Mechanism of Hydrogenolysis of an Iridium-Methyl Bond: Evidence for a Methane Complex Intermediate
Jesús Campos; Sabuj Kundu; Dale R. Pahls; Maurice Brookhart; Ernesto Carmona; Thomas R. Cundari; Journal of the American Chemical Society 135 (2013) 1217–1220; doi:10.1021/ja310982v

data_4119221
_publ_contact_author
;
        Jesus Campos
        Instituto de Investigaciones Qu\'imicas
        CSIC-Universidad de Sevilla
        Am\'erico Vespucio, 49
        Isla de la Cartuja 
        41092 SEVILLA
        Spain
;
_publ_contact_author_email       jesus.campos@ctq.csic.es
_publ_contact_author_fax         '34 954460565'
_publ_contact_author_phone       '34 954489554'
_publ_section_title
;
 Mechanism of Hydrogenolysis of an Iridium-Methyl Bond: Evidence for a
 Methane Complex Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1217
_journal_page_last               1220
_journal_paper_doi               10.1021/ja310982v
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C32 H12 B F24, C23 H43 Ir N O3 P2'
_chemical_formula_sum            'C55 H55 B F24 Ir N O3 P2'
_chemical_formula_weight         1498.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.9060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5555(3)
_cell_length_b                   18.3798(4)
_cell_length_c                   21.3098(4)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.21
_cell_volume                     6096.9(2)
_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      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            105503
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    2.358
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 x-ray Solutions, Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       needle
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         13980
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+11.9603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                11360
_reflns_number_total             13980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310982v_si_002.cif
_cod_data_source_block           jc00412a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4119221