Diverse Reactions of PhI(OTf)2 with Common 2-Electron Ligands: Complex Formation, Oxidation, and Oxidative Coupling
Thomas P. Pell; Shannon A. Couchman; Sara Ibrahim; David J. D. Wilson; Brian J. Smith; Peter J. Barnard; Jason L. Dutton; Inorganic Chemistry 51 (2012) 13034–13040; doi:10.1021/ic302176f

data_4331228
_publ_section_title
;
 Diverse Reactions of PhI(OTf)2 with Common 2-Electron Ligands: Complex
 Formation, Oxidation, and Oxidative Coupling
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13034
_journal_page_last               13040
_journal_paper_doi               10.1021/ic302176f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C22 H25 F6 I N4 O6 S2'
_chemical_formula_weight         746.48
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.866(4)
_cell_length_b                   9.752(2)
_cell_length_c                   13.102(3)
_cell_measurement_reflns_used    6500
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.1361
_cell_measurement_theta_min      2.7599
_cell_volume                     2793.8(10)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    SHELXP
_computing_publication_material  SHELXP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27604
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.8518
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.031
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.355
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.355
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+28.6932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                2338
_reflns_number_total             2713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302176f_si_002_2.cif
_cod_data_source_block           8_NMe2
_cod_database_code               4331228