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_1574988
_publ_section_title
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 Driving diverse bond functionalisation with <i>N</i>-heterocyclic
 silylene-coinage metal-aryl complexes.
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_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_absolute_configuration unk
_chemical_formula_moiety         'C25 H45 Cu N4 Si3, 0.5[C7H8]'
_chemical_formula_sum            'C28.5 H49 Cu N4 Si3'
_chemical_formula_weight         595.536
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_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                 101.101(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.9008(19)
_cell_length_b                   40.360(8)
_cell_length_c                   19.289(4)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.29
_cell_volume                     6800(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1412
_diffrn_reflns_av_unetI/netI     0.1440
_diffrn_reflns_Laue_measured_fraction_full 0.9984
_diffrn_reflns_Laue_measured_fraction_max 0.9984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53846
_diffrn_reflns_point_group_measured_fraction_full 0.9589
_diffrn_reflns_point_group_measured_fraction_max 0.9588
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.770
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             2557.916
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.0897
_refine_diff_density_min         -1.2133
_refine_diff_density_rms         0.2118
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.048(9)
_refine_ls_d_res_high            0.8331
_refine_ls_d_res_low             10.0899
_refine_ls_goodness_of_fit_ref   1.0676
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    143
_refine_ls_number_parameters     636
_refine_ls_number_reflns         11808
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.0616
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.1018
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+124.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.2047
_reflns_Friedel_coverage         0.919
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              48
_reflns_limit_k_min              -48
_reflns_limit_l_max              20
_reflns_limit_l_min              -23
_reflns_number_gt                8409
_reflns_number_total             11808
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5sc00879d2.cif
_cod_data_source_block           TRY_a
_cod_depositor_comments
'Adding full bibliography for 1574965--1574988.cif.'
_cod_original_cell_volume        6799(2)
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_original_formula_sum        'C28.5 H49 Cu1 N4 Si3'
_cod_database_code               1574988
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80396
 0.19604
2. Restrained distances
 N8-C47
 1.38 with sigma of 0.02
 C47-C56
 1.35 with sigma of 0.02
 C57-C56
 1.4 with sigma of 0.02
 C57-C49
 1.35 with sigma of 0.02
 N8-C49
 1.38 with sigma of 0.02
 N8-C49 \\sim N8-C49a
 with sigma of 0.02
 N8-C47 \\sim N8-C47a
 with sigma of 0.02
 C49-C57 \\sim C49a-C57a
 with sigma of 0.02
 C57-C56 \\sim C57a-C56
 with sigma of 0.02
 C56-C47 \\sim C56-C47a
 with sigma of 0.02
 N8-C57 \\sim N8-C57a
 with sigma of 0.04
 C49-C56 \\sim C49a-C56
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N8) \\sim Ueq, Uanis(C49a) \\sim Ueq, Uanis(C57a) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C47a) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C45) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C47) = Uanis(C47a)
Uanis(C57) = Uanis(C57a)
4. Others
 Sof(H56a)=Sof(C49a)=Sof(H49a)=Sof(C47a)=Sof(H47a)=Sof(C57a)=Sof(H57a)=1-FVAR(1)
 Sof(C49)=Sof(H49)=Sof(C57)=Sof(H57)=Sof(H56)=Sof(C47)=Sof(H47)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C3(H3), C28(H28), C7(H7), C25(H25), C29(H29), C6(H6), C22(H22),
 C31(H31), C23(H23), C30(H30), C24(H24), C5(H5), C4(H4), C49(H49), C57(H57),
 C56(H56), C56(H56a), C47(H47), C49a(H49a), C47a(H47a), C57a(H57a)
5.b Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C11(H11a,H11b,H11c), C9(H9a,H9b,H9c), C15(H15a,H15b,
 H15c), C10(H10a,H10b,H10c), C39(H39a,H39b,H39c), C34(H34a,H34b,H34c), C35(H35a,
 H35b,H35c), C45(H45a,H45b,H45c), C40(H40a,H40b,H40c), C17(H17a,H17b,H17c),
 C42(H42a,H42b,H42c), C41(H41a,H41b,H41c), C18(H18a,H18b,H18c), C19(H19a,H19b,
 H19c), C43(H43a,H43b,H43c), C20(H20a,H20b,H20c), C14(H14a,H14b,H14c), C21(H21a,
 H21b,H21c), C44(H44a,H44b,H44c), C13(H13a,H13b,H13c), C36(H36a,H36b,H36c),
 C16(H16a,H16b,H16c), C46(H46a,H46b,H46c)
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_smtbx_masks_special_details
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A solvent mask was calculated and 216 electrons were 
found in a volume of 864\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.5[C7H8] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'