Extended Utility of Molten-Salt Chemistry: Unprecedented Synthesis of a Water-Soluble Salt-Inclusion Solid Comprised of High-Nuclearity Vanadium Oxide Clusters
Wendy L. Queen; J. Palmer West; Joan Hudson; Shiou-Jyh Hwu; Inorganic Chemistry 50 (2011) 11064–11068; doi:10.1021/ic201605w

data_4326710
_publ_contact_author_address
;Department of Chemistry
Clemson University
Clemson, SC  29634-0973 
USA
;
_publ_contact_author_email       shwu@clemson.edu
_publ_contact_author_name        'Shiou-Jyh Hwu'
_publ_contact_author_phone       864-656-5031
_publ_section_title
;
 Extended Utility of Molten-Salt Chemistry: Unprecedented Synthesis of a
 Water-Soluble Salt-Inclusion Solid Comprised of High-Nuclearity Vanadium
 Oxide Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11064
_journal_page_last               11068
_journal_paper_doi               10.1021/ic201605w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'Cl6 Cs11 Na3 O36 V15'
_chemical_formula_weight         3083.78
_space_group_IT_number           187
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6 2'
_symmetry_space_group_name_H-M   'P -6 m 2'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   11.819(4)
_cell_length_b                   11.819(4)
_cell_length_c                   11.476(2)
_cell_measurement_reflns_used    1005
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3732
_cell_measurement_theta_min      2.6801
_cell_volume                     1388.3(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
 Number of images: 360
            Slice: -90.0000 - 90.0000
      Image width: 0.5000
         Exp time: 60.0000
    Rotation axis: Omega
            Omega: 0.0000
              Chi: 45.0000
              Phi: 0.0000
              XTD: 27.1383
           2theta: 0.0091
scan:
 Number of images: 120
            Slice: -30.0000 - 30.0000
      Image width: 0.5000
         Exp time: 60.0000
    Rotation axis: Omega
            Omega: 0.0000
              Chi: 45.0000
              Phi: 90.0000
              XTD: 27.1383
           2theta: 0.000
;
_diffrn_measurement_device_type  'Rigaku AFC8S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11873
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.895
_exptl_absorpt_correction_T_max  0.8267
_exptl_absorpt_correction_T_min  0.4378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.689
_exptl_crystal_description       cube
_exptl_crystal_F_000             1373
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+7.1276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                973
_reflns_number_total             1005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201605w_si_002.cif
_cod_data_source_block           cd6577-1
_cod_database_code               4326710