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_4349214
_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            'H0 K5.5 Na2 Nb24 O93 V4'
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_cell_angle_alpha                75.336(4)
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_cell_length_c                   26.4350(10)
_cell_measurement_reflns_used    10479
_cell_measurement_temperature    130(2)
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_cell_measurement_theta_min      3.6600
_cell_volume                     5775.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
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_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
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_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
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_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
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_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_theta_max         31.067
_diffrn_reflns_theta_min         3.374
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_exptl_absorpt_correction_T_max  1.00000
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_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    2.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             3893
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.104
_refine_diff_density_min         -3.916
_refine_diff_density_rms         0.513
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         32023
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1729
_refine_ls_R_factor_gt           0.1350
_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^)+(0.1567P)^2^+377.1802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3489
_refine_ls_wR_factor_ref         0.3656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21562
_reflns_number_total             32023
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b02108_si_003.cif
_cod_data_source_block           1_sq
_cod_original_formula_sum        'H0 K5.50 Na2 Nb24 O93 V4'
_cod_database_code               4349214
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.569
_shelx_estimated_absorpt_t_max   0.869
_shelx_res_checksum              96684
_shelx_hkl_checksum              24720
_shelx_fab_checksum              31342