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_7135139
_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         'C51 H107 Au Cl N Sb2 Si9, C5 H12'
_chemical_formula_sum            'C56 H119 Au Cl N Sb2 Si9'
_chemical_formula_weight         1535.24
_chemical_name_systematic        MB080
_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             2024-08-20
_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                 100.6480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0962(2)
_cell_length_b                   23.3405(3)
_cell_length_c                   18.1023(2)
_cell_measurement_reflns_used    187593
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      2.09
_cell_volume                     7514.29(15)
_computing_cell_refinement       'X-Area Recipe 2.0.1 (STOE, 2023)'
_computing_data_collection       'X-Area WinXpose 2.0.29.0 (STOE, 2023)'
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_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      100
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            183393
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.707
_diffrn_reflns_theta_min         2.087
_diffrn_source                   'Anton Paar Primux50'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  0.6240
_exptl_absorpt_correction_T_min  0.4962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'ashlar block'
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.456
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         21177
_refine_ls_number_restraints     599
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0499P)^2^+56.9619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20647
_reflns_number_total             21177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04941e2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7135139--7135140.cif.'
_cod_database_code               7135139
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8979(5)
 0.1021(5)
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. Restrained distances
 C57-C58 = C58-C59 = C59-C60 = C60-C61
 1.52 with sigma of 0.02
 C52-C53 = C53-C54 = C54-C55 = C55-C56
 1.52 with sigma of 0.02
 C57-C59 = C58-C60 = C59-C61
 2.54 with sigma of 0.04
 C52-C54 = C53-C55 = C54-C56
 2.54 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=
 Sof(H40F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
 Fixed Sof: 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) C56(0.5)
 H56A(0.5) H56B(0.5) H56C(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5)
 H58A(0.5) H58B(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C18(H18), C31(H31), C42(H42)
7.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C27(H27), C29(H29)
7.d Idealised Me refined as rotating group:
 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),
 C39A(H39D,H39E,H39F), C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F), C41(H41A,H41B,
 H41C), C41A(H41D,H41E,H41F), 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), C52(H52A,
 H52B,H52C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              92214
_olex2_submission_special_instructions 'No special instructions were received'