Catalytic Intramolecular Hydroamination with a Bifunctional Iridium Pyrazolato Complex: Substrate Scope and Mechanistic Elucidation
Kashiwame, Yohei; Kuwata, Shigeki; Ikariya, Takao; Organometallics 31 (2012) 8444–; doi:10.1021/om301063n

data_4079751
_publ_section_title
;
 Catalytic Intramolecular Hydroamination with a Bifunctional Iridium
 Pyrazolato Complex: Substrate Scope and Mechanistic Elucidation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8444
_journal_paper_doi               10.1021/om301063n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C32 H34 Ir N3 O2 S '
_chemical_formula_sum            'C32 H34 Ir N3 O2 S'
_chemical_formula_weight         716.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.959(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   22.6347(19)
_cell_length_b                   10.1885(5)
_cell_length_c                   26.0061(16)
_cell_measurement_reflns_used    16890
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5637.1(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      93.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43699
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    4.859
_exptl_absorpt_correction_T_max  0.233
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2848.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.71
_refine_diff_density_min         -1.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     771
_refine_ls_number_reflns         12840
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0001Fo^2^ + 0.6200\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                8972
_reflns_number_total             12840
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om301063n_si_002.cif
_cod_data_source_block           '__[Cp*Ir(NHTs)(C6H4PzHPh)](10)'
_cod_original_cell_volume        5637.1(6)
_cod_original_formula_sum        'C32 H34 Ir N3 O2 S '
_cod_database_code               4079751