Synthesis and structural characterization of a gamma-Keggin-type dimeric silicotungstate with a bis(mu-hydroxo) dizirconium core [(gamma-SiW10O36)2Zr2(mu-OH)2]10-.
Yamaguchi, Syuhei; Kikukawa, Yuji; Tsuchida, Kazutaka; Nakagawa, Yoshinao; Uehara, Kazuhiro; Yamaguchi, Kazuya; Mizuno, Noritaka; Inorganic chemistry 46 (2007) 8502–8504; doi:10.1021/ic701488s

data_4339522
_publ_section_title
;
 Synthesis and structural characterization of a gamma-Keggin-type dimeric
 silicotungstate with a bis(mu-hydroxo) dizirconium core
 [(gamma-SiW10O36)2Zr2(mu-OH)2]10-.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8502
_journal_page_last               8504
_journal_paper_doi               10.1021/ic701488s
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C114 H261 Cl4 N7 O74 Si2 W20 Zr2 '
_chemical_formula_sum            'C114 H261 Cl4 N7 O74 Si2 W20 Zr2'
_chemical_formula_weight         6971.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 108.7466(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   29.4764(7)
_cell_length_b                   35.6269(8)
_cell_length_c                   19.0523(3)
_cell_measurement_temperature    153.1
_cell_volume                     18946.4(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            48940
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_exptl_absorpt_coefficient_mu    12.350
_exptl_absorpt_correction_T_max  0.5775
_exptl_absorpt_correction_T_min  0.1485
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             12968.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.06
_refine_diff_density_min         -4.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         48940
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                21331
_reflns_number_total             48940
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic701488s-file001.cif
_cod_data_source_block           '_Template_texray.inf'
_cod_original_formula_sum        'C114 H261 Cl4 N7 O74 Si2 W20 Zr2 '
_cod_database_code               4339522