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_4107076
_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 H36 Cl F3 N2 Pd, 2(C6 H5 Cl)'
_chemical_formula_sum            'C45 H46 Cl3 F3 N2 Pd'
_chemical_formula_weight         884.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.885(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8630(3)
_cell_length_b                   13.6599(3)
_cell_length_c                   20.9345(15)
_cell_measurement_reflns_used    27467
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      2.20
_cell_volume                     4126.1(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_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_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn744+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-source rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69987
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    5.801
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7499
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+12.3489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                7171
_reflns_number_total             7499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2051099_si_002.cif
_cod_data_source_block           jmr1143
_cod_database_code               4107076