Cation-Dependent Self-assembly of Vanadium Polyoxoniobates.
Abramov, Pavel A.; Davletgildeeva, Anastasiia T.; Moroz, Nikolay K.; Kompankov, Nikolay B.; Santiago-Schübel, Beatrix; Sokolov, Maxim N.; Inorganic chemistry 55 (2016) 12807–12814; doi:10.1021/acs.inorgchem.6b02108

data_4349213
_publ_section_title
;
 Cation-Dependent Self-assembly of Vanadium Polyoxoniobates.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12807
_journal_page_last               12814
_journal_paper_doi               10.1021/acs.inorgchem.6b02108
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C2 H78 Na9 Nb14 O85 V'
_chemical_formula_weight         3021.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.466(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.784(3)
_cell_length_b                   14.1842(17)
_cell_length_c                   47.521(6)
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.52
_cell_volume                     15983(3)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
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_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            63787
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.702
_diffrn_reflns_theta_min         0.860
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_description       plate
_exptl_crystal_F_000             11728
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         18678
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+357.3163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13030
_reflns_number_total             18678
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b02108_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        15983(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4349213
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              57273
_shelx_hkl_checksum              62426