ueq, Uanis(C256) \\sim Ueq, Uanis(C257) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C201)=Sof(C202)=Sof(C203)=Sof(H203)=Sof(C204)=Sof(C205)=Sof(H205)=
 Sof(C206)=Sof(C207)=Sof(H207)=Sof(C208)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C209)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C210)=Sof(H210)=Sof(C211)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C212)=Sof(H21D)=Sof(H21E)=Sof(H21F)=
 Sof(C213)=Sof(H213)=Sof(C214)=Sof(H21G)=Sof(H21H)=Sof(H21I)=Sof(C215)=
 Sof(H21J)=Sof(H21K)=Sof(H21L)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=
 Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11P)=Sof(H11Q)=Sof(H11R)=Sof(C12)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C257)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C256)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C255)=Sof(H255)=1-FVAR(2)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C55)=Sof(H55)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 Sn1(H), Sn4(HA), C22(H22), C25(H25), C28(H28), C37(H37), C40(H40), C43(H43),
 C52(H52), C58(H58), C67(H67), C70(H70), C73(H73), C82(H82), C85(H85), C88(H88),
  C97(H97), C100(H100), C103(H103), C112(H112), C115(H115), C118(H118),
 C55(H55), C7(H7), C10(H10), C13(H13), C207(H207), C210(H210), C213(H213),
 C255(H255)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C33(H33), C35(H35), C48(H48), C50(H50), C63(H63),
 C65(H65), C78(H78), C80(H80), C93(H93), C95(H95), C108(H108), C110(H110),
 C3(H3), C5(H5), C203(H203), C205(H205)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,H87B,
 H87C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C98(H98A,H98B,H98C), C99(H99A,
 H99B,H99C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C104(H10G,H10H,H10I),
 C105(H10J,H10K,H10L), C113(H11A,H11B,H11C), C114(H11D,H11E,H11F), C116(H11G,
 H11H,H11I), C117(H11J,H11K,H11L), C119(H11M,H11N,H11O), C120(H12A,H12B,H12C),
 C57(H57A,H57B,H57C), C56(H56A,H56B,H56C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C11(H11P,H11Q,H11R), C12(H12D,H12E,H12F), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C208(H20A,H20B,H20C), C209(H20D,H20E,H20F), C211(H21A,H21B,H21C),
 C212(H21D,H21E,H21F), C214(H21G,H21H,H21I), C215(H21J,H21K,H21L), C257(H25A,
 H25B,H25C), C256(H25D,H25E,H25F)
;
_shelx_res_checksum              22425
_shelx_hkl_checksum              7772
_olex2_submission_special_instructions 'No special instructions were received'