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_4117859
_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         'C29 H38 Ir N P, C F3 O3 S'
_chemical_formula_sum            'C30 H38 F3 Ir N O3 P S'
_chemical_formula_weight         772.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.9240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.5889(19)
_cell_length_b                   8.4679(5)
_cell_length_c                   22.0407(14)
_cell_measurement_reflns_used    6565
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.49
_cell_volume                     6038.0(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            69766
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.595
_exptl_absorpt_correction_T_max  0.7100
_exptl_absorpt_correction_T_min  0.5268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       needle
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.627
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         9191
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+34.1078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                7399
_reflns_number_total             9191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301759m_si_001.cif
_cod_data_source_block           1-NCMe+
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4117859