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_7131442
_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         'C25 H33 Ir N2 O2'
_chemical_formula_sum            'C25 H33 Ir N2 O2'
_chemical_formula_weight         585.75
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 105.794(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9043(5)
_cell_length_b                   14.2370(8)
_cell_length_c                   9.2991(5)
_cell_measurement_reflns_used    3936
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.37
_cell_volume                     1134.35(11)
_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      101(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_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  0.0762
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            57318
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.577
_diffrn_reflns_theta_min         2.276
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.909
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.277
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Flack x determined using 3283 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         8278
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0069P)^2^+1.7402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     1
_reflns_number_gt                7368
_reflns_number_total             8278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06865f2.cif
_cod_data_source_block           ValNHCIrCOD
_cod_depositor_comments
'Adding full bibliography for 7131439--7131442.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7131442
_shelx_res_checksum              53712
_shelx_hkl_checksum              86373