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The double salt tetrapotassium disodium decavanadate decahydrate, K4Na2[V10O28]·10H2O, crystallizes in the triclinic system in space group P\overline 1. The centrosymmetric [V10O28]6− polyanion forms a three-dimensional network via Opolyanion...K+...Opolyanion coordination with K+ ions and Opolyanion...H—Owater...Na+ hydrogen bonds. The V...V distances are in the range 3.0601 (9)–3.271 (1) Å, and the four types of V—O bond lengths are in the ranges 1.597 (2)–1.621 (2) (Ot), 1.920 (2)–2.020 (2) (Oc), 1.682 (2)–2.072 (2) (Ob) and 2.088 (2)–2.368 (2) Å (Oh).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016453/br6109sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016453/br6109Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](V-O) = 0.002 Å
  • R factor = 0.034
  • wR factor = 0.094
  • Data-to-parameter ratio = 15.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: H20 K4 Na2 O38 V10 Atom count from _chemical_formula_moiety:H20 K160 O38 V10

Computing details top

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
Na2K4(V10O28)·10H2OZ = 1
Mr = 1339.94F(000) = 652
Triclinic, P1Dx = 2.654 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 8.620 (1) ÅCell parameters from 28 reflections
b = 10.387 (1) Åθ = 9.5–10.5°
c = 11.017 (2) ŵ = 3.30 mm1
α = 69.22 (1)°T = 298 K
β = 87.14 (1)°Hexagonal prism, pale brown
γ = 66.12 (1)°0.44 × 0.30 × 0.19 mm
V = 838.2 (2) Å3
Data collection top
Stoe Stadi-4
diffractometer
3393 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 27.5°, θmin = 2.0°
ω/2–θ scansh = 1111
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1996)
k = 1213
Tmin = 0.317, Tmax = 0.534l = 014
3845 measured reflections3 standard reflections every 60 min
3845 independent reflections intensity decay: 3.6%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0418P)2 + 1.8027P]
where P = (Fo2 + 2Fc2)/3
3845 reflections(Δ/σ)max < 0.001
244 parametersΔρmax = 0.95 e Å3
0 restraintsΔρmin = 1.08 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.31082 (6)0.49974 (5)0.52005 (5)0.01449 (12)
V20.47458 (7)0.20815 (6)0.76614 (5)0.01953 (13)
