#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:22:58 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185228 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/52/7225238.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_7225238
loop_
_publ_author_name
'Guo, Hai-Yang'
'Zhang, Xiao'
'Cui, Xiao-Bing'
'Huo, Qi-Sheng'
'Xu, Ji-Qing'
_publ_section_title
;
 Vanadoantimonates: from discrete clusters to high dimensional aggregates
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              5130
_journal_paper_doi               10.1039/C6CE00616G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'H16 O48 Sb8 V14'
_chemical_formula_weight         2471.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-26 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.348(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6766(10)
_cell_length_b                   11.9042(5)
_cell_length_c                   19.2758(15)
_cell_measurement_reflns_used    4048
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      3.42
_cell_volume                     2961.0(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    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16739
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.187
_diffrn_reflns_theta_min         3.157
_exptl_absorpt_coefficient_mu    5.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83285
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.772
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.242
_refine_diff_density_min         -2.367
_refine_diff_density_rms         0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6841
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0676
_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/[σ²(Fo²)+(0.0879P)²+86.6103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.2071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4914
_reflns_number_total             6841
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce00616g2.cif
_cod_data_source_block           shelx_4
_cod_depositor_comments
'Adding full bibliography for 7225235--7225239.cif.'
_cod_database_code               7225238
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.392
_shelx_estimated_absorpt_t_max   0.545
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Sb4 Sb 0.71304(6) 0.04471(7) -0.22214(5) 0.0334(2) Uani 1 1 d . .
Sb3 Sb 1.10146(7) 0.38786(7) 0.03924(5) 0.0367(2) Uani 1 1 d . .
Sb2 Sb 0.95032(7) 0.09928(7) -0.25280(5) 0.0367(2) Uani 1 1 d . .
Sb1 Sb 0.85962(7) 0.33791(7) 0.06729(5) 0.0402(2) Uani 1 1 d . .
V7 V 0.88450(17) 0.26755(16) -0.11252(12) 0.0323(5) Uani 1 1 d . .
V6 V 1.08589(17) 0.17591(16) 0.17643(12) 0.0336(5) Uani 1 1 d . .
V5 V 0.73254(17) 0.13654(19) -0.05394(13) 0.0365(5) Uani 1 1 d . .
V4 V 0.75023(17) -0.16344(18) -0.09875(13) 0.0364(5) Uani 1 1 d . .
V3 V 0.88756(19) -0.22522(19) 0.09951(14) 0.0417(6) Uani 1 1 d . .
V2 V 0.86906(19) 0.0756(2) 0.14183(15) 0.0436(6) Uani 1 1 d . .
V1 V 0.7305(2) -0.0660(3) 0.0313(2) 0.0622(8) Uani 1 1 d . .
O21 O 0.7868(7) 0.1401(7) -0.1362(5) 0.0347(19) Uani 1 1 d . .
O20 O 0.7966(7) -0.0863(7) -0.1715(5) 0.037(2) Uani 1 1 d . .
O19 O 0.9396(7) 0.2127(7) 0.1231(5) 0.041(2) Uani 1 1 d . .
O18 O 0.8345(8) 0.2592(7) -0.0262(5) 0.041(2) Uani 1 1 d . .
O17 O 0.9697(7) 0.1931(7) -0.1638(5) 0.038(2) Uani 1 1 d . .
O16 O 1.0271(7) 0.3004(7) -0.0491(5) 0.038(2) Uani 1 1 d . .
O15 O 1.0152(7) 0.0411(7) 0.1935(5) 0.038(2) Uani 1 1 d . .
O14 O 1.1306(7) 0.2527(7) 0.1028(5) 0.039(2) Uani 1 1 d . .
O13 O 0.8348(7) 0.3787(7) -0.1569(5) 0.042(2) Uani 1 1 d . .
O12 O 0.9734(7) 0.4276(7) 0.0577(6) 0.044(2) Uani 1 1 d . .
O11 O 0.7074(7) -0.0221(7) -0.0719(5) 0.038(2) Uani 1 1 d . .
O10 O 0.8015(8) 0.0845(8) -0.2783(5) 0.042(2) Uani 1 1 d . .
O9 O 0.7859(8) -0.2026(8) 0.0030(6) 0.045(2) Uani 1 1 d . .
O8 O 0.8434(7) -0.0823(8) 0.1237(6) 0.042(2) Uani 1 1 d . .
O7 O 0.6464(8) -0.2285(8) -0.1411(6) 0.048(2) Uani 1 1 d . .
O6 O 1.1177(8) 0.2500(8) 0.2488(5) 0.046(2) Uani 1 1 d . .
