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_4085109
_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_moiety         'C35 H41 Ir2 O2 S2, C F3 O3 S'
_chemical_formula_sum            'C36 H41 F3 Ir2 O5 S3'
_chemical_formula_weight         1091.27
_chemical_name_common            6-8
_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
_cell_angle_alpha                91.642(2)
_cell_angle_beta                 106.9960(10)
_cell_angle_gamma                100.0630(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4451(3)
_cell_length_b                   11.2528(3)
_cell_length_c                   16.5796(5)
_cell_measurement_reflns_used    9162
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      36.4420
_cell_measurement_theta_min      2.3384
_cell_volume                     1828.34(9)
_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-2014 (Sheldrick, 2014)'
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            141954
_diffrn_reflns_theta_full        36.49
_diffrn_reflns_theta_max         36.49
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.499
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.15
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.753
_refine_diff_density_min         -0.858
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         17908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0165
_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^)+(0.0172P)^2^+0.8160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0359
_refine_ls_wR_factor_ref         0.0371
_reflns_number_gt                15677
_reflns_number_total             17908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501115u_si_002.cif
_cod_data_source_block           IV
_cod_depositor_comments
'Adding full bibliography for 4085106--4085109.cif.'
_cod_database_code               4085109
_shelx_res_checksum              10874
_shelx_hkl_checksum              37456