Palladium(II) Containing γ-Keggin Silicodecatungstate That Efficiently Catalyzes Hydration of Nitriles
Tomohisa Hirano; Kazuhiro Uehara; Keigo Kamata; Noritaka Mizuno; Journal of the American Chemical Society 134 (2012) 6425–6433; doi:10.1021/ja3006012

data_4117783
_publ_contact_author_address
;
Department of Applied Chemistry, School of Engineering
The University of Tokyo
7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan)
;
_publ_contact_author_email       tmizuno@mail.ecc.u-tokyo.ac.jp
_publ_contact_author_fax         (+)81-3-5841-7220
_publ_contact_author_name        'Noritaka Mizuno'
_publ_contact_author_phone       (+)81-3-5841-7272
_publ_section_title
;
 Palladium(II) Containing \g-Keggin Silicodecatungstate That Efficiently
 Catalyzes Hydration of Nitriles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6425
_journal_page_last               6433
_journal_paper_doi               10.1021/ja3006012
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C673 N32 O320 Pd16 Si8 W80'
_chemical_formula_sum            'C168.25 B0 N8 O80 Pd4 Si2 W20'
_chemical_formula_weight         7571.54
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-04-21T14:04:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 89.94
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2918(2)
_cell_length_b                   45.0388(4)
_cell_length_c                   29.4768(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     26939.4(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      193
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0827
              2theta: -19.9067

;
_diffrn_measurement_device       'Rigaku MicroMax-007'
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       Saturn724
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            64820
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.82
_diffrn_source_current           30.0000
_diffrn_source_power             1.20000
_diffrn_source_voltage           40.0000
_exptl_absorpt_coefficient_mu    8.831
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       block
_exptl_crystal_F_000             13590
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         4.368
_refine_diff_density_min         -1.785
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1822
_refine_ls_number_reflns         64820
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_gt           0.0924
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+484.0238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2303
_reflns_number_gt                36825
_reflns_number_total             64820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3006012_si_002.cif
_cod_data_source_block           squeezed
_cod_database_code               4117783