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_7063695
_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), C16 H30 N4 Si'
_chemical_formula_sum            'C16 H30 I2 N4 Si'
_chemical_formula_weight         560.33
_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             2024-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_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                 102.171(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0436(15)
_cell_length_b                   22.182(4)
_cell_length_c                   11.772(2)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.502
_cell_measurement_theta_min      2.480
_cell_volume                     2308.4(7)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.1335
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.610
_diffrn_reflns_theta_min         1.836
_exptl_absorpt_coefficient_mu    2.781
_exptl_absorpt_correction_T_max  0.6347
_exptl_absorpt_correction_T_min  0.3570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1786 before and 0.1391 after correction.
The Ratio of minimum to maximum transmission is 0.5625.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.034
_refine_diff_density_min         -2.763
_refine_diff_density_rms         0.361
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         5340
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4460
_reflns_number_total             5340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04276j2.cif
_cod_data_source_block           mo_230420_km1_0m
_cod_depositor_comments
'Adding full bibliography for 7063694--7063696.cif.'
_cod_database_code               7063695
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
I1 \\sim I2 \\sim I3 \\sim I4 \\sim I5: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(I1) \\sim Ueq, Uanis(I2) \\sim Ueq, Uanis(I3) \\sim Ueq, Uanis(I4) \\sim
Ueq, Uanis(I5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Others
 Sof(I3)=1-FVAR(1)
 Sof(I1)=FVAR(1)
 Sof(I4)=Sof(I5)=0.5*(1-FVAR(3))
 Sof(I2)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C5(H5), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C11(H11), C12(H12), C13(H13)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,
 H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              27181
_shelx_hkl_checksum              69479
_olex2_submission_special_instructions 'No special instructions were received'