Selective replacement of organosilicon units in the cluster [(PhSi)<sub>4</sub>S<sub>6</sub>] with coinage metal complex fragments.
Nier, Simon; Ringelband, Sven; Dehnen, Stefanie; Chemical communications (Cambridge, England) 57 (2021) 10254–10257; doi:10.1039/d1cc04264e

data_7128881
_publ_section_title
;
 Selective replacement of organosilicon units in the cluster
 [(PhSi)<sub>4</sub>S<sub>6</sub>] with coinage metal complex fragments.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10254
_journal_page_last               10257
_journal_paper_doi               10.1039/d1cc04264e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'0.5(C36 H60 Ag3 P3 S6 Si3), 0.5(C36 H59 Ag3 P3 S6 Si3), 0.5(H)'
_chemical_formula_sum            'C36 H60 Ag3 P3 S6 Si3'
_chemical_formula_weight         1185.99
_chemical_name_systematic        '[(Et3PAg)3(PhSi)3S6]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-29 deposited with the CCDC.	2021-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.1788(14)
_cell_length_b                   21.4061(7)
_cell_length_c                   11.3403(3)
_cell_measurement_reflns_used    39148
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      1.04
_cell_volume                     9753.5(5)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  IPDS2
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            75912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.670
_diffrn_reflns_theta_min         1.078
_exptl_absorpt_coefficient_mu    1.647
_exptl_absorpt_correction_T_max  16.5
_exptl_absorpt_correction_T_min  0.5
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   analytical
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_recrystallization_method
'Layering with n-hexane at roomtemperature under exclusion of light'
_exptl_crystal_size_max          0.1323
_exptl_crystal_size_mid          0.0739015
_exptl_crystal_size_min          0.015503
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.496(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         18262
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0268P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0536
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                14630
_reflns_number_total             18262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04264e2.cif
_cod_data_source_block           sn177_pl
_cod_depositor_comments
'Adding full bibliography for 7128881--7128882.cif.'
_cod_database_code               7128881
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.504(17)
 0.496(17)
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.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C55(H55A,H55B), C65(H65A,H65B), C61(H61A,H61B), C59(H59A,
 H59B), C63(H63A,H63B), C69(H69A,H69B), C71(H71A,H71B), C67(H67A,H67B),
 C35(H35A,H35B), C29(H29A,H29B), C25(H25A,H25B), C33(H33A,H33B), C27(H27A,H27B),
  C31(H31A,H31B), C23(H23A,H23B), C19(H19A,H19B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C52(H52), C53(H53), C54(H54), C44(H44), C48(H48), C42(H42),
 C45(H45), C51(H51), C40(H40), C38(H38), C46(H46), C47(H47), C41(H41), C39(H39),
  C14(H14), C2(H2), C15(H15), C17(H17), C3(H3), C6(H6), C18(H18), C12(H12),
 C11(H11), C16(H16), C4(H4), C5(H5), C8(H8), C10(H10), C9(H9)
3.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C70(H70A,H70B,H70C), C58(H58A,H58B,H58C), C68(H68A,H68B,
 H68C), C72(H72A,H72B,H72C), C56(H56A,H56B,H56C), C60(H60A,H60B,H60C), C66(H66A,
 H66B,H66C), C62(H62A,H62B,H62C), C36(H36A,H36B,H), C24(H24A,H24B,H24C),
 C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C20(H20A,H20B,
 H20C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              23467
_shelx_hkl_checksum              5906
_olex2_submission_special_instructions 'No special instructions were received'