Palladium(IV) Monohydrocarbyls: Mechanistic Study of the Ligand-Enabled Oxidation of Palladium(II) Complexes with H2O2in Water
Oloo, Williamson N.; Zavalij, Peter Y.; Vedernikov, Andrei N.; Organometallics 32 (2013) 5601–; doi:10.1021/om400878u

data_4081698
_publ_section_title
;
 Palladium(IV) Monohydrocarbyls: Mechanistic Study of the Ligand-Enabled
 Oxidation of Palladium(II) Complexes with H2O2in Water
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5601
_journal_paper_doi               10.1021/om400878u
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C33 H22 F2 N4 O4 Pd2, 2(C H Cl3)'
_chemical_formula_sum            'C35 H24 Cl6 F2 N4 O4 Pd2'
_chemical_formula_weight         1028.08
_chemical_name_common            Pd2-complex
_chemical_name_systematic
;
Pd2-complex
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 111.8383(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.1268(14)
_cell_length_b                   9.2511(6)
_cell_length_c                   20.5534(14)
_cell_measurement_reflns_used    6112
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.4
_cell_volume                     3728.8(4)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      610,610,610,96
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0049416
_diffrn_orient_matrix_UB_12      0.1049261
_diffrn_orient_matrix_UB_13      -0.0088156
_diffrn_orient_matrix_UB_21      0.0469386
_diffrn_orient_matrix_UB_22      -0.0003328
_diffrn_orient_matrix_UB_23      0.0369599
_diffrn_orient_matrix_UB_31      0.0193048
_diffrn_orient_matrix_UB_32      -0.0259871
_diffrn_orient_matrix_UB_33      -0.0361060
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14714
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_id                'VEdern/Oloo Pd-complex 150K'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3281
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.036P)^2^+26.7P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                2823
_reflns_number_total             3281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400878u_si_002.cif
_cod_data_source_block           2165
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4081698
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 1926
_diffrn_measurement_frame_time-ccd 30
_diffrn_measurement_total_time-ccd 18.7
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_size-ccd 512