Synthesis and Structural Characterization of Inorganic-Organic-Inorganic Hybrids of Dipalladium-Substituted γ-Keggin Silicodecatungstates
Tomohisa Hirano; Kazuhiro Uehara; Sayaka Uchida; Mitsuhiro Hibino; Keigo Kamata; Noritaka Mizuno; Inorganic Chemistry 52 (2013) 2662–2670; doi:10.1021/ic302703k

data_4334046
_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
;
 Synthesis and Structural Characterization of Inorganic-Organic-Inorganic
 Hybrids of Dipalladium-Substituted \g-Keggin Silicodecatungstates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2662
_journal_page_last               2670
_journal_paper_doi               10.1021/ic302703k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C134 N8 O80 Pd4 Si2 W20'
_chemical_formula_sum            'C134 N8 O80 Pd4 Si2 W20'
_chemical_formula_weight         7160.2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             2013-01-23T12:16:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.6080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.0069(2)
_cell_length_b                   24.7919(3)
_cell_length_c                   27.3714(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    183
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     11528.7(3)
_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      183
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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: 44.9925
              2theta: -20.0751
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: 90.0000
                 XTD: 44.9925
              2theta: -20.0751

;
_diffrn_measurement_device       'Rigaku MicroMax-007'
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtfind.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       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            32066
_diffrn_reflns_theta_full        29.63
_diffrn_reflns_theta_max         29.63
_diffrn_reflns_theta_min         1.11
_diffrn_source_current           30.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           40.0000
_exptl_absorpt_coefficient_mu    10.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_description       block
_exptl_crystal_F_000             6384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         3.739
_refine_diff_density_min         -4.007
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         32066
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+183.6591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2427
_reflns_number_gt                20906
_reflns_number_total             32066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302703k_si_003_2.cif
_cod_data_source_block           II
_cod_database_code               4334046