O5 O 0.7664(7) 0.0934(8) 0.0475(5) 0.042(2) Uani 1 1 d . .
O4 O 0.6214(8) 0.1940(9) -0.0794(6) 0.055(3) Uani 1 1 d . .
O3 O 0.8426(9) -0.3212(9) 0.1380(7) 0.060(3) Uani 1 1 d . .
O2 O 0.8185(10) 0.1067(10) 0.2027(7) 0.065(3) Uani 1 1 d . .
O1 O 0.6192(11) -0.0892(14) 0.0419(9) 0.087(4) Uani 1 1 d . .
O1W O 0.8667(12) 0.9333(14) 0.6239(9) 0.090(4) Uani 1 1 d U .
O2W O 0.963(4) 0.547(4) 0.359(3) 0.148(16) Uani 0.5 1 d U P
O3W O 0.619(6) 0.615(7) 0.126(5) 0.25(3) Uani 0.5 1 d U P
O4W O 0.805(6) 0.328(7) 0.285(4) 0.27(3) Uani 0.5 1 d U P
O5W O 0.959(4) -0.014(5) 0.015(3) 0.155(17) Uani 0.5 1 d U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
Sb Sb -0.5866 1.5461 '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
O10 Sb4 O21 95.0(4) . .
O10 Sb4 O20 95.9(4) . .
O21 Sb4 O20 89.3(4) . .
O12 Sb3 O16 92.7(4) . .
O12 Sb3 O14 95.3(4) . .
O16 Sb3 O14 92.6(4) . .
O10 Sb2 O17 95.6(4) . .
O10 Sb2 O15 95.7(4) . 3_755
O17 Sb2 O15 92.1(4) . 3_755
O12 Sb1 O19 98.8(4) . .
O12 Sb1 O18 94.4(4) . .
O19 Sb1 O18 92.2(4) . .
O13 V7 O16 109.0(4) . .
O13 V7 O17 108.7(5) . .
O16 V7 O17 76.8(4) . .
O13 V7 O21 112.1(4) . .
O16 V7 O21 138.8(4) . .
O17 V7 O21 90.3(4) . .
O13 V7 O18 106.5(5) . .
O16 V7 O18 92.0(4) . .
O17 V7 O18 144.8(4) . .
O21 V7 O18 76.2(4) . .
O13 V7 V3 114.7(4) . 3_755
O16 V7 V3 38.3(3) . 3_755
O17 V7 V3 38.5(3) . 3_755
O21 V7 V3 118.8(3) . 3_755
O18 V7 V3 122.6(3) . 3_755
O13 V7 V5 113.2(4) . .
O16 V7 V5 121.4(3) . .
O17 V7 V5 122.4(3) . .
O21 V7 V5 38.0(3) . .
O18 V7 V5 38.3(3) . .
V3 V7 V5 132.11(9) 3_755 .
O6 V6 O14 108.6(5) . .
O6 V6 O15 108.4(5) . .
O14 V6 O15 143.0(4) . .
O6 V6 O20 110.8(5) . 3_755
O14 V6 O20 76.1(4) . 3_755
O15 V6 O20 91.2(4) . 3_755
O6 V6 O19 105.7(5) . .
O14 V6 O19 91.5(4) . .
O15 V6 O19 78.3(4) . .
O20 V6 O19 143.5(4) 3_755 .
O6 V6 V2 111.9(4) . .
O14 V6 V2 122.7(3) . .
O15 V6 V2 38.7(3) . .
O20 V6 V2 121.9(3) 3_755 .
O19 V6 V2 39.6(3) . .
O6 V6 V4 115.0(4) . 3_755
O14 V6 V4 38.3(3) . 3_755
O15 V6 V4 121.4(3) . 3_755
O20 V6 V4 37.8(3) 3_755 3_755
O19 V6 V4 122.2(3) . 3_755
V2 V6 V4 133.11(10) . 3_755
O4 V5 O5 108.2(5) . .
O4 V5 O11 105.7(5) . .
O5 V5 O11 83.6(4) . .
O4 V5 O21 108.7(5) . .
O5 V5 O21 143.1(4) . .
O11 V5 O21 88.2(4) . .
O4 V5 O18 106.5(5) . .
O5 V5 O18 90.7(4) . .
O11 V5 O18 147.5(4) . .
O21 V5 O18 77.3(4) . .
O4 V5 V1 110.0(5) . .
O5 V5 V1 41.6(3) . .
O11 V5 V1 42.2(3) . .
O21 V5 V1 123.3(3) . .
O18 V5 V1 126.7(3) . .
O4 V5 V7 111.1(5) . .
