Mechanism of the Iridium-Catalyzed Silylation of Aromatic C-H Bonds.
Karmel, Caleb; Hartwig, John F.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c03301

data_4135011
_publ_section_title
;
 Mechanism of the Iridium-Catalyzed Silylation of Aromatic C-H Bonds.
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03301
_journal_year                    2020
_chemical_formula_sum            'C46 H70 Ir N2 O7 P Si6'
_chemical_formula_weight         1154.75
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                76.7080(10)
_cell_angle_beta                 75.7050(10)
_cell_angle_gamma                81.4550(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1998(2)
_cell_length_b                   12.3637(2)
_cell_length_c                   19.2246(2)
_cell_measurement_reflns_used    38907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1940
_cell_measurement_theta_min      3.0260
_cell_volume                     2721.69(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65730
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.861
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    2.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
PROBLEM: NonSolvent Resd 1  C   Ueq(max) / Ueq(min) Range        6.4 Ratio
RESPONSE: Due to the unresolved minor disorder of atoms C3 and C4, among others
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.463
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         13464
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11943
_reflns_number_total             13464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03301_si_002.cif
_cod_data_source_block           Complex_3
_cod_database_code               4135011
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.691
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              7175
_shelx_hkl_checksum              8054