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_4104566
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       wernerka@u.washington.edu
_publ_contact_author_name        'Werner Kaminsky'
_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         'C27 H44 Ir N O2 P2'
_chemical_formula_sum            'C27 H44 Ir N O2 P2'
_chemical_formula_weight         668.79
_chemical_name_common            EJK-I-18
_chemical_name_systematic        EJK-I-18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.182(6)
_cell_angle_beta                 98.874(6)
_cell_angle_gamma                110.226(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3103(4)
_cell_length_b                   10.6257(8)
_cell_length_c                   17.3126(14)
_cell_measurement_reflns_used    6626
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1410.41(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0777
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10830
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.84
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    4.870
_exptl_absorpt_correction_T_max  0.6143
_exptl_absorpt_correction_T_min  0.3403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       Prism
_exptl_crystal_F_000             672.0
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         5.869
_refine_diff_density_min         -4.484
_refine_diff_density_rms         0.332
_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     310
_refine_ls_number_reflns         6922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                5281
_reflns_number_total             6922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901706b_si_003.cif
_cod_data_source_block           shelxl
_cod_database_code               4104566