O5 V5 V7 122.7(3) . .
O11 V5 V7 121.9(3) . .
O21 V5 V7 38.3(2) . .
O18 V5 V7 39.1(3) . .
V1 V5 V7 138.86(11) . .
O7 V4 O11 105.5(5) . .
O7 V4 O9 106.8(5) . .
O11 V4 O9 86.2(4) . .
O7 V4 O20 108.0(5) . .
O11 V4 O20 89.0(4) . .
O9 V4 O20 144.9(4) . .
O7 V4 O14 109.2(5) . 3_755
O11 V4 O14 145.0(4) . 3_755
O9 V4 O14 88.6(4) . 3_755
O20 V4 O14 75.8(4) . 3_755
O7 V4 V1 108.8(4) . .
O11 V4 V1 43.7(3) . .
O9 V4 V1 42.8(3) . .
O20 V4 V1 126.0(3) . .
O14 V4 V1 125.1(3) 3_755 .
O7 V4 V6 113.4(4) . 3_755
O11 V4 V6 120.8(3) . 3_755
O9 V4 V6 120.4(3) . 3_755
O20 V4 V6 38.0(3) . 3_755
O14 V4 V6 37.8(3) 3_755 3_755
V1 V4 V6 137.82(11) . 3_755
O3 V3 O8 108.8(6) . .
O3 V3 O9 106.4(5) . .
O8 V3 O9 85.8(4) . .
O3 V3 O16 106.7(5) . 3_755
O8 V3 O16 144.4(4) . 3_755
O9 V3 O16 86.7(4) . 3_755
O3 V3 O17 107.5(5) . 3_755
O8 V3 O17 90.1(4) . 3_755
O9 V3 O17 145.3(4) . 3_755
O16 V3 O17 76.8(4) 3_755 3_755
O3 V3 V1 110.2(5) . .
O8 V3 V1 43.0(3) . .
O9 V3 V1 43.2(3) . .
O16 V3 V1 123.9(3) 3_755 .
O17 V3 V1 126.9(3) 3_755 .
O3 V3 V7 112.4(5) . 3_755
O8 V3 V7 121.2(3) . 3_755
O9 V3 V7 119.0(3) . 3_755
O16 V3 V7 38.3(3) 3_755 3_755
O17 V3 V7 38.5(3) 3_755 3_755
V1 V3 V7 137.34(12) . 3_755
O2 V2 O5 108.3(6) . .
O2 V2 O8 105.3(6) . .
O5 V2 O8 84.4(4) . .
O2 V2 O15 107.1(6) . .
O5 V2 O15 144.5(4) . .
O8 V2 O15 89.0(4) . .
O2 V2 O19 107.3(6) . .
O5 V2 O19 89.1(4) . .
O8 V2 O19 147.2(4) . .
O15 V2 O19 77.9(4) . .
O2 V2 V1 110.0(5) . .
O5 V2 V1 42.5(3) . .
O8 V2 V1 42.1(3) . .
O15 V2 V1 124.3(3) . .
O19 V2 V1 125.9(3) . .
O2 V2 V6 112.1(5) . .
O5 V2 V6 121.3(3) . .
O8 V2 V6 121.8(3) . .
O15 V2 V6 38.6(3) . .
O19 V2 V6 39.2(3) . .
V1 V2 V6 137.94(12) . .
O1 V1 O8 111.1(7) . .
O1 V1 O9 111.1(7) . .
O8 V1 O9 84.8(4) . .
O1 V1 O5 109.9(7) . .
O8 V1 O5 82.5(4) . .
O9 V1 O5 138.9(4) . .
O1 V1 O11 109.1(7) . .
O8 V1 O11 139.7(4) . .
O9 V1 O11 83.5(4) . .
O5 V1 O11 81.6(4) . .
O1 V1 V3 115.1(6) . .
O8 V1 V3 42.2(3) . .
O9 V1 V3 42.9(3) . .
O5 V1 V3 117.5(3) . .
O11 V1 V3 119.1(3) . .
O1 V1 V4 114.0(6) . .
O8 V1 V4 119.2(3) . .
O9 V1 V4 41.9(3) . .
O5 V1 V4 116.3(3) . .
O11 V1 V4 41.8(3) . .
V3 V1 V4 81.86(11) . .
O1 V1 V2 114.8(6) . .
O8 V1 V2 41.6(3) . .
O9 V1 V2 118.3(3) . .
O5 V1 V2 41.1(3) . .
O11 V1 V2 115.9(3) . .
V3 V1 V2 80.59(11) . .
V4 V1 V2 131.09(13) . .
O1 V1 V5 113.2(6) . .
