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_4086672
_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_absolute_configuration ad
_chemical_formula_moiety         'C19 H27 Ir O2 S'
_chemical_formula_sum            'C19 H27 Ir O2 S'
_chemical_formula_weight         511.70
_chemical_name_common            CMP-1035-A
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1162(2)
_cell_length_b                   13.3585(3)
_cell_length_c                   15.0708(4)
_cell_measurement_reflns_used    275
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.6773
_cell_measurement_theta_min      2.6149
_cell_volume                     1835.30(8)
_computing_cell_refinement       'APEX3 v2015.5-2 (Bruker AXS)'
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59442
_diffrn_reflns_theta_full        36.38
_diffrn_reflns_theta_max         36.38
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.395
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.098
_refine_diff_density_max         3.434
_refine_diff_density_min         -0.894
_refine_ls_abs_structure_details
;

Flack x determined using 3541 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         8925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

w=1/[\s^2^(Fo^2^)+(0.0210P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0494
_reflns_number_gt                8360
_reflns_number_total             8925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00308_si_003.cif
_cod_data_source_block           rds379
_cod_database_code               4086672
_shelx_res_checksum              64821
_shelx_hkl_checksum              9892