Activation of carbon disulfide by a hypersilyl germylene.
Ajithkumar, V. S.; Khilari, Nripen; Ghanwat, Pratiksha B.; Venugopal, Geethu; Koley, Debasis; Sen, Sakya S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10814–10818; doi:10.1039/d4dt01573h

data_7716229
_publ_section_title
;
 Activation of carbon disulfide by a hypersilyl germylene.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10814
_journal_page_last               10818
_journal_paper_doi               10.1039/d4dt01573h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C25 H50 Ge N2 S2 Si4'
_chemical_formula_sum            'C25 H50 Ge N2 S2 Si4'
_chemical_formula_weight         627.74
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'Difference Fourier'
_audit_creation_date             2024-01-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-13 deposited with the CCDC.	2024-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                87.922(5)
_cell_angle_beta                 79.937(4)
_cell_angle_gamma                79.857(5)
_cell_formula_units_Z            6
_cell_length_a                   9.8098(14)
_cell_length_b                   23.143(4)
_cell_length_c                   24.199(3)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.46
_cell_volume                     5324.7(14)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon II CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.1061
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            123414
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.977
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Incoatech I\mS HB'
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  0.0991
_exptl_absorpt_correction_T_min  0.0645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.768
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Flack x determined using 13991 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.116(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1952
_refine_ls_number_reflns         49867
_refine_ls_number_restraints     431
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1227P)^2^+12.0256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                39932
_reflns_number_total             49867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01573h2.cif
_cod_data_source_block           mo_LGeCS2SiTMS3_UV_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct Method' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7716229--7716230.cif.
;
_cod_original_cell_volume        5324.7(13)
_cod_database_code               7716229
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.70463
 0.29537
2. Restrained distances
 C51-Ge3
 2.45 with sigma of 0.02
 Si20-C125
 1.85 with sigma of 0.02
 Si20-C12'
 1.85 with sigma of 0.02
 Si24-C148
 1.85 with sigma of 0.02
 Si24-C149
 1.85 with sigma of 0.02
 Si24-C150
 1.85 with sigma of 0.02
 Si24-C151
 1.85 with sigma of 0.02
 Si24-C153
 1.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S5) \\sim Ueq, Uanis(S6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(S11) \\sim Ueq, Uanis(S12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N7) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N9) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N11) \\sim Ueq, Uanis(N12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C12) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C56) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C58) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C86) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C140) \\sim Ueq, Uanis(C138) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C143) \\sim Ueq, Uanis(C144) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C121) \\sim Ueq, Uanis(C120) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C123) \\sim Ueq, Uanis(C124) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C125) \\sim Ueq, Uanis(C12') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C126) \\sim Ueq, Uanis(C127) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C134) \\sim Ueq, Uanis(C135) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C142) \\sim Ueq, Uanis(C143) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C147) \\sim Ueq, Uanis(C148) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C148) \\sim Ueq, Uanis(C149) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C148) \\sim Ueq, Uanis(C151) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C150) \\sim Ueq, Uanis(C153) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C125(0.7) H12S(0.7) H12T(0.7) H12U(0.7) C12'(0.3) H12V(0.3)
 H12W(0.3) H12X(0.3) C148(0.35) H113(0.35) H114(0.35) H115(0.35) C150(0.35)
 H15D(0.35) H15E(0.35) H15F(0.35) C151(0.65) H15G(0.65) H15H(0.65) H15I(0.65)
 C153(0.65) H15J(0.65) H15K(0.65) H15L(0.65)
5.a Me refined with riding coordinates:
 C125(H12S,H12T,H12U), C12'(H12V,H12W,H12X), C148(H113,H114,H115), C150(H15D,
 H15E,H15F), C151(H15G,H15H,H15I), C153(H15J,H15K,H15L)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C78(H78),
  C79(H79), C80(H80), C81(H81), C82(H82), C103(H103), C104(H104), C105(H105),
 C106(H106), C107(H107), C128(H128), C129(H129), C130(H130), C131(H131),
 C132(H132)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,
 H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,
 H86C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C),
 C96(H96A,H96B,H96C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,
 H99C), C100(H10D,H10E,H10F), C109(H10G,H10H,H10I), C110(H11G,H11H,H11I),
 C111(H11D,H11E,H11F), C113(H11J,H11K,H11L), C114(H11M,H11N,H11O), C115(H11P,
 H11Q,H11R), C117(H11S,H11T,H11U), C118(H11V,H11W,H11X), C119(H11Y,H11Z,H11'),
 C120(H12D,H12E,H12F), C121(H12G,H12H,H12I), C122(H12J,H12K,H12L), C123(H12M,
 H12N,H12O), C124(H12P,H12Q,H12R), C134(H13D,H13E,H13F), C135(H13G,H13H,H13I),
 C136(H13J,H13K,H13L), C138(H13M,H13N,H13O), C139(H13P,H13Q,H13R), C140(H14D,
 H14E,H14F), C142(H14G,H14H,H14I), C143(H14J,H14K,H14L), C144(H14M,H14N,H14O),
 C145(H14P,H14Q,H14R), C146(H14S,H14T,H14U), C147(H14V,H14W,H14X), C149(H110,
 H111,H112)
;
_shelx_res_checksum              84727
_shelx_hkl_checksum              97992
_olex2_submission_special_instructions 'No special instructions were received'