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_1575461
_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         'C51 H74 Ag N5 Si2, C7 H8'
_chemical_formula_sum            'C58 H82 Ag N5 Si2'
_chemical_formula_weight         1013.33
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-22
_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                71.802(6)
_cell_angle_beta                 77.731(6)
_cell_angle_gamma                88.727(6)
_cell_formula_units_Z            2
_cell_length_a                   14.0034(11)
_cell_length_b                   14.5552(11)
_cell_length_c                   14.8701(11)
_cell_measurement_reflns_used    44656
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.60
_cell_volume                     2810.3(4)
_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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
 994 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'single reflection optic'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43558
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.229
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_type              'Xenocs Genix3D microfocus'
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4681
_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    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         13279
_refine_ls_number_restraints     428
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0491P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10543
_reflns_number_total             13279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04287a2.cif
_cod_data_source_block           xf-si2ag1-new
_cod_depositor_comments
'Adding full bibliography for 1575461--1575467.cif.'
_cod_database_code               1575461
_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   0.974
_shelx_estimated_absorpt_t_min   0.917
_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
 C53-C54 = C53-C58 = C55-C56
 1.39 with sigma of 0.02
 C60-C65 = C60-C61 = C64-C63
 1.39 with sigma of 0.02
 C52-C53
 1.51 with sigma of 0.02
 C59-C60
 1.51 with sigma of 0.02
 C54-C55 = C56-C57 = C57-C58
 1.38 with sigma of 0.02
 C65-C64 = C63-C62 = C62-C61
 1.38 with sigma of 0.02
 C60-C64
 2.42 with sigma of 0.04
 C65-C63
 2.39 with sigma of 0.04
 C60-C62
 2.41 with sigma of 0.04
 C64-C62 = C63-C61
 2.4 with sigma of 0.04
 C52-C54 = C52-C58
 2.52 with sigma of 0.04
 C53-C55
 2.42 with sigma of 0.04
 C53-C57
 2.41 with sigma of 0.04
 C54-C56
 2.39 with sigma of 0.04
 C59-C65 = C59-C61
 2.52 with sigma of 0.04
 C55-C57 = C56-C58
 2.4 with sigma of 0.04
 C53-C57 \\sim C53-C55 \\sim C58-C56 \\sim C54-C58 \\sim C55-C57 \\sim C54-C56
 with sigma of 0.04
 C60-C65 \\sim C65-C64 \\sim C64-C63 \\sim C63-C62 \\sim C62-C61 \\sim C61-C60
 with sigma of 0.02
 C53-C54 \\sim C54-C55 \\sim C55-C56 \\sim C56-C57 \\sim C57-C58 \\sim C58-C53
 with sigma of 0.02
 C60-C62 \\sim C60-C64 \\sim C61-C63 \\sim C65-C61 \\sim C64-C62 \\sim C65-C63
 with sigma of 0.04
 C59-C61 \\sim C59-C65
 with sigma of 0.04
 C52-C58 \\sim C52-C54
 with sigma of 0.04
3. Restrained planarity
 C59, C60, C61, C62, C63, C64, C65
 with sigma of 0.01
 C52, C53, C54, C55, C56, C57, C58
 with sigma of 0.1
4. Rigid bond restraints
 C59, C60, C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C52, C53, C54, C55, C56, C57, C58
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65: within 2.5A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 2.5A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 C52, C53, C54, C55, C56, C57, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C60, C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C56(0.5) H56(0.5) C57(0.5)
 H57(0.5) C58(0.5) H58(0.5) C53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5)
 C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5) C60(0.5) C61(0.5) H61(0.5) C62(0.5)
 H62(0.5) C63(0.5) H63(0.5) C64(0.5) H64(0.5) C65(0.5) H65(0.5)
8.a Ternary CH refined with riding coordinates:
 C16(H16), C21(H21)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C56(H56),
  C57(H57), C58(H58), C54(H54), C55(H55), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65)
8.c Fitted hexagon refined as free rotating group:
 C56(C57,C58,C53,C54,C55)
8.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              1219
_olex2_submission_special_instructions 'No special instructions were received'