Crystal structure and electrochemistry properties of one two-dimensional heteropolyoxoniobate based on four- and five-vanadium-capped Keggin anions
Guo, Hui-Li; Wang, Yi-Kun; Qu, Xiao-Jie; Feng, Rui; Pang, Jing-Yu; Bai, Yan; Dang, Dong-Bin; New Journal of Chemistry 46 (2022) 1494–1497; doi:10.1039/D1NJ04891K

data_7061188
_publ_section_title
;
 Crystal structure and electrochemistry properties of one two-dimensional
 heteropolyoxoniobate based on four- and five-vanadium-capped Keggin
 anions
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1494
_journal_page_last               1497
_journal_paper_doi               10.1039/D1NJ04891K
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C96 H425 Cu16 K2 N64 Nb48 O233 V21'
_chemical_formula_weight         12830.23
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-01-08 deposited with the CCDC.	2022-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.3773(17)
_cell_length_b                   26.3773(17)
_cell_length_c                   27.4429(17)
_cell_measurement_reflns_used    7325
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.86
_cell_volume                     19094(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24395
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.484
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_description       stick
_exptl_crystal_F_000             12532
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.4631
_refine_diff_density_max         1.550
_refine_diff_density_min         -1.864
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       0.000016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4452
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0886P)^2^+393.6107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2987
_reflns_number_total             4452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04891k2.cif
_cod_data_source_block           ddb
_cod_depositor_comments          'Adding full bibliography for 7061188.cif.'
_cod_original_cell_volume        19094(3)
_cod_database_code               7061188
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.367
_shelx_estimated_absorpt_t_max   0.628
_shelx_res_checksum              40298