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_1575466
_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 Ag2 N5 Si2'
_chemical_formula_sum            'C60 H85 Ag2 N5 Si2'
_chemical_formula_weight         1148.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-24 deposited with the CCDC.	2025-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.425(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0057(10)
_cell_length_b                   25.263(2)
_cell_length_c                   17.7227(15)
_cell_measurement_reflns_used    38575
_cell_measurement_temperature    150
_cell_measurement_theta_max      64.64
_cell_measurement_theta_min      2.99
_cell_volume                     5760.2(8)
_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      150.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            Dectris
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  GaJET
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38672
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         64.561
_diffrn_reflns_theta_min         2.988
_exptl_absorpt_coefficient_mu    4.108
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.3581
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         13889
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11259
_reflns_number_total             13889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04287a2.cif
_cod_data_source_block           xfsi2ag2
_cod_depositor_comments
'Adding full bibliography for 1575461--1575467.cif.'
_cod_database_code               1575466
__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
;
;
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.494
_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-C20A \\sim N2-C20B
 with sigma of 0.02
 C20A-C23A \\sim C20B-C21B
 with sigma of 0.02
 C20A-C22A \\sim C20B-C22B
 with sigma of 0.02
 C20A-C21A \\sim C20B-C23B
 with sigma of 0.02
 C23A-C21A \\sim C21B-C23B
 with sigma of 0.04
 C23A-C22A \\sim C21B-C22B
 with sigma of 0.04
 C22A-C21A \\sim C22B-C23B
 with sigma of 0.04
 N2-C23A \\sim N2-C21B
 with sigma of 0.04
 N2-C22A \\sim N2-C22B
 with sigma of 0.04
 N2-C21A \\sim N2-C23B
 with sigma of 0.04
3. Rigid bond restraints
 C20B, C21B, C22B, C23B, C20A, C21A, C22A, C23A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20B \\sim C21B \\sim C22B \\sim C23B \\sim C20A \\sim C21A \\sim C22A \\sim
C23A: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2.5A
5. Others
 Sof(C20B)=Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22B)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(1)
 Sof(C20A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C36(H36), C37(H37), C38(H38), C52(H52), C53(H53), C54(H54), C55(H55),
  C56(H56)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C21B(H21A,H21B,H21C), C22B(H22A,H22B,
 H22C), C23B(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F)
;
_shelx_res_checksum              6886
_olex2_submission_special_instructions 'No special instructions were received'