Two organic‒inorganic hybrid polyoxovanadates as reusable catalysts for Knoevenagel condensation
Li, Chunxia; Zhong, Dandan; Huang, Xianqiang; Shen, Guodong; Li, Qiang; Du, Jiyuan; Li, Qianli; Wang, Suna; Li, Jikun; Dou, Jianmin; New Journal of Chemistry 43 (2019) 5813–; doi:10.1039/C8NJ06460A

data_7058233
_publ_section_title
;
 Two organic--inorganic hybrid polyoxovanadates as reusable catalysts for
 Knoevenagel condensation
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5813
_journal_paper_doi               10.1039/C8NJ06460A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C16 H57 N8 Ni3 O45.5 V10'
_chemical_formula_weight         1775.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-11 deposited with the CCDC.    2019-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.430(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.5903(17)
_cell_length_b                   9.3317(8)
_cell_length_c                   15.8463(12)
_cell_measurement_reflns_used    1670
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.569
_cell_measurement_theta_min      2.448
_cell_volume                     2714.7(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6800
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         2.219
_exptl_absorpt_coefficient_mu    2.768
_exptl_absorpt_correction_T_max  0.6361
_exptl_absorpt_correction_T_min  0.5815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_description       block
_exptl_crystal_F_000             1774
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1801
_reflns_number_total             2546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj06460a2.cif
_cod_data_source_block           180602b
_cod_depositor_comments
'Adding full bibliography for 7058232--7058233.cif.'
_cod_original_formula_sum        'C16 H57 N8 Ni3 O45.50 V10'
_cod_database_code               7058233
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.581
_shelx_estimated_absorpt_t_max   0.636
_shelx_res_checksum              96986