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_4079747
_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         'C25 H28 N, B F4, 0.625(C4 H10 O)'
_chemical_formula_sum            'C27.5 H34.25 B F4 N O0.63'
_chemical_formula_weight         475.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.064(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   14.6348(17)
_cell_length_b                   25.776(3)
_cell_length_c                   13.8000(16)
_cell_measurement_reflns_used    14399
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.12
_cell_volume                     5205.7(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42804
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2018.32
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.750
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     679
_refine_ls_number_reflns         11778
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 4.4200\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                9549
_reflns_number_total             11778
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om301063n_si_002.cif
_cod_data_source_block           4f.HBF4.0.625Et2O
_cod_original_cell_volume        5205.8(11)
_cod_original_formula_sum        'C27.50 H34.25 B F4 N O0.63'
_cod_database_code               4079747