Homogeneous perdehydrogenation and perhydrogenation of fused bicyclic N-heterocycles catalyzed by iridium complexes bearing a functional bipyridonate ligand.
Fujita, Ken-Ichi; Tanaka, Yui; Kobayashi, Masato; Yamaguchi, Ryohei; Journal of the American Chemical Society 136 (2014) 4829–4832; doi:10.1021/ja5001888

data_4121606
_publ_section_title
;
 Homogeneous perdehydrogenation and perhydrogenation of fused bicyclic
 N-heterocycles catalyzed by iridium complexes bearing a functional
 bipyridonate ligand.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4829
_journal_page_last               4832
_journal_paper_doi               10.1021/ja5001888
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C26 H32 Ir N3 O4 '
_chemical_formula_sum            'C26 H32 Ir N3 O4'
_chemical_formula_weight         642.78
_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                89.7280(13)
_cell_angle_beta                 77.932(2)
_cell_angle_gamma                66.2153(18)
_cell_formula_units_Z            2
_cell_length_a                   9.0891(6)
_cell_length_b                   9.5888(4)
_cell_length_c                   15.5410(7)
_cell_measurement_reflns_used    13632
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     1207.22(11)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      173.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11387
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    5.583
_exptl_absorpt_correction_T_max  0.433
_exptl_absorpt_correction_T_min  0.226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.79
_refine_diff_density_min         -1.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4983
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0006Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0324
_reflns_number_gt                4976
_reflns_number_total             5440
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja5001888_si_003.cif
_cod_data_source_block           '_compound2a'
_cod_original_cell_volume        1207.23(11)
_cod_original_formula_sum        'C26 H32 Ir N3 O4 '
_cod_database_code               4121606