Substitution of Hyp (Hyp = Si(SiMe3)3) at metalloid [Ge9(Hyp)3]- clusters using phosphine stabilized Au(I)Cl.
Schnepf, Andreas; Gienger, Christian; Dalton Transactions  (2022) –; doi:10.1039/D2DT01665F

data_7710960
_publ_section_title
;
 Substitution of Hyp (Hyp = Si(SiMe3)3) at metalloid [Ge9(Hyp)3]- clusters
 using phosphine stabilized Au(I)Cl.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01665F
_journal_year                    2022
_chemical_formula_moiety         'C72 H172 Au4 Ge18 O4 P4 Si16'
_chemical_formula_sum            'C72 H172 Au4 Ge18 O4 P4 Si16'
_chemical_formula_weight         3769.89
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.305(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7399(19)
_cell_length_b                   24.623(3)
_cell_length_c                   35.814(4)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.165
_cell_measurement_theta_min      2.384
_cell_volume                     13796(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  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_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 0.995
_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  0.0685
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            97050
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.594
_diffrn_reflns_theta_min         2.004
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.307
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1066 before and 0.0712 after correction.
The Ratio of minimum to maximum transmission is 0.6609.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             7248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, thf, toluene'
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         21106
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.004
_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^+40.5504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16272
_reflns_number_total             21106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01665f2.cif
_cod_data_source_block           42_sq
_cod_database_code               7710960
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.389
_shelx_estimated_absorpt_t_min   0.268
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C531 \\sim C541: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C533 \\sim C543: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
3. Others
 Sof(Si54)=Sof(C541)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C542)=Sof(H54D)=
 Sof(H54E)=Sof(H54F)=Sof(C543)=Sof(H54G)=Sof(H54H)=Sof(H54I)=1-FVAR(1)
 Sof(Si53)=Sof(C531)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C532)=Sof(H53D)=
 Sof(H53E)=Sof(H53F)=Sof(C533)=Sof(H53G)=Sof(H53H)=Sof(H53I)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C101(H101), C104(H104), C201(H201), C204(H204)
4.b Aromatic/amide H refined with riding coordinates:
 C109(H109), C110(H110), C209(H209), C210(H210)
4.c Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C103(H10D,H10E,H10F), C105(H10G,H10H,H10I), C106(H10J,
 H10K,H10L), C202(H20A,H20B,H20C), C203(H20D,H20E,H20F), C205(H20G,H20H,H20I),
 C206(H20J,H20K,H20L), C411(H41A,H41B,H41C), C412(H41D,H41E,H41F), C413(H41G,
 H41H,H41I), C421(H42A,H42B,H42C), C422(H42D,H42E,H42F), C423(H42G,H42H,H42I),
 C431(H43A,H43B,H43C), C432(H43D,H43E,H43F), C433(H43G,H43H,H43I), C511(H51A,
 H51B,H51C), C512(H51D,H51E,H51F), C513(H51G,H51H,H51I), C521(H52A,H52B,H52C),
 C522(H52D,H52E,H52F), C523(H52G,H52H,H52I), C531(H53A,H53B,H53C), C532(H53D,
 H53E,H53F), C533(H53G,H53H,H53I), C541(H54A,H54B,H54C), C542(H54D,H54E,H54F),
 C543(H54G,H54H,H54I)
;
_shelx_res_checksum              80450
_shelx_fab_checksum              61342
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'