Trinuclear anionic gold clusters bridged by dialkylsilylene and dialkylgermylene
Li, Yinhuan; Guorong, Zhen; Lu, Huang; Rong, Zhang; Wang, Liliang; Qi, Fan; Kira, Mitsuo; Li, Zhifang; Chemical Communications  (2022) –; doi:10.1039/D2CC02054H

data_7130072
_publ_section_title
;
 Trinuclear anionic gold clusters bridged by dialkylsilylene and
 dialkylgermylene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02054H
_journal_year                    2022
_chemical_formula_moiety         'C48 H120 Au3 Si15, K'
_chemical_formula_sum            'C56 H134 Au3 K O2 Si15'
_chemical_formula_weight         1890.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_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
;
2022-03-22 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0257(7)
_cell_length_b                   19.7111(8)
_cell_length_c                   28.0391(10)
_cell_measurement_reflns_used    6529
_cell_measurement_temperature    200
_cell_measurement_theta_max      60.06
_cell_measurement_theta_min      3.15
_cell_volume                     9962.5(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            124978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.702
_diffrn_reflns_theta_min         3.152
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.11
_diffrn_source_power             0.0555
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.454
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.2955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1699 before and 0.0997 after correction.
The Ratio of minimum to maximum transmission is 0.3924.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.799
_refine_diff_density_min         -1.881
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         9187
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1149P)^2^+99.8872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2461
_refine_ls_wR_factor_ref         0.2586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6955
_reflns_number_total             9187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02054h2.cif
_cod_data_source_block           cxy3118_0m
_cod_database_code               7130072
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.322
_shelx_estimated_absorpt_t_min   0.140
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9_$1-C8_$1 = C24-C24_$1
 1.54 with sigma of 0.02
 H22C-H18C
 2.2 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C9(H9A,H9B), C8(H8A,H8B)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C2(H2A,H2B,
 H2C), C18(H18A,H18B,H18C), C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C3(H3A,H3B,
 H3C), C12(H12A,H12B,H12C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              6570
_shelx_hkl_checksum              95843
_shelx_fab_checksum              78414
_olex2_submission_special_instructions 'No special instructions were received'