V30.52954 (6)0.49445 (6)0.74540 (5)0.01700 (12)
V40.82986 (6)0.21084 (6)0.72371 (5)0.01911 (13)
V50.62322 (6)0.21477 (6)0.49938 (5)0.01716 (12)
K10.18488 (10)0.78857 (9)0.50573 (9)0.03254 (18)
K20.26515 (16)0.81715 (13)0.92705 (10)0.0635 (4)
Na0.07082 (17)0.66774 (15)0.86876 (13)0.0279 (3)
Oh10.4307 (2)0.6251 (2)0.39380 (19)0.0155 (4)
Oc20.3180 (3)0.6169 (2)0.6196 (2)0.0162 (4)
Oc30.3969 (3)0.3805 (2)0.4129 (2)0.0162 (4)
Ob40.1250 (3)0.6252 (2)0.4279 (2)0.0189 (4)
Ob50.2656 (3)0.3680 (2)0.6425 (2)0.0185 (4)
Ob60.7057 (3)0.1162 (2)0.8254 (2)0.0215 (4)
Ob70.4436 (3)0.3577 (2)0.8349 (2)0.0206 (4)
Ob80.7518 (3)0.3614 (2)0.7985 (2)0.0198 (4)
Ob90.5187 (3)0.1299 (2)0.6315 (2)0.0202 (4)
Ob100.8300 (3)0.1321 (2)0.5958 (2)0.0196 (4)
Ot110.3945 (3)0.1030 (3)0.8652 (2)0.0304 (5)
Ot120.4948 (3)0.5977 (3)0.8333 (2)0.0238 (5)
Ot131.0241 (3)0.1100 (3)0.7909 (2)0.0278 (5)
Ot140.6594 (3)0.1132 (3)0.4099 (2)0.0243 (5)
Ow10.0300 (3)0.5184 (3)0.7436 (3)0.0383 (7)
Hw1A0.09390.45610.76820.057*
Hw1B0.08940.45750.74090.057*
Ow20.0289 (4)0.8147 (3)0.7004 (3)0.0533 (9)
Hw2A0.14300.76900.67530.080*
Hw2B0.01400.91850.65610.080*
Ow30.3404 (4)0.8173 (3)0.7436 (3)0.0453 (8)
Hw3A0.39060.92050.74120.068*
Hw3B0.42110.77120.76800.068*
Ow40.2044 (3)0.4874 (3)0.9860 (2)0.0315 (6)
Hw4A0.25740.52781.03000.047*
Hw4B0.28280.43820.93350.047*
Ow50.0692 (4)0.8226 (3)0.9772 (3)0.0441 (7)
Hw5A0.07790.77991.07010.066*
Hw5B0.15900.92410.93920.066*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0116 (2)0.0131 (2)0.0163 (2)0.00295 (18)0.00095 (18)0.00516 (19)
V20.0187 (3)0.0167 (3)0.0184 (3)0.0058 (2)0.00202 (19)0.0029 (2)
V30.0181 (2)0.0156 (2)0.0146 (2)0.00338 (19)0.00013 (19)0.00645 (19)
V40.0149 (2)0.0158 (2)0.0198 (3)0.00167 (19)0.00293 (19)0.0037 (2)
V50.0177 (2)0.0125 (2)0.0182 (3)0.00258 (19)0.00069 (19)0.0064 (2)
K10.0293 (4)0.0290 (4)0.0396 (4)0.0094 (3)0.0038 (3)0.0160 (3)
K20.0656 (7)0.0447 (6)0.0379 (5)0.0176 (5)0.0048 (5)0.0140 (4)
Na0.0299 (7)0.0250 (7)0.0282 (7)0.0113 (6)0.0024 (6)0.0092 (6)
Oh10.0137 (9)0.0141 (9)0.0154 (10)0.0031 (8)0.0008 (8)0.0047 (8)
Oc20.0143 (9)0.0141 (9)0.0174 (10)0.0022 (8)0.0009 (8)0.0067 (8)
