Iridium(I) complexes with bidentate NHC ligands as catalysts for dehydrogenative directed C-H silylation.
Manguin, Romane; Galiana-Cameo, María; Kittikool, Tanakorn; Barthes, Cécile; Thongpaen, Jompol; Bancal, Etienne; Mallet-Ladeira, Sonia; Yotphan, Sirilata; Castarlenas, Ricardo; Mauduit, Marc; Sortais, Jean-Baptiste; Baslé, Olivier; Chemical communications (Cambridge, England) 59 (2023) 4193–4196; doi:10.1039/d2cc06865f

data_7131440
_publ_section_title
;
 Iridium(I) complexes with bidentate NHC ligands as catalysts for
 dehydrogenative directed C-H silylation.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4193
_journal_page_last               4196
_journal_paper_doi               10.1039/d2cc06865f
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H35 Ir N2 O2'
_chemical_formula_sum            'C26 H35 Ir N2 O2'
_chemical_formula_weight         599.78
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      20
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.3819(10)
_cell_length_b                   27.2526(18)
_cell_length_c                   26.1453(17)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.23
_cell_volume                     10247.5(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            101612
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.101
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_min         1.494
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.234
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.402
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Flack x determined using 3644 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         9138
_refine_ls_number_restraints     666
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+124.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8524
_reflns_number_total             9138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06865f2.cif
_cod_data_source_block           LeuNHClrCOD
_cod_depositor_comments
'Adding full bibliography for 7131439--7131442.cif.'
_cod_database_code               7131440
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              27629
_shelx_hkl_checksum              28147
_shelx_fab_checksum              99491