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_4086673
_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_moiety         'C19 H26 Ir N O2 S'
_chemical_formula_sum            'C19 H26 Ir N O2 S'
_chemical_formula_weight         524.67
_chemical_name_common            CMP-1035-B
_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   mixed
_cell_angle_alpha                83.1780(10)
_cell_angle_beta                 83.2700(10)
_cell_angle_gamma                74.4480(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7906(2)
_cell_length_b                   9.2091(2)
_cell_length_c                   11.8914(3)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      36.3909
_cell_measurement_theta_min      2.3052
_cell_volume                     917.17(4)
_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)'
_diffrn_ambient_temperature      100.(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  0.0259
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47975
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.404
_exptl_absorpt_correction_T_max  0.42
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.653
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         8042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0142
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+0.2664P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0306
_refine_ls_wR_factor_ref         0.0309
_reflns_number_gt                7659
_reflns_number_total             8042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00308_si_003.cif
_cod_data_source_block           rds378
_cod_database_code               4086673
_shelx_res_checksum              94955
_shelx_hkl_checksum              19841