New organic‒inorganic hybrid compounds based on [SiNb12V2O42]12− with high catalytic activity for styrene epoxidation
Zhang, Ting-Ting; Zhang, Xiao; Lü, Ying; Li, Guo-Dong; Xiao, Li-Na; Cui, Xiao-Bing; Xu, Ji-Qing; Inorganic Chemistry Frontiers 4 (2017) 1397–; doi:10.1039/C7QI00318H

data_4349745
_publ_section_title
;
 New organic--inorganic hybrid compounds based on [SiNb12V2O42]12&#x2212;
 with high catalytic activity for styrene epoxidation
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1397
_journal_paper_doi               10.1039/C7QI00318H
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C24 H112 Cu6 N24 Nb12 O50 Si V2'
_chemical_formula_weight         3163.50
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5357(4)
_cell_length_b                   14.5357(4)
_cell_length_c                   22.999(2)
_cell_measurement_reflns_used    3077
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.7130
_cell_measurement_theta_min      3.5910
_cell_volume                     4859.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14332
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.925
_diffrn_reflns_theta_min         3.004
_exptl_absorpt_coefficient_mu    2.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72413
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_description       block
_exptl_crystal_F_000             3100
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.565
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.242
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2982
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0994
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1058P)^2^+126.0086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2499
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2096
_reflns_number_total             2982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00318h2.cif
_cod_data_source_block           2
_cod_original_cell_volume        4859.3(5)
_cod_database_code               4349745
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              7766
_shelx_hkl_checksum              73097