#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/31/2203141.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2203141
loop_
_publ_author_name
'Lee, Uk'
'Joo, Hea-Chung'
_publ_section_title
;
 A novel monoprotonated decavanadate,
 K₄Na[HV₁₀O₂₈]·10H₂O
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i22
_journal_page_last               i24
_journal_paper_doi               10.1107/S1600536804000893
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'K4 Na [H V10 O28] , 10H2O'
_chemical_formula_moiety         'H O28 V10 5- , 10H2 O , 4K + , Na +'
_chemical_formula_structural     'K4 [Na (H2 O)6] [H V10 O28] (H2 O)4'
_chemical_formula_sum            'H21 K4 Na O38 V10'
_chemical_formula_weight         1317.96
_chemical_name_systematic
;
tetrapotassium sodium hydrogendecavanadate decahydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 95.78(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.804(2)
_cell_length_b                   11.034(2)
_cell_length_c                   13.748(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      10.4
_cell_measurement_theta_min      9.5
_cell_volume                     1630.6(6)
_computing_cell_refinement       STADI4
_computing_data_collection       'STADI4 (Stoe, 1996)'
_computing_data_reduction        'X-RED (Stoe, 1996)'
_computing_molecular_graphics
'ORTEPIII (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe STADI4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3731
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        3.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.381
_exptl_absorpt_correction_T_max  0.7716
_exptl_absorpt_correction_T_min  0.1623
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    2.684
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'tetragonal plate'
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.759
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0524P)²+4.4779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                2768
_reflns_number_total             3731
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br6134.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2203141
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
V1 0.59825(7) 0.72243(7) 0.73747(5) 0.01308(17) Uani d . 1 V
V2 0.89274(7) 0.72146(8) 0.53687(6) 0.01764(19) Uani d . 1 V
V3 0.60767(7) 0.72429(9) 0.51615(6) 0.01894(19) Uani d . 1 V
V4 0.75513(7) 0.51673(7) 0.63997(6) 0.01633(19) Uani d . 1 V
V5 0.75031(7) 0.92626(7) 0.63897(6) 0.01554(19) Uani d . 1 V
K1 0.26547(11) 0.77905(13) 0.53613(9) 0.0323(3) Uani d . 1 K
K2 0.46048(15) 0.79143(15) 0.23514(10) 0.0459(4) Uani d . 1 K
Na 0.7500 1.0061(3) 0.2500 0.0250(6) Uani d S 1 Na
Oh1 0.7479(3) 0.7210(3) 0.6528(2) 0.0143(6) Uani d . 1 O
Oc2 0.6351(3) 0.5505(3) 0.7404(2) 0.0143(6) Uani d . 1 O
Oc3 0.6351(3) 0.8935(3) 0.7408(2) 0.0150(6) Uani d . 1 O
Ob4 0.5062(3) 0.7218(3) 0.8299(2) 0.0184(7) Uani d . 1 O
Ob5 0.7497(3) 0.7216(3) 0.4538(2) 0.0184(7) Uani d . 1 O
Ob6 0.5030(3) 0.7225(3) 0.6326(2) 0.0181(7) Uani d . 1 O
Ob7 0.8745(3) 0.8876(3) 0.5635(2) 0.0183(7) Uani d . 1 O
Ob8 0.6264(3) 0.8895(3) 0.5446(2) 0.0192(7) Uani d . 1 O
Ob9 0.8730(3) 0.5555(3) 0.5628(2) 0.0185(7) Uani d . 1 O
Ob10 0.6226(3) 0.5539(3) 0.5421(2) 0.0195(7) Uani d . 1 O
Ot11 1.0021(3) 0.7255(4) 0.4659(3) 0.0273(8) Uani d . 1 O
Ot12 0.4949(3) 0.7267(4) 0.4309(2) 0.0267(8) Uani d . 1 O
Ot13 0.7529(3) 1.0723(3) 0.6388(3) 0.0236(8) Uani d . 1 O
