Bis(N-heterocyclic carbene)s incorporating silicon in the ligand backbone
Puerta Lombardi, Braulio M.; McCallum, Katia A.; Harrison, Alexander; Louwe, Devon S.; Espejo, Jayar; Bouzidi, Karima; Roesler, Roland; New Journal of Chemistry 49 (2025) 6554–6560; doi:10.1039/D4NJ04276J

data_7063694
_publ_section_title
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 Bis(N-heterocyclic carbene)s incorporating silicon in the ligand backbone
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_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6554
_journal_page_last               6560
_journal_paper_doi               10.1039/D4NJ04276J
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         '2(I), C24 H44 N4 O Si2'
_chemical_formula_sum            'C24 H44 I2 N4 O Si2'
_chemical_formula_weight         714.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2025-03-10 deposited with the CCDC.	2025-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.535(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.128(5)
_cell_length_b                   21.250(6)
_cell_length_c                   12.140(3)
_cell_measurement_reflns_used    5308
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.01
_cell_volume                     3203.3(15)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection
'APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.'
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11303
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.690
_diffrn_reflns_theta_min         1.900
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.060
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0832 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.7924.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.7596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2993
_reflns_number_total             3669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04276j2.cif
_cod_data_source_block           mo_bp_230817_cysiosisalt_0m
_cod_depositor_comments
'Adding full bibliography for 7063694--7063696.cif.'
_cod_database_code               7063694
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.570
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C5(H5A,H5B), C9(H9A,H9B), C6(H6A,H6B), C8(H8A,H8B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              36144
_shelx_hkl_checksum              33993
_olex2_submission_special_instructions 'No special instructions were received'