Oxidation of a Cyclometalated Pd(II) Dimer with "CF3+": Formation and Reactivity of a Catalytically Competent Monomeric Pd(IV) Aquo Complex
Yingda Ye; Nicholas D. Ball; Jeff W. Kampf; Melanie S. Sanford; Journal of the American Chemical Society 132 (2010) 14682–14687; doi:10.1021/ja107780w

data_4103333
_publ_section_title
;
 Oxidation of a Cyclometalated Pd(II) Dimer with "CF3+": Formation and
 Reactivity of a Catalytically Competent Monomeric Pd(IV) Aquo Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14682
_journal_page_last               14687
_journal_paper_doi               10.1021/ja107780w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C18 H16 F3 N O5 Pd'
_chemical_formula_sum            'C18 H16 F3 N O5 Pd'
_chemical_formula_weight         489.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.684(2)
_cell_angle_beta                 80.014(2)
_cell_angle_gamma                89.799(2)
_cell_formula_units_Z            4
_cell_length_a                   10.1764(15)
_cell_length_b                   13.225(2)
_cell_length_c                   13.805(2)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.30
_cell_volume                     1829.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56032
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.8469
_exptl_absorpt_correction_T_min  0.7530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.041
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9142
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+4.9562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                8494
_reflns_number_total             9142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107780w_si_002.cif
_cod_data_source_block           yy259
_cod_database_code               4103333