Synthesis and reactivity of a small distibacycle featuring an Au-Sb bimetallic linkage.
Palui, Prasenjit; Bollenbeck, Matthias; Langellotti, Vincenzo; Schnakenburg, Gregor; Gomila, Rosa M.; Frontera, Antonio; Bismuto, Alessandro; Chemical communications (Cambridge, England) 61 (2025) 19309–19312; doi:10.1039/d5cc04941e

data_7135140
_publ_section_title
;
 Synthesis and reactivity of a small distibacycle featuring an Au-Sb
 bimetallic linkage.
;
_journal_issue                   97
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              19309
_journal_page_last               19312
_journal_paper_doi               10.1039/d5cc04941e
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         '2(C51 H107 Au Cl N Sb2 Si9), C4 H10 O'
_chemical_formula_sum            'C106 H224 Au2 Cl2 N2 O Sb4 Si18'
_chemical_formula_weight         3000.31
_chemical_name_systematic        MBO80-2
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-08-13 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.1800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5283(3)
_cell_length_b                   36.1287(8)
_cell_length_c                   17.2150(4)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    104.00
_cell_measurement_theta_max      28.610
_cell_measurement_theta_min      2.413
_cell_volume                     7359.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      104.00
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS 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 D8 Venture'
_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  0.0936
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            99734
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.853
_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
_exptl_absorpt_coefficient_mu    2.931
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1151 before and 0.0757 after correction.
The Ratio of minimum to maximum transmission is 0.8333.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       plate
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         16043
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0179P)^2^+10.8044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13073
_reflns_number_total             16043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04941e2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7135139--7135140.cif.'
_cod_database_code               7135140
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.540
_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. Restrained distances
 O-C54
 1.41 with sigma of 0.02
 O-C53
 1.42 with sigma of 0.02
 C55-C54
 1.48 with sigma of 0.02
 C53-C52
 1.5 with sigma of 0.02
 O-C55 = O-C52
 2.37 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C01V, C3A, C4, C14, C15, C16, C17, C48, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C01V)=Sof(H01A)=Sof(H01B)=Sof(H01C)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(H3AC)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Fixed Sof: O(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C18(H18), C31(H31), C42(H42)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C27(H27), C29(H29)
5.d Idealised Me refined as rotating group:
 C01V(H01A,H01B,H01C), C3A(H3AA,H3AB,H3AC), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C),
 C55(H55A,H55B,H55C)
;
_shelx_res_checksum              30992
_olex2_submission_special_instructions 'No special instructions were received'