Ot14 0.7561(3) 0.3710(3) 0.6408(3) 0.0238(8) Uani d . 1 O
OW1 0.2145(4) 0.5539(4) 0.6186(3) 0.0388(10) Uani d . 1 O
OW2 0.2500 0.7773(5) 0.7500 0.0292(12) Uani d S 1 O
OW3 0.7500 0.7933(6) 0.2500 0.0456(16) Uani d S 1 O
OW4 0.5906(4) 0.9997(4) 0.3582(3) 0.0423(11) Uani d . 1 O
OW5 0.8910(4) 1.0145(5) 0.3893(3) 0.0517(14) Uani d . 1 O
OW6 0.5891(4) 0.5658(4) 0.2630(3) 0.0411(11) Uani d . 1 O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
V3 V1 V2 . 2_656 176.30(3)
V3 V1 V4 . 2_656 118.12(3)
V2 V1 V4 2_656 2_656 59.92(3)
V3 V1 V5 . . 59.92(3)
V2 V1 V5 2_656 . 117.75(3)
V4 V1 V5 2_656 . 118.99(3)
V3 V1 V5 . 2_656 117.49(3)
V2 V1 V5 2_656 2_656 60.20(3)
V4 V1 V5 2_656 2_656 91.14(3)
V5 V1 V5 . 2_656 57.58(3)
V3 V1 V4 . . 61.07(3)
V2 V1 V4 2_656 . 116.88(3)
V4 V1 V4 2_656 . 57.05(3)
V5 V1 V4 . . 90.29(3)
V5 V1 V4 2_656 . 117.39(3)
V3 V2 V1 . 2_656 91.32(3)
V3 V2 V4 . . 61.93(3)
V1 V2 V4 2_656 . 61.03(3)
V3 V2 V5 . . 60.10(3)
V1 V2 V5 2_656 . 61.13(3)
V4 V2 V5 . . 92.32(3)
V1 V3 V2 . . 92.37(3)
V1 V3 V5 . . 61.86(3)
V2 V3 V5 . . 61.20(3)
V1 V3 V4 . . 61.81(3)
V2 V3 V4 . . 59.92(3)
V5 V3 V4 . . 91.79(3)
V4 V4 V2 2_656 . 121.26(3)
V4 V4 V3 2_656 . 117.77(3)
V2 V4 V3 . . 58.15(3)
V4 V4 V1 2_656 . 60.65(3)
V2 V4 V1 . . 88.48(3)
V3 V4 V1 . . 57.12(3)
V5 V5 V3 2_656 . 119.48(3)
V5 V5 V2 2_656 . 119.80(3)
V3 V5 V2 . . 58.69(3)
V5 V5 V1 2_656 . 61.27(3)
V3 V5 V1 . . 58.22(3)
V2 V5 V1 . . 88.78(3)
Ob6 V1 Ob4 . . 106.8(2)
Ob6 V1 Oc3 . . 97.3(2)
Ob4 V1 Oc3 . . 97.0(2)
Ob6 V1 Oc2 . . 97.2(2)
Ob4 V1 Oc2 . . 96.6(2)
Oc3 V1 Oc2 . . 156.30(10)
Ob6 V1 Oh1 . . 87.90(10)
Ob4 V1 Oh1 . . 165.30(10)
Oc3 V1 Oh1 . . 81.40(10)
Oc2 V1 Oh1 . . 80.50(10)
Ob6 V1 Oh1 . 2_656 166.50(10)
Ob4 V1 Oh1 . 2_656 86.80(10)
Oc3 V1 Oh1 . 2_656 81.10(10)
Oc2 V1 Oh1 . 2_656 80.40(10)
OH1 V1 Oh1 . 2_656 78.60(10)
Ot11 V2 Ob5 . . 104.4(2)
Ot11 V2 Ob9 . . 104.3(2)
Ob5 V2 Ob9 . . 90.8(2)
Ot11 V2 Ob7 . . 100.9(2)
Ob5 V2 Ob7 . . 91.3(2)
Ob9 V2 Ob7 . . 153.40(10)
Ot11 V2 Ob4 . 2_656 100.7(2)
Ob5 V2 Ob4 . 2_656 155.00(10)
Ob9 V2 Ob4 . 2_656 83.8(2)
Ob7 V2 Ob4 . 2_656 83.10(10)
Ot11 V2 Oh1 . . 174.4(2)
Ob5 V2 Oh1 . . 81.10(10)
Ob9 V2 Oh1 . . 76.90(10)
Ob7 V2 Oh1 . . 77.30(10)
Ob4 V2 Oh1 2_656 . 73.90(10)
Ot12 V3 Ob5 . . 105.6(2)
Ot12 V3 Ob8 . . 101.3(2)
Ob5 V3 Ob8 . . 92.0(2)
Ot12 V3 Ob10 . . 101.3(2)
Ob5 V3 Ob10 . . 90.7(2)
Ob8 V3 Ob10 . . 155.70(10)
Ot12 V3 Ob6 . . 97.6(2)
Ob5 V3 Ob6 . . 156.70(10)
Ob8 V3 Ob6 . . 84.40(10)
Ob10 V3 Ob6 . . 83.60(10)
Ot12 V3 Oh1 . . 172.0(2)
Ob5 V3 Oh1 . . 82.40(10)
Ob8 V3 Oh1 . . 78.20(10)
Ob10 V3 Oh1 . . 78.20(10)
Ob6 V3 Oh1 . . 74.40(10)
Ot14 V4 Ob9 . . 103.8(2)
Ot14 V4 Ob10 . . 103.0(2)
Ob9 V4 Ob10 . . 93.4(2)
Ot14 V4 Oc2 . 2_656 100.4(2)
Ob9 V4 Oc2 . 2_656 92.60(10)
Ob10 V4 Oc2 . 2_656 153.7(2)
Ot14 V4 Oc2 . . 100.6(2)
Ob9 V4 Oc2 . . 154.8(2)
Ob10 V4 Oc2 . . 87.40(10)
Oc2 V4 Oc2 2_656 . 76.60(10)
Ot14 V4 Oh1 . . 174.7(2)
Ob9 V4 Oh1 . . 80.80(10)
Ob10 V4 Oh1 . . 79.10(10)
Oc2 V4 Oh1 2_656 . 76.60(10)
Oc2 V4 Oh1 . . 74.60(10)
Ot13 V5 Ob8 . . 103.5(2)
Ot13 V5 Ob7 . . 102.7(2)
Ob8 V5 Ob7 . . 94.2(2)
Ot13 V5 Oc3 . 2_656 100.0(2)
Ob8 V5 Oc3 . 2_656 154.6(2)
Ob7 V5 Oc3 . 2_656 89.90(10)
Ot13 V5 Oc3 . . 101.2(2)
Ob8 V5 Oc3 . . 89.70(10)
Ob7 V5 Oc3 . . 154.2(2)
Oc3 V5 Oc3 2_656 . 76.40(10)
Ot13 V5 Oh1 . . 175.3(2)
Ob8 V5 Oh1 . . 79.80(10)
Ob7 V5 Oh1 . . 80.20(10)
Oc3 V5 Oh1 2_656 . 76.20(10)
Oc3 V5 Oh1 . . 75.40(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 V2 2_656 3.0940(10) ?