O8 V1 V5 116.5(3) . .
O9 V1 V5 117.1(3) . .
O5 V1 V5 40.7(3) . .
O11 V1 V5 41.0(3) . .
V3 V1 V5 131.65(13) . .
V4 V1 V5 79.67(11) . .
V2 V1 V5 78.87(10) . .
V5 O21 V7 103.8(4) . .
V5 O21 Sb4 116.0(4) . .
V7 O21 Sb4 138.6(5) . .
V4 O20 V6 104.2(4) . 3_755
V4 O20 Sb4 116.9(5) . .
V6 O20 Sb4 138.7(5) 3_755 .
Sb1 O19 V6 138.1(5) . .
Sb1 O19 V2 120.7(5) . .
V6 O19 V2 101.1(4) . .
Sb1 O18 V5 119.8(5) . .
Sb1 O18 V7 137.6(5) . .
V5 O18 V7 102.6(4) . .
V7 O17 V3 103.0(4) . 3_755
V7 O17 Sb2 138.9(5) . .
V3 O17 Sb2 118.1(5) 3_755 .
V3 O16 V7 103.4(4) 3_755 .
V3 O16 Sb3 116.6(4) 3_755 .
V7 O16 Sb3 139.9(5) . .
V6 O15 V2 102.7(4) . .
V6 O15 Sb2 138.5(5) . 3_755
V2 O15 Sb2 118.4(4) . 3_755
V6 O14 V4 103.9(4) . 3_755
V6 O14 Sb3 141.6(5) . .
V4 O14 Sb3 114.4(5) 3_755 .
Sb1 O12 Sb3 132.6(5) . .
V4 O11 V5 149.2(5) . .
V4 O11 V1 94.5(4) . .
V5 O11 V1 96.8(4) . .
Sb4 O10 Sb2 132.9(5) . .
V4 O9 V3 151.1(6) . .
V4 O9 V1 95.3(4) . .
V3 O9 V1 94.0(5) . .
V3 O8 V2 149.3(6) . .
V3 O8 V1 94.8(4) . .
V2 O8 V1 96.3(4) . .
V2 O5 V5 148.5(6) . .
V2 O5 V1 96.4(4) . .
V5 O5 V1 97.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb4 O10 1.930(10) .
Sb4 O21 1.985(8) .
Sb4 O20 1.988(8) .
Sb3 O12 1.957(10) .
Sb3 O16 1.967(8) .
Sb3 O14 1.982(9) .
Sb2 O10 1.938(10) .
Sb2 O17 1.991(9) .
Sb2 O15 1.991(9) 3_755
Sb1 O12 1.946(10) .
Sb1 O19 1.948(9) .
Sb1 O18 1.958(9) .
V7 O13 1.600(9) .
V7 O16 1.967(9) .
V7 O17 1.969(10) .
V7 O21 1.973(9) .
V7 O18 2.000(10) .
V7 V3 3.085(3) 3_755
V7 V5 3.095(3) .
V6 O6 1.585(9) .
V6 O14 1.949(9) .
V6 O15 1.957(9) .
V6 O20 1.958(9) 3_755
V6 O19 1.972(9) .
V6 V2 3.059(3) .
V6 V4 3.084(3) 3_755
V5 O4 1.589(10) .
V5 O5 1.924(10) .
V5 O11 1.931(9) .
V5 O21 1.961(9) .
V5 O18 1.967(9) .
V5 V1 2.922(4) .
V4 O7 1.586(10) .
V4 O11 1.908(9) .
V4 O9 1.915(11) .
V4 O20 1.950(9) .
V4 O14 1.969(9) 3_755
V4 V1 2.854(4) .
V4 V6 3.084(3) 3_755
V3 O3 1.592(11) .
V3 O8 1.914(10) .
V3 O9 1.937(10) .
V3 O16 1.965(9) 3_755
V3 O17 1.972(9) 3_755
V3 V1 2.840(4) .
V3 V7 3.085(3) 3_755
V2 O2 1.591(12) .
V2 O5 1.905(10) .
V2 O8 1.922(9) .
V2 O15 1.959(9) .
V2 O19 1.989(9) .
V2 V1 2.880(4) .
V1 O1 1.625(14) .
V1 O8 1.943(10) .
V1 O9 1.947(10) .
V1 O5 1.958(10) .
V1 O11 1.977(10) .
O20 V6 1.957(9) 3_755
O17 V3 1.972(9) 3_755
O16 V3 1.965(9) 3_755
O15 Sb2 1.991(9) 3_755
O14 V4 1.969(9) 3_755
O5W O5W 1.45(9) 3_755
