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_7128882
_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         'C91 H128 Cu3 Na6 O7 P3 S18 Si9, 2(C4 H8 O)'
_chemical_formula_sum            'C103 H152 Cu3 Na6 O10 P3 S18 Si9'
_chemical_formula_weight         2801.60
_chemical_name_systematic        Na2[(Me3PCu)(PhSi)3S6]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                107.582(3)
_cell_angle_beta                 115.295(3)
_cell_angle_gamma                99.475(3)
_cell_formula_units_Z            2
_cell_length_a                   19.0521(9)
_cell_length_b                   19.7933(8)
_cell_length_c                   21.5839(9)
_cell_measurement_reflns_used    74013
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      1.12
_cell_volume                     6595.4(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'IPDS II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            86552
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.807
_diffrn_reflns_theta_min         1.384
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.8418
_exptl_absorpt_correction_T_min  0.8408
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             2924
_refine_diff_density_max         1.830
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         27877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0478P)^2^+6.2245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21558
_reflns_number_total             27877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04264e2.cif
_cod_data_source_block           sr26_2_sq
_cod_depositor_comments
'Adding full bibliography for 7128881--7128882.cif.'
_cod_original_cell_volume        6595.4(5)
_cod_database_code               7128882
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C58(H58A,H58B), C59(H59A,H59B), C86(H86A,H86B), C21(H21A,
 H21B), C26(H26A,H26B), C52(H52B,H52A), C54(H54A,H54B), C25(H25A,H25B),
 C88(H88A,H88B), C55(H55A,H55B), C30(H30A,H30B), C53(H53A,H53B), C87(H87A,H87B),
  C85(H85A,H85B), C19(H19A,H19B), C23(H23A,H23B), C20(H20A,H20B), C56(H56A,
 H56B), C57(H57A,H57B), C24(H24A,H24B), C27(H27A,H27B), C29(H29A,H29B),
 C28(H28A,H28B), C100(H10A,H10B), C95(H95A,H95B), C83(H83A,H83B), C103(H10C,
 H10D), C92(H92A,H92B), C101(H10E,H10F), C102(H10G,H10H), C81(H81A,H81B),
 C93(H93A,H93B), C94(H94A,H94B), C84(H84A,H84B), C82(H82A,H82B)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C76(H76), C18(H18), C16(H16), C41(H41), C6(H6), C2(H2), C45(H45),
 C47(H47), C14(H14), C15(H15), C17(H17), C35(H35), C51(H51), C68(H68), C64(H64),
  C36(H36), C39(H39), C37(H37), C78(H78), C3(H3), C77(H77), C65(H65), C43(H43),
 C10(H10), C44(H44), C5(H5), C38(H38), C66(H66), C74(H74), C73(H73), C4(H4),
 C50(H50), C48(H48), C12(H12), C80(H80), C79(H79), C67(H67), C49(H49), C72(H72),
  C70(H70), C8(H8), C11(H11), C9(H9), C71(H71)
2.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C90(H90A,H90B,
 H90C), C62(H62A,H62B,H62C), C91(H91A,H91B,H91C), C33(H33A,H33B,H33C), C89(H89A,
 H89B,H89C), C61(H61A,H61B,H61C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8098
_shelx_hkl_checksum              17531
_shelx_fab_checksum              75328
_olex2_submission_special_instructions 'No special instructions were received'