Double Geminal C-H Activation and Reversible α-Elimination in 2-Aminopyridine Iridium(III) Complexes: The Role of Hydrides and Solvent in Flattening the Free Energy Surface
Eric Clot; Junyi Chen; Dong-Heon Lee; So Young Sung; Leah N. Appelhans; Jack W. Faller; Robert H. Crabtree; Odile Eisenstein; Journal of the American Chemical Society 126 (2004) 8795–8804; doi:10.1021/ja048473j

data_4112760
_publ_contact_author_address
;
     Department of Chemistry, Yale University, New Haven, CT 06520-8107 USA
;
_publ_contact_author_email       ' Jack.faller@yale.edu '
_publ_contact_author_fax         ' (203)-432-6144 '
_publ_contact_author_name        ' J. W. Faller'
_publ_contact_author_phone       ' (203)-432-3954 '
_publ_section_title
;
 Double Geminal C-H Activation and Reversible \a-Elimination in
 2-Aminopyridine Iridium(III) Complexes: The Role of Hydrides and Solvent
 in Flattening the Free Energy Surface
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8795
_journal_page_last               8804
_journal_paper_doi               10.1021/ja048473j
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C47 H46 B Cl4 F4 Ir N2 P2'
_chemical_formula_weight         1121.68
_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'
_audit_creation_date             2003-12-03
_audit_creation_method           'by teXsan for Windows v1.06'
_cell_angle_alpha                90
_cell_angle_beta                 110
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.8735(11)
_cell_length_b                   10.8667(3)
_cell_length_c                   18.3822(4)
_cell_measurement_reflns_used    23039
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     9361.6(4)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo-SMN
_computing_publication_material  'teXsan for Windows v. 1.06 (MSC 1999)'
_computing_structure_refinement  'teXsan for Windows v. 1.06 (MSC 1999)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      183.2
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
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_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_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  0.05780
_diffrn_reflns_av_sigmaI/netI    0.106
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28041
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.219
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       plate
_exptl_crystal_F_000             4464.00
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.70
_refine_diff_density_min         -1.77
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.260
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     550
_refine_ls_number_reflns         5981
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0600
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                5981
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_reflns_threshold_expression     I>5.00\s(I)
_cod_data_source_file            ja048473jsi20040317_052009.cif
_cod_data_source_block           '_2111Ir(PPh3)2H2(PyCC3H6N)'
_cod_original_cell_volume        9331.3(3)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C47 H46 B Cl4 F4 Ir N2 P2 '
_cod_database_code               4112760