Oc30.0142 (9)0.0156 (10)0.0181 (10)0.0049 (8)0.0009 (8)0.0068 (8)
Ob40.0142 (10)0.0186 (10)0.0206 (11)0.0041 (8)0.0000 (8)0.0066 (9)
Ob50.0160 (10)0.0168 (10)0.0209 (11)0.0061 (8)0.0033 (8)0.0059 (8)
Ob60.0204 (11)0.0173 (10)0.0195 (11)0.0041 (9)0.0010 (8)0.0025 (9)
Ob70.0205 (10)0.0211 (11)0.0176 (10)0.0066 (9)0.0033 (8)0.0066 (9)
Ob80.0181 (10)0.0195 (10)0.0179 (10)0.0045 (9)0.0018 (8)0.0059 (9)
Ob90.0211 (10)0.0143 (10)0.0226 (11)0.0060 (8)0.0008 (9)0.0050 (9)
Ob100.0173 (10)0.0123 (9)0.0233 (11)0.0010 (8)0.0001 (8)0.0056 (8)
Ot110.0317 (13)0.0282 (13)0.0273 (13)0.0149 (11)0.0050 (10)0.0029 (10)
Ot120.0261 (11)0.0264 (12)0.0212 (11)0.0084 (10)0.0030 (9)0.0141 (10)
Ot130.0193 (11)0.0241 (12)0.0304 (13)0.0013 (9)0.0067 (9)0.0071 (10)
Ot140.0256 (11)0.0202 (11)0.0277 (12)0.0059 (9)0.0018 (9)0.0134 (10)
Ow10.0287 (13)0.0449 (16)0.0592 (19)0.0189 (12)0.0165 (13)0.0365 (15)
Ow20.0533 (19)0.0259 (14)0.068 (2)0.0113 (13)0.0395 (17)0.0129 (14)
Ow30.0384 (15)0.0235 (13)0.067 (2)0.0088 (12)0.0164 (14)0.0103 (13)
Ow40.0249 (12)0.0380 (14)0.0265 (13)0.0080 (11)0.0026 (10)0.0119 (11)
Ow50.0582 (19)0.0288 (14)0.0295 (14)0.0021 (13)0.0096 (13)0.0098 (12)
Geometric parameters (Å, º) top
V1—V1i3.271 (1)V5—Ob91.819 (2)
V1—V23.1001 (9)V5—Ob101.829 (2)
V1—V3i3.1607 (9)V5—Ot141.619 (2)
V1—V4i3.0601 (9)K1—Oc3ii2.923 (2)
V1—V5i3.1725 (7)K1—Ob42.807 (2)
V2—V43.0847 (8)K1—Ob5ii2.951 (2)
V3—V5i3.0795 (9)K1—Ob9ii2.973 (2)
V3—V43.1145 (8)K1—Ot14iii2.870 (2)
V4—V53.0969 (9)K1—Ow12.937 (3)
V1—Oh12.088 (2)K1—Ow23.047 (4)
V1—Oh1i2.132 (2)K1—Ow32.938 (4)
V1—Oc21.924 (2)K2—Ob6iv3.086 (3)
V1—Oc31.920 (2)K2—Ob7iv3.172 (2)
V1—Ob41.682 (2)K2—Ob8iv2.966 (3)
V1—Ob51.707 (2)K2—Ot11v3.420 (3)
V2—Oh1i2.368 (2)K2—Ot122.827 (2)
V2—Ob52.019 (2)K2—Ot13iii2.788 (3)
V2—Ob61.858 (2)K2—Ow23.313 (4)
V2—Ob71.881 (2)K2—Ow52.889 (4)
V2—Ob91.885 (2)Na—Ow12.337 (3)
V2—Ot111.597 (2)Na—Ow22.325 (3)
V3—Oh1i2.228 (2)Na—Ow32.365 (3)
V3—Oc21.997 (2)Na—Ow42.407 (3)
V3—Oc3i2.020 (2)Na—Ow4vi2.444 (3)
V3—Ob71.824 (2)Na—Ow52.324 (3)
V3—Ob81.821 (2)Ow1—Hw1a0.9714
V3—Ot121.621 (2)Ow1—Hw1b0.9709
V4—Oh1i2.291 (2)Ow2—Hw2a0.9784
V4—Ob4i2.072 (2)Ow2—Hw2b0.9265
V4—Ob61.822 (2)Ow3—Hw3a0.9709
