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_4085108
_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            'C18 H22 I Ir O S'
_chemical_formula_weight         605.51
_chemical_name_common            DF5-55h
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6278(3)
_cell_length_b                   13.2227(4)
_cell_length_c                   16.0076(5)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      35.1912
_cell_measurement_theta_min      2.6818
_cell_volume                     1826.19(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32798
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    9.115
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.5301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.240
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.716
_refine_ls_abs_structure_details
;
Flack x determined using 3086 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0006(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         7300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0155
_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^)+(0.0115P)^2^+1.1906P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0328
_refine_ls_wR_factor_ref         0.0330
_reflns_number_gt                7155
_reflns_number_total             7300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501115u_si_002.cif
_cod_data_source_block           III
_cod_depositor_comments
'Adding full bibliography for 4085106--4085109.cif.'
_cod_database_code               4085108
_shelx_res_checksum              50172