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_1574967
_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         'C54 H90 B2 Cu2 N6 O4 Si6, 0.5[C7H8]'
_chemical_formula_sum            'C57.5 H94 B2 Cu2 N6 O4 Si6'
_chemical_formula_weight         1250.62
_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
_audit_creation_date             2025-05-11
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.861(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.839(2)
_cell_length_b                   18.764(4)
_cell_length_c                   17.165(4)
_cell_measurement_reflns_used    2845
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      17.77
_cell_measurement_theta_min      2.37
_cell_volume                     3489.2(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.5188
_diffrn_reflns_av_unetI/netI     0.3559
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45346
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.880
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5518
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1222 before and 0.0943 after correction.
The Ratio of minimum to maximum transmission is 0.7400.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1330
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6152
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.2414
_refine_ls_R_factor_gt           0.1016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.2244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2551
_reflns_number_total             6152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00879d2.cif
_cod_data_source_block           mo_mg_snt_cm_bcat_solve_0m_a
_cod_depositor_comments
'Adding full bibliography for 1574965--1574988.cif.'
_cod_original_formula_sum        'C57.50 H94 B2 Cu2 N6 O4 Si6'
_cod_database_code               1574967
_shelx_shelxl_version_number     2014/7
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Same fragment restrains
{C12A, C12A, C15A} sigma for 1-2: 0.02, 1-3: 0.04
{C12, C12, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C12, C14, C15}
{C9, C10, C11} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C9, C10, C11}
4. Others
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6), C5(H5), C24(H24), C25(H25), C26(H26), C27(H27)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C00O(H00A,H00B,
 H00C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F), C12A(H12D,
 H12E,H12F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 46 electrons were 
found in a volume of 588\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C7H8] per Asymmetric Unit 
which account for 50 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22322
_shelx_fab_checksum              90653
_olex2_submission_special_instructions 'No special instructions were received'