Cationic Ir(III) Alkylidenes Are Key Intermediates in C-H Bond Activation and C-C Bond-Forming Reactions
Jesús Campos; Joaquín López-Serrano; Eleuterio Álvarez; Ernesto Carmona; Journal of the American Chemical Society 134 (2012) 7165–7175; doi:10.1021/ja301759m

data_4117862
_publ_section_title
;
 Cationic Ir(III) Alkylidenes Are Key Intermediates in C-H Bond Activation
 and C-C Bond-Forming Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7165
_journal_page_last               7175
_journal_paper_doi               10.1021/ja301759m
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C32 H12 B F24, C27 H33 Ir P'
_chemical_formula_sum            'C59 H45 B F24 Ir P'
_chemical_formula_weight         1443.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                87.003(4)
_cell_angle_beta                 74.514(3)
_cell_angle_gamma                88.167(3)
_cell_formula_units_Z            4
_cell_length_a                   17.2137(15)
_cell_length_b                   17.9944(16)
_cell_length_c                   19.2836(18)
_cell_measurement_reflns_used    7698
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.43
_cell_volume                     5747.4(9)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            168196
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.468
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
program SADABS, Bruker (2001). 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       needle
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1553
_refine_ls_number_reflns         20614
_refine_ls_number_restraints     432
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+1.5287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                16148
_reflns_number_total             20614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301759m_si_005.cif
_cod_data_source_block           4+
_cod_database_code               4117862