V1 V3 . 3.0550(10) ?
V1 V4 2_656 3.1560(10) ?
V1 V5 . 3.1690(10) ?
V1 V5 2_656 3.1720(10) ?
V1 V4 . 3.2060(10) ?
V2 V3 . 3.0650(10) ?
V2 V4 . 3.1220(10) ?
V2 V5 . 3.1430(10) ?
V3 V4 . 3.1840(10) ?
V3 V5 . 3.1100(10) ?
V4 V4 2_656 3.039(2) ?
V5 V5 2_656 3.054(2) ?
V1 Oh1 . 2.085(3) yes
V1 Oh1 2_656 2.129(3) yes
V1 Oc2 . 1.939(3) yes
V1 Oc3 . 1.929(3) yes
V1 Ob4 . 1.691(3) yes
V1 Ob6 . 1.684(3) yes
V2 Oh1 . 2.343(3) yes
V2 Ob4 2_656 2.036(3) yes
V2 Ob5 . 1.827(3) yes
V2 Ob7 . 1.884(4) yes
V2 Ob9 . 1.881(4) yes
V2 Ot11 . 1.607(3) yes
V3 Oh1 . 2.292(3) yes
V3 Ob5 . 1.832(3) yes
V3 Ob6 . 2.051(3) yes
V3 Ob8 . 1.871(4) yes
V3 Ob10 . 1.917(4) yes
V3 Ot12 . 1.603(3) yes
V4 Oh1 . 2.263(3) yes
V4 Oc2 . 2.021(3) yes
V4 Oc2 2_656 1.964(3) yes
V4 Ob9 . 1.790(3) yes
V4 Ob10 . 1.908(3) yes
V4 Ot14 . 1.608(4) yes
V5 Oh1 . 2.273(3) yes
V5 Oc3 . 1.997(3) yes
V5 Oc3 2_656 1.996(3) yes
V5 Ob7 . 1.827(3) yes
V5 Ob8 . 1.814(3) yes
V5 Ot13 . 1.612(4) yes
K1 Ob6 . 2.838(3) yes
K1 Ot11 1_455 2.970(4) yes
K1 Ot12 . 3.048(4) yes
K1 Ot13 3_676 2.901(4) yes
K1 Ot14 3_666 2.932(4) yes
K1 OW1 . 2.808(5) yes
K1 OW2 . 2.9619(14) yes
K1 OW4 3_676 3.167(5) yes
K1 OW5 3_676 3.073(6) yes
K2 Ot11 2_655 2.925(4) yes
K2 Ot12 . 2.773(4) yes
K2 Ot13 3_676 3.374(4) yes
K2 Ot13 4_575 2.906(4) yes
K2 Ot14 4_565 3.032(4) yes
K2 OW3 . 3.1141(17) yes
K2 OW4 . 3.105(5) yes
K2 OW6 . 2.858(5) yes
Na OW2 3_676 2.390(6) yes
Na OW3 . 2.348(7) yes
Na OW4 2_655 2.387(4) yes
Na OW4 . 2.387(4) yes
Na OW5 2_655 2.325(4) yes
Na OW5 . 2.325(4) yes
OW1 OW6 4_566 2.839(6) yes
OW1 Ob9 3_666 2.845(5) yes
OW1 OW6 3_666 2.864(7) yes
OW2 Ob4 2_556 2.938(3) yes
OW2 OW1 2_556 3.057(6) yes
OW3 Ob5 . 2.911(4) yes
OW3 Ob5 2_655 2.911(4) yes
OW3 OW6 . 3.069(7) yes
OW3 OW6 2_655 3.069(7) yes
OW4 Oc3 3_676 2.919(5) yes
OW4 Ob8 . 2.827(5) yes
OW4 Ob8 3_676 3.068(5) yes
OW5 Ob7 . 2.796(5) yes
OW5 Ob7 3_776 2.771(5) yes
OW6 Oc2 3_666 2.738(5) yes
Ob10 Ob10 3_666 3.025(7) yes
