C-H Bond Activation at Palladium(IV) Centers
Joy M. Racowski; Nicholas D. Ball; Melanie S. Sanford; Journal of the American Chemical Society 133 (2011) 18022–18025; doi:10.1021/ja2051099

data_4107075
_publ_section_title
;
 C-H Bond Activation at Palladium(IV) Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18022
_journal_page_last               18025
_journal_paper_doi               10.1021/ja2051099
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C33 H32 F6 N2 O2 Pd'
_chemical_formula_sum            'C33 H32 F6 N2 O2 Pd'
_chemical_formula_weight         709.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 112.163(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9697(5)
_cell_length_b                   13.7277(4)
_cell_length_c                   16.5604(12)
_cell_measurement_reflns_used    9368
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      6.62
_cell_volume                     3151.7(3)
_computing_cell_refinement       FS-PROCESS
_computing_data_collection       'Crystal Clear 2.0'
_computing_data_reduction        FS-PROCESS
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      95(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17539
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         6.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.347
_exptl_absorpt_correction_T_max  0.9289
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       chip
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.501
_refine_diff_density_min         -3.167
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1166P)^2^+28.1030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2483
_reflns_number_gt                4104
_reflns_number_total             5430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2051099_si_001.cif
_cod_data_source_block           shelxl
_cod_database_code               4107075