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The crystal structure of the title compound, poly[deca-μ-aqua-octa­aqua-μ-deca­vanadato-dilithium(I)tetra­sodium(I)] [Li2Na4(H2O)18{V10O28}]n, consists of polymeric chains composed of centrosymmetric [V10O28]6− polyanions with Ci symmetry linked by [LiNa2(H2O)9]3+ cation groups via O-polyanion—Na-group—O-polyanion coordination, with Na—O bond lengths of 2.366 (2)–2.495 (2) Å. The lithium disodium nona­hydrate is composed of two NaO6 octa­hedra and one LiO4 tetra­hedron. Hydrogen bonds occur between the polyanion and the cation group, and within the cation group. Intra­chain OW—H...O hydrogen bonds stabilize the polymeric chain structure, while inter­chain OW—H...O hydrogen bonds link neighbouring polymeric chains to form the complete supramolecular structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805023123/br6199sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805023123/br6199Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](V-O) = 0.001 Å
  • R factor = 0.027
  • wR factor = 0.097
  • Data-to-parameter ratio = 16.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 6 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 9 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 10 H2 O
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 2002); data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: CRYSTALS (Watkin et al., 1996); molecular graphics: WinGX (Farrugia, 1999); software used to prepare material for publication: CrystalStructure.

poly[penta-µ-aqua-tetraaqua-µ-decavanadato-lithium(I)disodium(I)] top
Crystal data top
[Li2Na4(H2O)18V10O28]Z = 1
Mr = 1387.51F(000) = 684.00
Triclinic, P1Dx = 2.326 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.7107 Å
a = 8.5386 (6) ÅCell parameters from 5541 reflections
b = 10.6333 (7) Åθ = 2.5–27.5°
c = 11.8912 (6) ŵ = 2.42 mm1
α = 105.636 (3)°T = 273 K
β = 101.852 (3)°Block, orange
γ = 99.257 (3)°0.40 × 0.30 × 0.20 mm
V = 990.4 (1) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
3990 reflections with F2 > 2σ(F2)
Detector resolution: 10.00 pixels mm-1Rint = 0.024
ω scansθmax = 27.5°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1011
Tmin = 0.438, Tmax = 0.616k = 1313
9308 measured reflectionsl = 1515
4471 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: difference Fourier map
wR(F2) = 0.097H-atom parameters constrained
S = 1.02 w = 1/[0.001Fo2 + σ(Fo2)]/(4Fo2)
4467 reflections(Δ/σ)max < 0.001
280 parametersΔρmax = 0.48 e Å3
Primary atom site location: structure-invariant direct methodsΔρmin = 0.52 e Å3
Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement using reflections with F2 > 2.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.78731 (4)0.66163 (3)0.27151 (3)0.01683 (9)
V20.59589 (4)0.76990 (3)0.07942 (3)0.01567 (9)
V30.30870 (4)0.51024 (3)0.00358 (3)0.01229 (9)
V40.50849 (4)0.40158 (3)0.18695 (3)0.01479 (9)
V50.42980 (4)0.68105 (3)0.26387 (3)0.01749 (9)
Na10.2248 (1)0.85169 (9)0.51660 (8)0.0262 (2)
Na20.0062 (1)0.7475 (1)0.6890 (1)0.0418 (3)
O10.9595 (2)0.7141 (2)0.3711 (1)0.0272 (4)
