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_4081697
_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         'C23 H20 N3 O4 Pd, C2 F3 O2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C27 H25 F3 N3 O6.5 Pd'
_chemical_formula_weight         658.90
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.746(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.5322(10)
_cell_length_b                   40.711(5)
_cell_length_c                   17.656(2)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.3
_cell_volume                     5376.6(11)
_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      100(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0224955
_diffrn_orient_matrix_UB_12      0.0155712
_diffrn_orient_matrix_UB_13      0.0438846
_diffrn_orient_matrix_UB_21      -0.0597188
_diffrn_orient_matrix_UB_22      -0.0155540
_diffrn_orient_matrix_UB_23      0.0327732
_diffrn_orient_matrix_UB_31      0.1174597
_diffrn_orient_matrix_UB_32      -0.0109010
_diffrn_orient_matrix_UB_33      0.0158836
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49181
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2664.2
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     485
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0387
_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^)+(0.024P)^2^+9.95P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                7442
_reflns_number_total             9430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400878u_si_002.cif
_cod_data_source_block           2032
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C54 H50 F6 N6 O13 Pd2'
_cod_original_formula_weight         1317.80
_cod_original_formula_moiety       '2(C23 H20 N3 O4 Pd), 2(C2 F3 O2), C4 H10 O'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5376.5(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4081697