Synthesis and Photocatalytic Properties of a New Heteropolyoxoniobate Compound: K10[Nb2O2(H2O)2][SiNb12O40].12H2O
Zhenyu Zhang; Qipu Lin; Dharmalingam Kurunthu; Tao Wu; Fan Zuo; Shou-Tian Zheng; Christopher J. Bardeen; Xianhui Bu; Pingyun Feng; Journal of the American Chemical Society 133 (2011) 6934–6937; doi:10.1021/ja201670x

data_4106123
_publ_section_title
;
 Synthesis and Photocatalytic Properties of a New Heteropolyoxoniobate
 Compound: K10[Nb2O2(H2O)2][SiNb12O40].12H2O
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6934
_journal_page_last               6937
_journal_paper_doi               10.1021/ja201670x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'Nb28 O96 Si2, 24(O), 8(K0.13), 19(K)'
_chemical_formula_sum            'K20 Nb28 O120 Si2'
_chemical_formula_weight         5359.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.5765(4)
_cell_length_b                   16.5765(4)
_cell_length_c                   19.2519(10)
_cell_measurement_reflns_used    6006
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.83
_cell_measurement_theta_min      2.74
_cell_volume                     5290.0(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19720
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.855
_exptl_absorpt_correction_T_max  0.592
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.365
_exptl_crystal_description       octahydron
_exptl_crystal_F_000             5032.0
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.503
_refine_diff_density_min         -2.379
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2461
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+239.7755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2025
_reflns_number_gt                2161
_reflns_number_total             2461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201670x_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        5290.0(2)
_cod_database_code               4106123