Oxyfunctionalization with Cp*Ir(III)(NHC)(Me)(Cl) with O2: Identification of a Rare Bimetallic Ir(IV) μ-Oxo Intermediate.
Lehman, Matthew C.; Pahls, Dale R.; Meredith, Joseph M.; Sommer, Roger D.; Heinekey, D. Michael; Cundari, Thomas R.; Ison, Elon A.; Journal of the American Chemical Society 137 (2015) 3574–3584; doi:10.1021/ja512905t

data_4123494
_publ_section_title
;
 Oxyfunctionalization with Cp*Ir(III)(NHC)(Me)(Cl) with O2: Identification
 of a Rare Bimetallic Ir(IV) \m-Oxo Intermediate.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3574
_journal_page_last               3584
_journal_paper_doi               10.1021/ja512905t
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'2(C32 H12 B F24), (C30 H46 Cl2 Ir2 N4), 2(C H2 Cl2)'
_chemical_formula_sum            'C96 H74 B2 Cl6 F48 Ir2 N4'
_chemical_formula_weight         2814.31
_chemical_name_common            1612
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                99.4710(10)
_cell_angle_beta                 92.0140(10)
_cell_angle_gamma                99.0600(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2843(6)
_cell_length_b                   14.6396(7)
_cell_length_c                   14.7149(8)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      33.0915
_cell_measurement_theta_min      2.5791
_cell_volume                     2572.6(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'XT, XXXXX'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            87061
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_refine_diff_density_max         5.434
_refine_diff_density_min         -2.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         10530
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+23.9080P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                9523
_reflns_number_total             10530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja512905t_si_001.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4123494--4123495.cif.'
_cod_database_code               4123494
_shelx_res_checksum              33338
_shelx_hkl_checksum              13997