Reactivity of Pd(II) Complexes with Electrophilic Chlorinating Reagents: Isolation of Pd(IV) Products and Observation of C-Cl Bond-Forming Reductive Elimination
Salena R. Whitfield; Melanie S. Sanford; Journal of the American Chemical Society 129 (2007) 15142–15143; doi:10.1021/ja077866q

data_4110286
_publ_section_title
;
 Reactivity of Pd(II) Complexes with Electrophilic Chlorinating Reagents:
 Isolation of Pd(IV) Products and Observation of C-Cl Bond-Forming
 Reductive Elimination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15142
_journal_page_last               15143
_journal_paper_doi               10.1021/ja077866q
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C26 H20 Cl N3 O2 Pd, 3(C H Cl3)'
_chemical_formula_sum            'C29 H23 Cl10 N3 O2 Pd'
_chemical_formula_weight         906.40
_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                73.298(7)
_cell_angle_beta                 87.149(7)
_cell_angle_gamma                75.923(8)
_cell_formula_units_Z            2
_cell_length_a                   9.264(5)
_cell_length_b                   12.458(7)
_cell_length_c                   16.136(9)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      23.19
_cell_measurement_theta_min      2.48
_cell_volume                     1729.7(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-1K'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53162
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.7750
_exptl_absorpt_correction_T_min  0.7049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
  detector absorption and other corrections, University of
  Gottingen, Germany 2003.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.079
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.128
_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     406
_refine_ls_number_reflns         8613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0665P)^2^+5.0280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                7034
_reflns_number_total             8613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077866q-file002.cif
_cod_data_source_block           sw642
_cod_database_code               4110286