Hemilabile N-Xylyl-N'-methylperimidine Carbene Iridium Complexes as Catalysts for C-H Activation and Dehydrogenative Silylation: Dual Role of N-Xylyl Moiety for ortho-C-H Bond Activation and Reductive Bond Cleavage
Gyeongshin Choi; Hayato Tsurugi; Kazushi Mashima; Journal of the American Chemical Society 135 (2013) 13149–13161; doi:10.1021/ja406519u

data_4120724
_publ_section_title
;
 Hemilabile N-Xylyl-N'-methylperimidine Carbene Iridium Complexes as
 Catalysts for C-H Activation and Dehydrogenative Silylation: Dual Role of
 N-Xylyl Moiety for ortho-C-H Bond Activation and Reductive Bond Cleavage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13149
_journal_page_last               13161
_journal_paper_doi               10.1021/ja406519u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C32 H36 Ir N2 O2'
_chemical_formula_sum            'C32 H36 Ir N2 O2'
_chemical_formula_weight         672.85
_chemical_name_common            1g
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.999(13)
_cell_angle_beta                 89.465(18)
_cell_angle_gamma                87.969(13)
_cell_formula_units_Z            4
_cell_length_a                   11.950(2)
_cell_length_b                   12.2366(10)
_cell_length_c                   18.754(2)
_cell_measurement_reflns_used    5694
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     2699.0(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21611
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    4.979
_exptl_absorpt_correction_T_max  0.225
_exptl_absorpt_correction_T_min  0.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         12.900
_refine_diff_density_min         -4.136
_refine_diff_density_rms         0.409
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1702P)^2^+11.4192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2445
_reflns_number_gt                7429
_reflns_number_total             10053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406519u_si_001_04.cif
_cod_data_source_block           1g
_cod_original_cell_volume        2699.1(6)
_cod_database_code               4120724