V4—Ob81.893 (2)Ow3—Hw3b0.9714
V4—Ob101.864 (2)Ow4—Hw4a0.9704
V4—Ot131.613 (2)Ow4—Hw4b0.9711
V5—Oh1i2.253 (2)OW5—Hw5a0.9730
V5—Oc2i2.015 (2)Ow5—Hw5b0.9716
V5—Oc31.995 (2)
V4i—V1—V2176.49 (2)Ob9—V5—Oc389.85 (9)
V4i—V1—V3i60.06 (2)Ob10—V5—Oc3154.64 (9)
V2—V1—V3i118.27 (2)Ot14—V5—Oc2i99.8 (1)
V4i—V1—V5i59.56 (2)Ob9—V5—Oc2i154.81 (9)
V2—V1—V5i118.00 (2)Ob10—V5—Oc2i89.01 (9)
V3i—V1—V5i89.58 (2)Oc3—V5—Oc2i76.27 (9)
V4i—V1—V1i88.13 (2)Ot14—V5—Oh1i174.6 (1)
V2—V1—V1i88.39 (2)Ob9—V5—Oh1i81.17 (9)
V3i—V1—V1i58.89 (2)Ob10—V5—Oh1i80.18 (8)
V5i—V1—V1i58.85 (2)OC3—V5—OH1i76.17 (8)
V4—V2—V190.85 (2)OC2i—V5—OH1i75.19 (8)
V5i—V3—V4119.32 (2)Ob4—K1—Ot14iii122.30 (7)
V1i—V4—V292.62 (2)Ob4—K1—Oc3ii112.37 (7)
V1i—V4—V562.03 (2)Ot14iii—K1—Oc3ii119.96 (7)
V2—V4—V560.96 (2)Ob4—K1—Ow178.12 (7)
V1i—V4—V361.57 (2)Ot14iii—K1—Ow1143.03 (7)
V2—V4—V360.547 (19)Oc3ii—K1—Ow167.67 (7)
V5—V4—V391.83 (2)Ob4—K1—Ow3140.35 (8)
V3i—V5—V4119.17 (2)Ot14iii—K1—Ow383.43 (8)
Ob4—V1—Ob5106.6 (1)Oc3ii—K1—Ow368.32 (7)
Ob4—V1—Oc398.1 (1)Ow1—K1—Ow365.40 (8)
Ob5—V1—Oc396.1 (1)Ob4—K1—Ob5ii73.82 (6)
Ob4—V1—Oc297.2 (1)Ot14iii—K1—Ob5ii118.88 (7)
Ob5—V1—Oc297.0 (1)Oc3ii—K1—Ob5ii54.76 (6)
Oc3—V1—Oc2156.10 (9)Ow1—K1—Ob5ii95.43 (7)
Ob4—V1—Oh188.34 (9)Ow3—K1—Ob5ii122.81 (7)
Ob5—V1—Oh1165.08 (9)Ob4—K1—Ob9ii121.50 (7)
Oc3—V1—Oh181.06 (9)Ot14iii—K1—Ob9ii76.09 (7)
Oc2—V1—Oh181.09 (9)Oc3ii—K1—Ob9ii54.43 (6)
Ob4—V1—Oh1i166.7 (1)Ow1—K1—Ob9ii122.10 (7)
Ob5—V1—Oh1i86.74 (9)Ow3—K1—Ob9ii92.01 (7)
Oc3—V1—Oh1i80.69 (8)Ob5ii—K1—Ob9ii51.85 (6)
Oc2—V1—Oh1i80.24 (8)Ob4—K1—Ow286.76 (7)
Oh1—V1—Oh1i78.36 (9)Ot14iii—K1—Ow284.94 (8)
Ot11—V2—Ob6105.0 (1)Oc3ii—K1—Ow2122.58 (7)
Ot11—V2—Ob7104.1 (1)Ow1—K1—Ow264.35 (8)
Ob6—V2—Ob789.9 (1)Ow3—K1—Ow264.30 (8)
Ot11—V2—Ob9101.6 (1)Ob5ii—K1—Ow2154.80 (7)
Ob6—V2—Ob990.9 (1)Ob9ii—K1—Ow2151.36 (7)
Ob7—V2—Ob9153.1 (1)Ot13iii—K2—Ot12130.18 (8)
Ot11—V2—Ob5100.8 (1)Ot13iii—K2—Ow572.21 (8)
Ob6—V2—Ob5154.1 (1)Ot12—K2—Ow5119.03 (9)
Ob7—V2—Ob584.54 (9)Ot13iii—K2—Ob8iv123.32 (8)
Ob9—V2—Ob583.05 (9)Ot12—K2—Ob8iv103.76 (7)
Ot11—V2—Oh1i174.7 (1)Ow5—K2—Ob8iv66.59 (8)
Ob6—V2—Oh1i80.15 (9)Ot13iii—K2—Ob6iv93.38 (7)
Ob7—V2—Oh1i76.88 (8)Ot12—K2—Ob6iv131.44 (7)
