Investigations of Iridium-Mediated Reversible C-H Bond Cleavage: Characterization of a 16-Electron Iridium(III) Methyl Hydride Complex
Wesley H. Bernskoetter; Susan Kloek Hanson; Sara K. Buzak; Zoe Davis; Peter S. White; Rodney Swartz; Karen I. Goldberg; Maurice Brookhart; Journal of the American Chemical Society 131 (2009) 8603–8613; doi:10.1021/ja901706b

data_4104565
_publ_section_title
;
 Investigations of Iridium-Mediated Reversible C-H Bond Cleavage:
 Characterization of a 16-Electron Iridium(III) Methyl Hydride Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8603
_journal_page_last               8613
_journal_paper_doi               10.1021/ja901706b
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C22 H43 Ir N O2 P2, C32 H12 B F24, C H2 Cl2'
_chemical_formula_sum            'C55 H57 B Cl2 F24 Ir N O2 P2'
_chemical_formula_weight         1555.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.337(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7439(2)
_cell_length_b                   23.6882(3)
_cell_length_c                   19.7743(3)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.41
_cell_volume                     6352.59(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            85397
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.347
_exptl_absorpt_correction_T_max  0.6733
_exptl_absorpt_correction_T_min  0.4956
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker-AXS APEX2 Numerical'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.290
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         13868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+20.7423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                11957
_reflns_number_total             13868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901706b_si_002.cif
_cod_data_source_block           c08401
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4104565