On-demand switching from mono-silylene to bis-silylene to access mono-, di- and mixed coinage metal complexes.
Sun, Xiaofei; Jin, Da; Yadav, Ravi; Kraetschmer, Frederic; Köppe, Ralf; Roesky, Peter W.; Chemical science 16 (2025) 16057–16062; doi:10.1039/d5sc04287a

data_1575463
_publ_section_title
;
 On-demand switching from mono-silylene to bis-silylene to access mono-,
 di- and mixed coinage metal complexes.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              16057
_journal_page_last               16062
_journal_paper_doi               10.1039/d5sc04287a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C60 H85 Au2 N5 Si2, 4(C6 D6)'
_chemical_formula_sum            'C84 H85 Au2 D24 N5 Si2'
_chemical_formula_weight         1663.02
_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             2025-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-02 deposited with the CCDC.	2025-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.237(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4582(17)
_cell_length_b                   13.7319(8)
_cell_length_c                   25.7140(19)
_cell_measurement_reflns_used    30352
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.25
_cell_measurement_theta_min      2.18
_cell_volume                     7611.2(9)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details
;
 488 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28983
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.308
_diffrn_reflns_theta_min         2.186
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    3.929
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.381
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         10128
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0496P)^2^+40.5703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8262
_reflns_number_total             10128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04287a2.cif
_cod_data_source_block           xfjdaucu25-04-14
_cod_depositor_comments
'Adding full bibliography for 1575461--1575467.cif.'
_cod_database_code               1575463
__shelx_shelxl_version_number    2019/2
_audit_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_audit_contact_letter
;
;
_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. Restrained distances
 N2-C00L \\sim N2-C14
 with sigma of 0.02
 C00L-C013 \\sim C14-C16
 with sigma of 0.02
 C00L-C016 \\sim C14-C15
 with sigma of 0.02
 C00L-C017 \\sim C14-C17
 with sigma of 0.02
 N2-C013 \\sim N2-C16
 with sigma of 0.04
 N2-C016 \\sim N2-C15
 with sigma of 0.04
 N2-C017 \\sim N2-C17
 with sigma of 0.04
 C013-C016 \\sim C16-C15
 with sigma of 0.04
 C013-C017 \\sim C16-C17
 with sigma of 0.04
 C016-C017 \\sim C15-C17
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C00L \\sim C013 \\sim C14 \\sim C15 \\sim C16 \\sim C016 \\sim C017 \\sim C17:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=1-FVAR(1)
 Sof(C00L)=Sof(C013)=Sof(H01A)=Sof(H01B)=Sof(H01C)=Sof(C016)=Sof(H01D)=
 Sof(H01E)=Sof(H01F)=Sof(C017)=Sof(H01G)=Sof(H01H)=Sof(H01I)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C27(H27)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C30(H30),
 C31(H31), C38(D38), C39(D39), C40(D40), C41(D41), C42(D42), C43(D43), C32(D32),
  C33(D33), C34(D34), C35(D35), C36(D36), C37(D37)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C013(H01A,H01B,H01C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C016(H01D,H01E,H01F), C017(H01G,H01H,H01I),
 C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              6503
_olex2_submission_special_instructions 'No special instructions were received'