Niobium uptake by {P2W12} polyoxoanion with [NbO(C2O4)2(H2O)2]− as Nb source
Shmakova, Alexandra A.; Sukhikh, Taisiya S.; Volchek, Victoria V.; Yanshole, Vadim; Stass, Dmitri V.; Filatov, Eugeniy Yu.; Glebov, Eugeniy M.; Abramov, Pavel A.; Sokolov, Maxim N.; Inorganica Chimica Acta 502 (2020) 119319–; doi:10.1016/j.ica.2019.119319

data_1565367
_publ_section_title
;
 Niobium uptake by {P2W12} polyoxoanion with [NbO(C2O4)2(H2O)2]&#x2212; as
 Nb source
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119319
_journal_paper_doi               10.1016/j.ica.2019.119319
_journal_volume                  502
_journal_year                    2020
_chemical_formula_sum            'C16 N8 Nb6.4 O144.78 P4 W29.6'
_chemical_formula_weight         8781.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.5879(12)
_cell_length_b                   21.9143(13)
_cell_length_c                   18.3017(11)
_cell_measurement_reflns_used    9115
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6900
_cell_measurement_theta_min      2.2777
_cell_volume                     7856.1(8)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            100308
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.729
_diffrn_reflns_theta_min         1.523
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    22.167
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.712
_exptl_crystal_description       block
_exptl_crystal_F_000             7646
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.424
_refine_diff_density_min         -1.786
_refine_diff_density_rms         0.344
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         10476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+223.4652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8737
_reflns_number_total             10476
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2020-502-119319.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C16 N8 Nb6.40 O144.78 P4 W29.60'
_cod_database_code               1565367
_shelx_estimated_absorpt_t_min   0.117
_shelx_estimated_absorpt_t_max   0.176