Inter- and Intramolecular Activation of Aromatic C-H Bonds by Diphosphine and Hydrido-Bridged Dinuclear Iridium Complexes
Ken-ichi Fujita; Hirohide Nakaguma; Taro Hamada; Ryohei Yamaguchi; Journal of the American Chemical Society 125 (2003) 12368–12369; doi:10.1021/ja036929b

data_4114256
_publ_contact_author_name        ' Ken-ichi Fujita'
_publ_section_title
;
 Inter- and Intramolecular Activation of Aromatic C-H Bonds by Diphosphine
 and Hydrido-Bridged Dinuclear Iridium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12368
_journal_page_last               12369
_journal_paper_doi               10.1021/ja036929b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C46 H53 F3 Ir2 O3 P2 S'
_chemical_formula_weight         1189.37
_space_group_IT_number           4
_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'
_cell_angle_alpha                90
_cell_angle_beta                 107.89(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.459(8)
_cell_length_b                   13.782(9)
_cell_length_c                   14.696(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291.2
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      10.2
_cell_volume                     2209(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows version 1.06'
_computing_publication_material  'teXsan for Windows version 1.06'
_computing_structure_refinement  'teXsan for Windows version 1.06'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      291.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.06814
_diffrn_orient_matrix_UB_12      -0.00984
_diffrn_orient_matrix_UB_13      -0.06091
_diffrn_orient_matrix_UB_21      -0.04472
_diffrn_orient_matrix_UB_22      -0.04069
_diffrn_orient_matrix_UB_23      0.03482
_diffrn_orient_matrix_UB_31      -0.04201
_diffrn_orient_matrix_UB_32      0.05927
_diffrn_orient_matrix_UB_33      0.01379
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.04210
_diffrn_reflns_av_sigmaI/netI    0.064
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5532
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        -1.11
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.207
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1160.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.47
_refine_diff_density_min         -2.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.206
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     493
_refine_ls_number_reflns         4293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0440
_refine_ls_wR_factor_ref         0.0440
_reflns_number_gt                4293
_reflns_number_total             5278
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ja036929bsi20030701_035827_1.cif
_cod_data_source_block           '_complex6'
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C46 H53 F3 Ir2 O3 P2 S '
_cod_database_code               4114256