A Palladium-Oxo Complex. Stabilization of This Proposed Catalytic Intermediate by an Encapsulating Polytungstate Ligand [J. Am. Chem.Soc.2005,127, 11948-11949].
Travis M. Anderson; Rui Cao; Elena Slonkina; Britt Hedman; Keith O. Hodgson; Kenneth I. Hardcastle; Wade A. Neiwert; Shaoxiong Wu; Martin L. Kirk; Sushilla Knottenbelt; Ezra C. Depperman; Bineta Keita; Louis Nadjo; Djamaladdin G. Musaev; Keiji Morokuma; Craig L. Hill; Journal of the American Chemical Society 130 (2008) 2877–2877; doi:10.1021/ja711078v

data_4107495
_publ_section_title
;
 A Palladium-Oxo Complex. Stabilization of This Proposed Catalytic
 Intermediate by an Encapsulating Polytungstate Ligand [J. Am.
 Chem.Soc.2005,127, 11948-11949].
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2877
_journal_page_last               2877
_journal_paper_doi               10.1021/ja711078v
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'H18.80 K9.80 Na3 O80.30 P2 Pd W19'
_chemical_formula_sum            'H18.8 K9.8 Na3 O80.3 P2 Pd W19'
_chemical_formula_weight         5417.39
_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                90.536(2)
_cell_angle_beta                 103.247(2)
_cell_angle_gamma                108.671(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8734(15)
_cell_length_b                   17.225(2)
_cell_length_c                   22.814(3)
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.36
_cell_volume                     4285.4(9)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            82689
_diffrn_reflns_theta_full        26.68
_diffrn_reflns_theta_max         26.68
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    26.222
_exptl_absorpt_correction_T_max  0.1605
_exptl_absorpt_correction_T_min  0.0209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, sHELDRICK 2007'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.198
_exptl_crystal_description       prism
_exptl_crystal_F_000             4725
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         5.637
_refine_diff_density_min         -4.351
_refine_diff_density_rms         0.445
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1050
_refine_ls_number_reflns         17969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1439
_reflns_number_gt                15946
_reflns_number_total             17969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711078v-file001.cif
_cod_data_source_block           pdinnerfs
_cod_original_cell_volume        4285.3(9)
_cod_original_formula_sum        'H18.80 K9.80 Na3 O80.30 P2 Pd W19'
_cod_database_code               4107495