Ob9—V2—Oh1i76.83 (8)Ow5—K2—Ob6iv91.13 (8)
Ob5—V2—Oh1i73.99 (8)Ob8iv—K2—Ob6iv51.80 (6)
Ot12—V3—Ob8102.9 (1)Ot13iii—K2—Ob7iv139.41 (8)
Ot12—V3—Ob7102.9 (1)Ot12—K2—Ob7iv81.64 (7)
Ob8—V3—Ob794.7 (1)Ow5—K2—Ob7iv118.16 (8)
Ot12—V3—Oc299.5 (1)Ob8iv—K2—Ob7iv51.65 (6)
Ob8—V3—Oc2155.07 (9)Ob6iv—K2—Ob7iv49.91 (6)
Ob7—V3—Oc290.8 (1)Ot13iii—K2—Ow270.10 (8)
Ot12—V3—Oc3i99.3 (1)Ot12—K2—Ow275.47 (7)
Ob8—V3—Oc3i89.57 (9)Ow5—K2—Ow260.46 (8)
Ob7—V3—Oc3i155.84 (9)Ob8iv—K2—Ow2116.26 (8)
Oc2—V3—Oc3i76.11 (9)Ob6iv—K2—Ow2150.02 (7)
Ot12—V3—Oh1i174.0 (1)Ob7iv—K2—Ow2150.39 (7)
Ob8—V3—Oh1i80.37 (9)Ot13iii—K2—Ot11v63.31 (7)
Ob7—V3—Oh1i81.73 (9)Ot12—K2—Ot11v109.14 (8)
Oc2—V3—Oh1i76.37 (8)Ow5—K2—Ot11v128.60 (8)
Oc3i—V3—Oh1i75.55 (8)Ob8iv—K2—Ot11v119.11 (7)
Ot13—V4—Ob6105.1 (1)Ob6iv—K2—Ot11v68.07 (7)
Ot13—V4—Ob10100.5 (1)Ob7iv—K2—Ot11v84.28 (7)
Ob6—V4—Ob1093.1 (1)Ow2—K2—Ot11v120.78 (7)
Ot13—V4—Ob8102.5 (1)Ow5—Na—Ow285.1 (1)
Ob6—V4—Ob890.8 (1)Ow5—Na—Ow1169.7 (1)
Ob10—V4—Ob8154.78 (9)Ow2—Na—Ow186.3 (1)
Ot13—V4—Ob4i97.5 (1)Ow5—Na—Ow3100.0 (1)
Ob6—V4—Ob4i157.37 (9)Ow2—Na—Ow385.6 (1)
Ob10—V4—Ob4i83.46 (9)Ow1—Na—Ow384.9 (1)
Ob8—V4—Ob4i83.43 (9)Ow5—Na—Ow488.1 (1)
Ot13—V4—Oh1i171.9 (1)Ow2—Na—Ow496.5 (1)
Ob6—V4—Oh1i83.03 (9)Ow1—Na—Ow487.3 (1)
Ob10—V4—Oh1i78.46 (8)Ow3—Na—Ow4171.8 (1)
Ob8—V4—Oh1i77.29 (8)Ow5—Na—Ow4vi103.2 (1)
OB4i—V4—OH1i74.36 (8)Ow2—Na—Ow4vi169.6 (1)
Ot14—V5—Ob9103.4 (1)Ow1—Na—Ow4vi86.0 (1)
Ot14—V5—Ob10102.1 (1)Ow3—Na—Ow4vi86.8 (1)
Ob9—V5—Ob1095.5 (1)Ow4—Na—Ow4vi90.1 (1)
Ot14—V5—Oc3100.7 (1)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x1, y+1, z; (iv) x+1, y+1, z+2; (v) x, y+1, z; (vi) x, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
Ow1—Hw1a···Ob4ii0.972.643.100 (3)109
Ow1—Hw1b···Ob50.971.942.811 (3)148
Ow2—Hw2a···Oc20.981.952.856 (3)152
Ow2—Hw2b···Ob10iii0.931.952.839 (4)160
Ow3—Hw3a···Ob9iii0.971.912.767 (3)146
Ow3—Hw3b···Ot14ii0.972.502.989 (4)111
Ow4—Hw4b···Ob70.971.832.799 (3)174
Ow4—Hw4a···Ot12iv0.972.282.980 (3)128
Ow5—Hw5b···Ob6iii0.971.842.789 (4)163
Ow5—Hw5a···Ot13iv0.972.372.959 (4)119
Symmetry codes: (ii) x, y+1, z+1; (iii) x1, y+1, z; (iv) x+1, y+1, z+2.
 

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