CO<sub>2</sub> hydrosilylation catalyzed by an N-heterocyclic carbene (NHC)-stabilized stannyliumylidene.
Niu, Dechuang; Kostenko, Arseni; Kelly, John A.; Sarkar, Debotra; Xu, Huihui; Inoue, Shigeyoshi; Chemical science 16 (2025) 4014–4022; doi:10.1039/d4sc07116f

data_1573733
_publ_section_title
;
 CO<sub>2</sub> hydrosilylation catalyzed by an N-heterocyclic carbene
 (NHC)-stabilized stannyliumylidene.
;
_journal_issue                   9
_journal_name_full               'Chemical science'
_journal_page_first              4014
_journal_page_last               4022
_journal_paper_doi               10.1039/d4sc07116f
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C38 H49 N4 Sn, C32 H12 B F22.8, 1.2(F)'
_chemical_formula_sum            'C70.01 H61 B F24 N4 Sn'
_chemical_formula_weight         1543.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2025-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                102.535(3)
_cell_angle_beta                 101.839(3)
_cell_angle_gamma                109.969(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4232(4)
_cell_length_b                   17.0569(6)
_cell_length_c                   18.5469(7)
_cell_measurement_reflns_used    8008
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.6920
_cell_measurement_theta_min      2.5250
_cell_volume                     3711.1(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.921
_diffrn_reflns_theta_min         2.562
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         14585
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.7637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11675
_reflns_number_total             14585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07116f2.cif
_cod_data_source_block           cu-3470
_cod_depositor_comments
'Adding full bibliography for 1573732--1573734.cif.'
_cod_original_cell_volume        3711.1(2)
_cod_database_code               1573733
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.712
_olex2_refinement_description
;
1. Restrained distances
 F25-F27 \\sim F25-F26 \\sim F27-F26
 with sigma of 0.04
 C46-C41 \\sim C46-F25 \\sim C46-F27 \\sim C46-F26
 with sigma of 0.02
2. Others
 Fixed Sof: F30(0.5) F28(0.5) F29(0.5) F17(0.5) F16(0.5) F18(0.5) F25(0.6)
 F27(0.6) F26(0.6) F6(0.4) F5(0.4) F4(0.4)
3.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C48(H48), C68(H68), C60(H60), C52(H52), C64(H64), C56(H56),
 C40(H40), C50(H50), C58(H58), C66(H66), C42(H42), C5(H5), C18(H18), C4(H4),
 C20(H20), C11(H11), C3(H3), C9(H9)
3.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C22(H22A,H22B,
 H22C), C31(H31A,H31B,H31C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C35(H35A,
 H35B,H35C), C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C36(H36A,H36B,H36C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58309
_shelx_fab_checksum              88527
_olex2_submission_special_instructions 'No special instructions were received'