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_4349747
_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 H132 Cu6 N24 Nb12 O60 Si V2'
_chemical_formula_weight         3343.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_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                 96.757(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8976(5)
_cell_length_b                   20.6011(8)
_cell_length_c                   16.2057(6)
_cell_measurement_reflns_used    6942
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7580
_cell_measurement_theta_min      3.9180
_cell_volume                     4939.1(3)
_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 0.978
_diffrn_measured_fraction_theta_max 0.843
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12063
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.038
_diffrn_reflns_theta_min         3.057
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83979
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    2.248
_exptl_crystal_description       block
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.809
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5712
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+87.8145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5001
_reflns_number_total             5712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00318h2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               4349747
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.596
_shelx_estimated_absorpt_t_max   0.688
_shelx_res_checksum              51769
_shelx_hkl_checksum              25156