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_1565366
_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            'C14 H42 K0.5 N6.8 Nb6 O138.4 P4 W30'
_chemical_formula_weight         8736.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                100.927(3)
_cell_angle_beta                 96.488(2)
_cell_angle_gamma                105.419(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5004(3)
_cell_length_b                   23.0057(8)
_cell_length_c                   27.1162(8)
_cell_measurement_reflns_used    11293
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.0100
_cell_measurement_theta_min      3.4360
_cell_volume                     7851.9(4)
_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    '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      130(2)
_diffrn_detector_area_resol_mean 10.6168
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.1101
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.818
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            61436
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.608
_diffrn_reflns_theta_min         3.302
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    22.450
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.695
_exptl_crystal_description       prism
_exptl_crystal_F_000             7633
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         5.379
_refine_diff_density_min         -4.866
_refine_diff_density_rms         0.567
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1523
_refine_ls_number_reflns         36137
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0789
_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^)+(0.0927P)^2^+3.7011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20019
_reflns_number_total             36137
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2020-502-119319.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C14 H42 K0.50 N6.80 Nb6 O138.40 P4 W30'
_cod_database_code               1565366
_shelx_estimated_absorpt_t_min   0.212
_shelx_estimated_absorpt_t_max   0.400