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_7710958
_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         'C84 H216 Au4 Ge18 P4 Si16'
_chemical_formula_sum            'C84 H216 Au4 Ge18 P4 Si16'
_chemical_formula_weight         3894.36
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2021-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2022(2)
_cell_length_b                   15.1707(2)
_cell_length_c                   27.4875(3)
_cell_measurement_reflns_used    77581
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      38.2050
_cell_measurement_theta_min      2.0110
_cell_volume                     7447.92(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     24.00  88.00   0.50   30.00    --   31.72-145.00-133.00  128
  2  \w     13.00  76.00   0.50   30.00    --   31.72-125.00  33.00  126
  3  \w    -49.00  43.00   0.50   30.00    --  -29.22  77.00 120.00  184
  4  \w    -27.00   1.00   0.50   30.00    --  -29.22 -98.00 171.15   56
  5  \w   -101.00 -10.00   0.50   30.00    --  -29.22 -77.00  60.00  182
  6  \w    -34.00  -2.00   0.50   30.00    --  -29.22 -93.00 -40.76   64
  7  \w    -42.00  -8.00   0.50   30.00    --  -29.22 -81.00 118.75   68
  8  \w    -40.00   5.00   0.50   30.00    --   31.72 -19.00-150.00   90
  9  \w     39.00 103.00   0.50   30.00    --   31.72-178.00 150.00  128
 10  \w    -39.00  21.00   0.50   30.00    --   31.72 -37.00 120.00  120
 11  \w     16.00  79.00   0.50   30.00    --   31.72-130.00-101.65  126
 12  \w      7.00  72.00   0.50   30.00    --   31.72-116.00  18.42  130
 13  \w    -40.00   5.00   0.50   30.00    --   31.72 -19.00  30.00   90
 14  \w     15.00  78.00   0.50   30.00    --   31.72-128.00  71.08  126
 15  \w    -17.00  38.00   0.50   30.00    --   31.72   0.00 -90.00  110
 16  \w     42.00 102.00   0.50   30.00    --   31.72 178.00 -30.00  120
 17  \w    -23.00  62.00   0.50   30.00    --   31.72 -99.00 120.00  170
 18  \w    -40.00   5.00   0.50   30.00    --   31.72 -19.00 150.00   90
 19  \w    -39.00  21.00   0.50   30.00    --   31.72 -37.00 -90.00  120
 20  \w    -40.00   5.00   0.50   30.00    --   31.72 -19.00  60.00   90
 21  \w     12.00  37.00   0.50   30.00    --   31.72  77.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0061089000
_diffrn_orient_matrix_UB_12      0.0141535000
_diffrn_orient_matrix_UB_13      0.0234978000
_diffrn_orient_matrix_UB_21      -0.0009851000
_diffrn_orient_matrix_UB_22      0.0444453000
_diffrn_orient_matrix_UB_23      -0.0081173000
_diffrn_orient_matrix_UB_31      -0.0392154000
_diffrn_orient_matrix_UB_32      -0.0033198000
_diffrn_orient_matrix_UB_33      -0.0085798000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            174242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.001
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.695
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf, toluene, pentane'
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.053
_refine_diff_density_max         3.312
_refine_diff_density_min         -2.380
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         14643
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0279P)^2^+31.7513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12563
_reflns_number_total             14643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01665f2.cif
_cod_data_source_block           1008g2s
_cod_database_code               7710958
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C82H212Au4Ge18P4Si16
_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
 C110-C109 = C114-C113 = C115-C114 = C111-C110 = C112-C111 = C116-C115
 1.54 with sigma of 0.02
 C214-C213 = C210-C209 = C214-C215 = C211-C210 = C216-C215 = C211-C212
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C110 \\sim C114: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C111 \\sim C115: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C109 \\sim C113: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C209 \\sim C213: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C116) \\sim Ueq, Uanis(C112) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C213)=Sof(H21H)=Sof(H21I)=Sof(C214)=Sof(H21J)=Sof(H21K)=Sof(C215)=
 Sof(H21L)=Sof(H21M)=Sof(C216)=Sof(H21N)=Sof(H21O)=Sof(H21P)=1-FVAR(1)
 Sof(C209)=Sof(H20S)=Sof(H20T)=Sof(C210)=Sof(H21A)=Sof(H21B)=Sof(C211)=
 Sof(H21C)=Sof(H21D)=Sof(C212)=Sof(H21E)=Sof(H21F)=Sof(H21G)=FVAR(1)
 Sof(C113)=Sof(H11H)=Sof(H11I)=Sof(C114)=Sof(H11J)=Sof(H11K)=Sof(C115)=
 Sof(H11L)=Sof(H11M)=Sof(C116)=Sof(H11N)=Sof(H11O)=Sof(H11P)=1-FVAR(2)
 Sof(C109)=Sof(H10S)=Sof(H10T)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(C111)=
 Sof(H11C)=Sof(H11D)=Sof(C112)=Sof(H11E)=Sof(H11F)=Sof(H11G)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C105(H10J,H10K), C106(H10L,
 H10M), C107(H10N,H10O), C109(H10S,H10T), C110(H11A,H11B), C111(H11C,H11D),
 C113(H11H,H11I), C114(H11J,H11K), C115(H11L,H11M), C201(H20A,H20B), C202(H20C,
 H20D), C203(H20E,H20F), C205(H20J,H20K), C206(H20L,H20M), C207(H20N,H20O),
 C209(H20S,H20T), C210(H21A,H21B), C211(H21C,H21D), C213(H21H,H21I), C214(H21J,
 H21K), C215(H21L,H21M)
5.b Me refined with riding coordinates:
 C104(H10G,H10H,H10I), C108(H10P,H10Q,H10R), C112(H11E,H11F,H11G), C116(H11N,
 H11O,H11P), C204(H20G,H20H,H20I), C208(H20P,H20Q,H20R), C212(H21E,H21F,H21G),
 C216(H21N,H21O,H21P), 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)
;
_shelx_res_checksum              95612
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.486
_oxdiff_exptl_absorpt_empirical_full_min 0.758
_oxdiff_exptl_absorpt_spherical_max 0.575
_oxdiff_exptl_absorpt_spherical_min 0.559