Sandwich-Type Zinc-Containing Polyoxometalates with a Hexaprismane Core [{Zn2W(O)O3}2]4+ Synthesized by Thermally Induced Isomerization of a Metastable Polyoxometalate
Yuji Kikukawa; Kazuya Yamaguchi; Noritaka Mizuno; Inorganic Chemistry 49 (2010) 8194–8196; doi:10.1021/ic101419a

data_4316561
_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
;
 Sandwich-Type Zinc-Containing Polyoxometalates with a Hexaprismane Core
 [{Zn2W(O)O3}2]4+ Synthesized by Thermally Induced Isomerization of a
 Metastable Polyoxometalate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8194
_journal_page_last               8196
_journal_paper_doi               10.1021/ic101419a
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C128 N8 O74 Si2 W20 Zn4'
_chemical_formula_sum            'C128 N8 O74 Si2 W20 Zn4'
_chemical_formula_weight         6828.02
_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'
_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             2010-08-11T13:31:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 119.0360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.7252(4)
_cell_length_b                   26.3949(5)
_cell_length_c                   27.7763(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     22259.1(7)
_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      153
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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: 45.4809
              2theta: -20.7688
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: 45.4809
              2theta: -20.7688

;
_diffrn_measurement_device       'Rigaku MicroMax-007'
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       Saturn70
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            30608
_diffrn_reflns_theta_full        29.44
_diffrn_reflns_theta_max         29.44
_diffrn_reflns_theta_min         1.02
_diffrn_source_current           100.0000
_diffrn_source_power             5.000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    10.784
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12176
_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         3.095
_refine_diff_density_min         -3.757
_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     707
_refine_ls_number_reflns         30608
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_gt           0.0777
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2444
_reflns_number_gt                15815
_reflns_number_total             30608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101419a_si_003.cif
_cod_data_source_block           squeeze
_cod_database_code               4316561