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_4114257
_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            'C39 H59 F3 Ir2 O3 P2 S'
_chemical_formula_weight         1111.34
_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'
_cell_angle_alpha                112.75(3)
_cell_angle_beta                 97.02(3)
_cell_angle_gamma                98.27(2)
_cell_formula_units_Z            2
_cell_length_a                   13.702(3)
_cell_length_b                   14.763(4)
_cell_length_c                   11.466(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    203.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     2076.1(13)
_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      203.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06818
_diffrn_orient_matrix_UB_12      0.01726
_diffrn_orient_matrix_UB_13      -0.01805
_diffrn_orient_matrix_UB_21      0.00697
_diffrn_orient_matrix_UB_22      -0.07129
_diffrn_orient_matrix_UB_23      -0.02551
_diffrn_orient_matrix_UB_31      -0.03093
_diffrn_orient_matrix_UB_32      -0.01616
_diffrn_orient_matrix_UB_33      -0.09122
_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  0.01820
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9991
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        -0.51
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.597
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1088.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.26
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.302
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6752
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0330
_refine_ls_wR_factor_ref         0.0330
_reflns_number_gt                6752
_reflns_number_total             9515
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja036929bsi20030701_035827_2.cif
_cod_data_source_block           '_complex3'
_cod_original_cell_volume        2076(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C39 H59 F3 Ir2 O3 P2 S '
_cod_database_code               4114257