Driving diverse bond functionalisation with <i>N</i>-heterocyclic silylene-coinage metal-aryl complexes.
Ghosh, Moushakhi; Gaurav, Kumar; Panwaria, Prakash; Panday, Rishukumar; Tothadi, Srinu; Khan, Shabana; Chemical science 16 (2025) 14518–14533; doi:10.1039/d5sc00879d

data_1574980
_publ_section_title
;
 Driving diverse bond functionalisation with <i>N</i>-heterocyclic
 silylene-coinage metal-aryl complexes.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              14518
_journal_page_last               14533
_journal_paper_doi               10.1039/d5sc00879d
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '4(C30 H49 N3 Si2), 1[C7H8]'
_chemical_formula_sum            'C127 H196 N12 Si8'
_chemical_formula_weight         2115.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.573(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.070(4)
_cell_length_b                   39.582(15)
_cell_length_c                   16.882(6)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      2.47
_cell_volume                     6568(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            135403
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.036
_diffrn_reflns_theta_min         1.029
_diffrn_source_current           19.0
_diffrn_source_power             0.76
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6465
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.8670.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             2308
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         17298
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+6.1342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14173
_reflns_number_total             17298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00879d2.cif
_cod_data_source_block           a1_a_CCDC6
_cod_depositor_comments
'Adding full bibliography for 1574965--1574988.cif.'
_cod_database_code               1574980
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 C1A-C1B
 1.51 with sigma of 0.02
 C1B-C1C = C1B-C1G = C1D-C1E
 1.39 with sigma of 0.02
 C1C-C1D = C1E-C1F = C1F-C1G
 1.38 with sigma of 0.02
 C1A-C1C = C1A-C1G
 2.52 with sigma of 0.04
 C1B-C1D
 2.42 with sigma of 0.04
 C1B-C1F
 2.41 with sigma of 0.04
 C1C-C1E
 2.39 with sigma of 0.04
 C1D-C1F = C1E-C1G
 2.4 with sigma of 0.04
 C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1G \\sim C1G-C1B
 with sigma of 0.02
 C1B-C1F \\sim C1B-C1D \\sim C1G-C1E \\sim C1C-C1G \\sim C1D-C1F \\sim C1C-C1E
 with sigma of 0.04
 C1A-C1G \\sim C1A-C1C
 with sigma of 0.04
2. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C1G) \\sim Ueq, Uanis(C1F)
\\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1C) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C1A(0.5) C1B(0.5) C1C(0.5) C1D(0.5) C1E(0.5) C1F(0.5) C1G(0.5)
6.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C52(H52), C55(H55)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4), C7(H7), C6(H6), C21(H21), C22(H22), C23(H23),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C48(H48), C49(H49), C50(H50)
6.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), C16(H16A,H16B,H16C), C18(H18A,
 H18B,H18C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C)
;
_shelx_res_checksum              89096
_olex2_submission_special_instructions 'No special instructions were received'