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_4121604
_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         'C10 H21 N2 O0.50 '
_chemical_formula_sum            'C10 H21 N2 O0.5'
_chemical_formula_weight         177.29
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 113.194(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   22.675(3)
_cell_length_b                   6.1256(9)
_cell_length_c                   16.5599(18)
_cell_measurement_reflns_used    7397
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.5
_cell_volume                     2114.2(5)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.087
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8937
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             792.00
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    refU
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1311
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0020Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                1293
_reflns_number_total             2388
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja5001888_si_001.cif
_cod_data_source_block           '_compound3a'
_cod_original_cell_volume        2114.3(5)
_cod_original_formula_sum        'C10 H21 N2 O0.50 '
_cod_database_code               4121604