C‒H Bond Activation by Cationic Iridium(III) NHC Complexes: A Combined Experimental and Computational Study
Meredith, Joseph M.; Robinson, Robert; Goldberg, Karen I.; Kaminsky, Werner; Heinekey, D. Michael; Organometallics 31 (2012) 1879–; doi:10.1021/om2012166

data_4076449
_publ_section_title
;
 C--H Bond Activation by Cationic Iridium(III) NHC Complexes: A Combined
 Experimental and Computational Study
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1879
_journal_paper_doi               10.1021/om2012166
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C30 H46 Cl2 Ir2 N4, 2(C19 H3 B F15)'
_chemical_formula_sum            'C68 H52 B2 Cl2 F30 Ir2 N4'
_chemical_formula_weight         1972.06
_chemical_name_common            JMM02053
_chemical_name_systematic        JMM02053
_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                64.004(2)
_cell_angle_beta                 68.406(2)
_cell_angle_gamma                72.1790(17)
_cell_formula_units_Z            1
_cell_length_a                   12.1212(4)
_cell_length_b                   12.4125(7)
_cell_length_c                   13.5343(7)
_cell_measurement_reflns_used    419
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1676.10(14)
_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, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.950
_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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11439
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    4.177
_exptl_absorpt_correction_T_max  0.2668
_exptl_absorpt_correction_T_min  0.1919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.43
_refine_diff_density_max         1.735
_refine_diff_density_min         -2.201
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                6870
_reflns_number_total             7942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2012166_si_003.cif
_cod_data_source_block           IMe_Cl_bimetallic_6b
_cod_database_code               4076449