#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/67/4326710.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4326710
loop_
_publ_author_name
'Wendy L. Queen'
'J. Palmer West'
'Joan Hudson'
'Shiou-Jyh Hwu'
_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       'ω 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/[σ²(Fo²)+(0.0721P)²+7.1276P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+y, -x, -z'
'-y, x-y, z'
'x, y, -z'
'-x+y, -x, z'
'-y, x-y, -z'
'-y, -x, -z'
'-x+y, y, z'
'x, x-y, -z'
'-y, -x, z'
'-x+y, y, -z'
'x, x-y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cs1 Cs 0.29074(14) 0.14537(7) 0.5000 0.0363(4) Uani 1 4 d S
Cs2 Cs 0.47286(5) -0.05428(10) 0.79875(9) 0.0396(3) Uani 1 2 d S
Cs3 Cs 0.6667 0.3333 1.0000 0.0729(12) Uani 1 12 d S
Cl1 Cl 0.0000 0.0000 1.0000 0.038(2) Uani 1 12 d S
V1 V 0.3041(2) 0.15203(11) 0.85362(17) 0.0213(4) Uani 1 2 d S
Cs4 Cs 0.6667 0.3333 0.6053(3) 0.0401(8) Uani 0.50 6 d SP
V2 V 0.6811(3) -0.15945(14) 1.0000 0.0183(6) Uani 1 4 d S
V3 V 0.10196(9) -0.10196(9) 0.75901(17) 0.0184(4) Uani 1 2 d S
Cl3 Cl 0.3333 -0.3333 0.6559(5) 0.0286(12) Uani 1 6 d S
O1 O 0.1495(4) 0.2989(8) 0.6436(8) 0.0234(19) Uani 1 2 d S
Cl4 Cl 0.5036(3) -0.5036(3) 0.5000 0.0415(13) Uani 1 4 d S
Na1 Na 0.2312(4) 0.4624(7) 0.5000 0.0347(18) Uani 1 4 d S
O2 O 0.3741(13) 0.1871(6) 1.0000 0.026(3) Uani 1 4 d S
O3 O 0.4328(11) 0.2164(6) 0.7725(11) 0.038(2) Uani 1 2 d S
O4 O 0.2406(6) -0.0291(5) 0.8742(5) 0.0215(12) Uani 1 1 d .
O5 O -0.0800(5) -0.1601(9) 0.7372(8) 0.0255(18) Uani 1 2 d S
O6 O 0.5230(12) -0.2385(6) 1.0000 0.035(3) Uani 1 4 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 V1 O2 102.1(6) . .
O3 V1 O4 110.6(2) . .
O2 V1 O4 91.1(2) . .
O3 V1 O4 110.6(2) . 12
O2 V1 O4 91.1(2) . 12
O4 V1 O4 137.3(4) . 12
O3 V1 O5 102.6(5) . 3
O2 V1 O5 155.3(5) . 3
O4 V1 O5 80.2(2) . 3
O4 V1 O5 80.2(2) 12 3
O3 V1 V3 111.1(3) . .
O2 V1 V3 127.8(3) . .
O4 V1 V3 40.20(19) . .
O4 V1 V3 112.1(2) 12 .
O5 V1 V3 40.03(10) 3 .
O3 V1 V3 111.1(3) . 3
O2 V1 V3 127.8(3) . 3
O4 V1 V3 112.1(2) . 3
O4 V1 V3 40.20(19) 12 3
O5 V1 V3 40.03(10) 3 3
V3 V1 V3 75.46(9) . 3
O6 V2 O4 104.8(2) . 5_655
O6 V2 O4 104.8(2) . 2_657
O4 V2 O4 93.9(3) 5_655 2_657
O6 V2 O4 104.8(2) . 11_657
O4 V2 O4 150.5(4) 5_655 11_657
O4 V2 O4 78.5(3) 2_657 11_657
O6 V2 O4 104.8(2) . 8_655
O4 V2 O4 78.5(3) 5_655 8_655
O4 V2 O4 150.5(4) 2_657 8_655
O4 V2 O4 93.9(3) 11_657 8_655
O6 V2 V3 113.05(6) . 2_657
O4 V2 V3 124.9(2) 5_655 2_657
O4 V2 V3 39.43(17) 2_657 2_657
O4 V2 V3 39.43(17) 11_657 2_657
O4 V2 V3 124.9(2) 8_655 2_657
O6 V2 V3 113.05(6) . 5_655
O4 V2 V3 39.43(17) 5_655 5_655
O4 V2 V3 124.9(2) 2_657 5_655
O4 V2 V3 124.9(2) 11_657 5_655
O4 V2 V3 39.43(17) 8_655 5_655
V3 V2 V3 133.90(12) 2_657 5_655
O1 V3 O5 106.6(3) 5 .
O1 V3 O5 106.6(3) 5 3
O5 V3 O5 95.4(5) . 3
O1 V3 O4 110.1(3) 5 .
O5 V3 O4 142.6(3) . .
O5 V3 O4 80.9(3) 3 .
O1 V3 O4 110.1(3) 5 10
O5 V3 O4 80.9(3) . 10
O5 V3 O4 142.6(3) 3 10
O4 V3 O4 80.2(3) . 10
O1 V3 V1 113.75(6) 5 .
O5 V3 V1 127.1(3) . .
O5 V3 V1 41.8(3) 3 .
O4 V3 V1 39.12(17) . .
O4 V3 V1 113.57(19) 10 .
O1 V3 V1 113.75(6) 5 5
O5 V3 V1 41.8(3) . 5
O5 V3 V1 127.1(3) 3 5
O4 V3 V1 113.57(19) . 5
O4 V3 V1 39.12(17) 10 5
V1 V3 V1 131.70(10) . 5
O1 V3 V2 120.7(3) 5 3_545
O5 V3 V2 112.2(3) . 3_545
O5 V3 V2 112.2(3) 3 3_545
O4 V3 V2 40.27(17) . 3_545
O4 V3 V2 40.27(17) 10 3_545
V1 V3 V2 74.47(5) . 3_545
V1 V3 V2 74.47(5) 5 3_545
V1 O2 V1 133.8(8) . 4_557
V1 O4 V3 100.7(3) . .
V1 O4 V2 137.3(3) . 3_545
V3 O4 V2 100.3(2) . 3_545
V3 O5 V3 140.7(5) . 5
V3 O5 V1 98.2(3) . 5
V3 O5 V1 98.2(3) 5 5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O3 1.614(11) .
V1 O2 1.826(6) .
V1 O4 1.896(6) .
V1 O4 1.896(6) 12
V1 O5 1.989(10) 3
V1 V3 2.954(2) .
V1 V3 2.954(2) 3
Cs4 Cs4 2.416(8) 2_666
V2 O6 1.618(13) .
V2 O4 1.975(6) 5_655
V2 O4 1.975(6) 2_657
V2 O4 1.975(6) 11_657
V2 O4 1.975(6) 8_655
V2 V3 3.006(2) 2_657
V2 V3 3.006(2) 5_655
V3 O1 1.643(9) 5
V3 O5 1.919(3) .
V3 O5 1.919(3) 3
V3 O4 1.940(6) .
V3 O4 1.940(6) 10
V3 V1 2.954(2) 5
V3 V2 3.006(2) 3_545
O1 V3 1.643(9) 3
O2 V1 1.826(6) 4_557
O4 V2 1.975(6) 3_545
O5 V3 1.919(3) 5
O5 V1 1.989(9) 5
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139136323
