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_7063696
_publ_section_title
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 Bis(N-heterocyclic carbene)s incorporating silicon in the ligand backbone
;
_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), C22 H38 N4 Si, H2 O'
_chemical_formula_sum            'C22 H40 I2 N4 O Si'
_chemical_formula_weight         658.47
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-27
_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                 100.478(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.276(2)
_cell_length_b                   15.400(3)
_cell_length_c                   15.149(2)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.338
_cell_measurement_theta_min      2.372
_cell_volume                     2816.2(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0630
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31390
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         1.687
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.295
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0845 before and 0.0747 after correction.
The Ratio of minimum to maximum transmission is 0.8366.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6470
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0690P)^2^+7.7011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5022
_reflns_number_total             6470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04276j2.cif
_cod_data_source_block           mo_bp_230624_cysisalt_0m
_cod_depositor_comments
'Adding full bibliography for 7063694--7063696.cif.'
_cod_original_cell_volume        2816.1(8)
_cod_database_code               7063696
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.496
_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. Restrained distances
 O1-H1A = O1-H1B
 0.84 with sigma of 0.01
 H1A-H1B
 1.33 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C11(H11), C17(H17)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              33095
_shelx_hkl_checksum              12105
_olex2_submission_special_instructions 'No special instructions were received'