Nondirected C‒H Activation of Arenes with Cp*Ir(III) Acetate Complexes: An Experimental and Computational Study
Frasco, Daniel A.; Mukherjee, Sriparna; Sommer, Roger D.; Perry, Cody M.; Lambic, Nikola S.; Abboud, Khalil A.; Jakubikova, Elena; Ison, Elon A.; Organometallics 35 (2016) 2435–; doi:10.1021/acs.organomet.6b00308

data_4086674
_publ_section_title
;
 Nondirected C--H Activation of Arenes with Cp*Ir(III) Acetate Complexes:
 An Experimental and Computational Study
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              2435
_journal_paper_doi               10.1021/acs.organomet.6b00308
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C14 H24 Cl2 Ir N O'
_chemical_formula_weight         485.44
_chemical_name_common            DF5-23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 114.0590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4301(5)
_cell_length_b                   7.6155(3)
_cell_length_c                   14.5741(5)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      33.2372
_cell_measurement_theta_min      2.8022
_cell_volume                     1563.79(10)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32594
_diffrn_reflns_theta_full        33.25
_diffrn_reflns_theta_max         33.25
_diffrn_reflns_theta_min         2.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.872
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.999
_refine_diff_density_min         -0.894
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         6023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.6764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0424
_reflns_number_gt                5480
_reflns_number_total             6023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00308_si_003.cif
_cod_data_source_block           I
_cod_database_code               4086674