Bis-N-heterocyclic Carbene Palladium(IV) Tetrachloride Complexes: Synthesis, Reactivity, and Mechanisms of Direct Chlorinations and Oxidations of Organic Substrates
A. Scott McCall; Hongwang Wang; John M. Desper; Stefan Kraft; Journal of the American Chemical Society 133 (2011) 1832–1848; doi:10.1021/ja107342b

data_4105614
_publ_contact_author_address     '7840 Sunset Lane, Indianapolis, IN 46260'
_publ_contact_author_email       skraft@ksu.edu
_publ_contact_author_fax         1-615-658-0046
_publ_contact_author_name        'Kraft, Stefan'
_publ_contact_author_phone       1-785-341-8173
_publ_section_title
;
 Bis-N-heterocyclic Carbene Palladium(IV) Tetrachloride Complexes:
 Synthesis, Reactivity, and Mechanisms of Direct Chlorinations and
 Oxidations of Organic Substrates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1832
_journal_page_last               1848
_journal_paper_doi               10.1021/ja107342b
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
;
(C9 H12 N4)2 (Pd Cl4)2 (C1 H2 Cl2)3
;
_chemical_formula_sum            'C21 H30 Cl14 N8 Pd2'
_chemical_formula_weight         1103.63
_chemical_name_systematic
'1,1'-Dimethyl-3,3'-Methylene-4-Diimidazolin-2,2'-Diylidene-Palladium(IV) Tetrachloride'
_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                 91.644(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6703(6)
_cell_length_b                   18.5451(11)
_cell_length_c                   13.1767(8)
_cell_measurement_reflns_used    6491
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.49
_cell_measurement_theta_min      2.69
_cell_volume                     1873.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.915
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19678
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_description       needle
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.758
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         5968
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0500P)^2^+3.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                4425
_reflns_number_total             5968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107342b_si_002.cif
_cod_data_source_block           sm0804m
_cod_database_code               4105614