ortho-C‒H Activation of Thiobenzoic Acid: Synthesis, Characterization, and Reactivity of Iridium Thiobenzoate Complexes
Frasco, Daniel A.; Sommer, Roger D.; Ison, Elon A.; Organometallics 34 (2015) 275–; doi:10.1021/om501115u

data_4085106
_publ_section_title
;
 ortho-C--H Activation of Thiobenzoic Acid: Synthesis, Characterization,
 and Reactivity of Iridium Thiobenzoate Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              275
_journal_paper_doi               10.1021/om501115u
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C34 H38 Ir2 O2 S2'
_chemical_formula_weight         927.16
_chemical_name_common            C20H26IrO3S
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                66.309(2)
_cell_angle_beta                 77.213(2)
_cell_angle_gamma                72.572(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7597(3)
_cell_length_b                   9.5564(3)
_cell_length_c                   10.3206(4)
_cell_measurement_reflns_used    9706
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      34.5693
_cell_measurement_theta_min      2.1695
_cell_volume                     749.76(5)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_data_collection       'Bruker Instrument Service v2009, 11, 0, 0'
_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      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13645
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.035
_exptl_absorpt_correction_T_max  0.29
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         5.328
_refine_diff_density_min         -4.542
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4338
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                4064
_reflns_number_total             4338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501115u_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4085106--4085109.cif.'
_cod_database_code               4085106