Iridium and rhodium complexes bearing a silyl-bipyridine pincer ligand: synthesis, structures and catalytic activity for C–H borylation of arenes
Komuro, Takashi; Mochizuki, Daiki; Hashimoto, Hisako; Tobita, Hiromi; Dalton Transactions  (2022) –; doi:10.1039/D2DT01227H

data_7710547
_publ_section_title
;
 Iridium and rhodium complexes bearing a silyl-bipyridine pincer ligand:
 synthesis, structures and catalytic activity for C--H borylation of
 arenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01227H
_journal_year                    2022
_chemical_formula_moiety         'C22 H37 Cl Ir N2 P Si'
_chemical_formula_sum            'C22 H37 Cl Ir N2 P Si'
_chemical_formula_weight         616.24
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-04-18 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.406(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8176(8)
_cell_length_b                   9.3483(4)
_cell_length_c                   18.1721(9)
_cell_measurement_reflns_used    40025
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     2518.4(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics
;
'ORTEP-3', 'Yadokari-XG (Wakita, Nemoto et al., 2009)'
;
_computing_publication_material
;
'Yadokari-XG (Wakita, Nemoto et al., 2009)'
;
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'DIRDIF-2008 (PATTY)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28834
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.392
_exptl_absorpt_coefficient_mu    5.529
_exptl_absorpt_correction_T_max  0.351852
_exptl_absorpt_correction_T_min  0.192021
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
HIGASHI, T. (1999). Shape - Program to obtain Crystal Shape using CCD camera.
Rigaku Corporation, Tokyo, Japan.
HIGASHI, T. (1999). Numabs - Numerical Absorption Correction, 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.220
_refine_diff_density_max         2.065
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0299P)^2^+2.4321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5526
_reflns_number_total             5774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01227h2.cif
_cod_data_source_block           complex-3
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7710547
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.339
_shelx_estimated_absorpt_t_max   0.376
_shelx_res_checksum              89773
_shelx_hkl_checksum              69306