O20.7894 (2)0.7920 (1)0.1962 (1)0.0182 (3)
O30.6315 (2)0.9024 (1)0.0402 (1)0.0252 (4)
O40.3971 (2)0.6651 (1)0.0493 (1)0.0138 (3)
O50.1470 (2)0.4454 (1)0.1285 (1)0.0165 (3)
O60.3151 (2)0.3544 (1)0.0401 (1)0.0138 (3)
O70.4710 (2)0.2660 (1)0.2233 (1)0.0225 (4)
O80.7085 (2)0.4885 (1)0.2831 (1)0.0179 (3)
O90.5446 (1)0.5739 (1)0.1162 (1)0.0132 (3)
O100.6422 (2)0.7255 (1)0.3551 (1)0.0193 (3)
O110.4782 (2)0.8122 (1)0.1877 (1)0.0198 (3)
O120.2404 (2)0.5991 (1)0.1089 (1)0.0176 (3)
O130.3961 (2)0.5080 (1)0.2739 (1)0.0173 (3)
O140.3319 (2)0.7523 (2)0.3546 (1)0.0284 (4)
O150.2600 (2)1.0422 (2)0.4521 (1)0.0290 (4)
O160.4808 (2)0.9312 (1)0.6652 (1)0.0291 (4)
O170.0608 (2)0.9448 (2)0.6432 (2)0.0303 (4)
O180.1555 (2)0.6484 (2)0.5706 (2)0.0383 (5)
O190.2580 (3)0.6177 (2)0.5676 (2)0.0551 (7)
O200.2060 (2)0.8305 (1)0.8840 (2)0.0298 (4)
O210.0552 (2)0.6102 (2)0.8107 (2)0.0285 (4)
O220.1331 (2)0.8813 (2)0.8537 (2)0.0358 (5)
O230.0669 (2)0.8304 (2)1.1090 (2)0.0321 (4)
Li10.0023 (5)0.7854 (4)0.9355 (4)0.034 (1)
H10.30401.11840.51600.032*
H20.33601.04240.41500.033*
H30.49310.99710.70870.034*
H40.49810.87010.69570.034*
H50.11171.02120.70000.034*
H60.02230.96210.61800.034*
H70.10000.58450.50050.047*
H80.21140.60550.61450.047*
H90.32780.57860.59930.069*
H100.32400.64630.52160.069*
H110.25810.90200.89850.038*
H120.27020.77700.89950.038*
H130.13880.56830.79070.039*
H140.00280.54530.82470.038*
H150.11770.96430.85200.043*
H160.22980.85530.83700.043*
H170.01500.80871.14750.041*
H180.12300.77881.12850.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0150 (2)0.0188 (2)0.0125 (2)0.0008 (1)0.0002 (1)0.0023 (1)
V20.0192 (2)0.0104 (2)0.0153 (2)0.0017 (1)0.0030 (1)0.0029 (1)
V30.0115 (2)0.0129 (2)0.0124 (2)0.0032 (1)0.0027 (1)0.0039 (1)
V40.0173 (2)0.0149 (2)0.0129 (2)0.0031 (1)0.0033 (1)0.0062 (1)
V50.0186 (2)0.0177 (2)0.0143 (2)0.0046 (1)0.0059 (1)0.0005 (1)
Na10.0260 (4)0.0274 (5)0.0239 (4)0.0056 (4)0.0081 (4)0.0052 (4)
Na20.0483 (6)0.0382 (6)0.0418 (6)0.0040 (5)0.0171 (5)0.0168 (5)
O10.0196 (7)0.0321 (9)0.0231 (8)0.0001 (6)0.0027 (6)0.0073 (7)
O20.0177 (7)0.0149 (6)0.0176 (7)0.0006 (5)0.0029 (5)0.0021 (5)
O30.0307 (8)0.0148 (7)0.0289 (8)0.0017 (6)0.0061 (7)0.0080 (6)
O40.0141 (6)0.0128 (6)0.0151 (6)0.0046 (5)0.0031 (5)0.0050 (5)
O50.0123 (6)0.0192 (7)0.0173 (7)0.0034 (5)0.0021 (5)0.0059 (5)
O60.0143 (6)0.0130 (6)0.0140 (6)0.0029 (5)0.0036 (5)0.0045 (5)
O70.0251 (7)0.0216 (7)0.0246 (8)0.0049 (6)0.0058 (6)0.0141 (6)
O80.0170 (7)0.0213 (7)0.0160 (7)0.0047 (5)0.0020 (5)0.0082 (6)
O90.0138 (7)0.0116 (6)0.0134 (6)0.0025 (5)0.0029 (5)0.0033 (5)
O100.0210 (7)0.0188 (7)0.0136 (6)0.0021 (5)0.0028 (5)0.0004 (5)
O110.0238 (7)0.0141 (6)0.0202 (7)0.0058 (5)0.0064 (6)0.0021 (5)
O120.0162 (6)0.0189 (7)0.0186 (7)0.0065 (5)0.0060 (5)0.0048 (6)
O130.0175 (6)0.0201 (7)0.0155 (7)0.0042 (5)0.0059 (5)0.0063 (5)
O140.0297 (8)0.0304 (8)0.0255 (8)0.0123 (7)0.0134 (7)0.0018 (7)
O150.0293 (8)0.0248 (8)0.0268 (8)0.0049 (6)0.0063 (7)0.0002 (7)
O160.0426 (9)0.0173 (7)0.0254 (8)0.0085 (7)0.0060 (7)0.0049 (6)
O170.0276 (8)0.0259 (8)0.0319 (9)0.0088 (7)0.0037 (7)0.0020 (7)
O180.044 (1)0.037 (1)0.0348 (9)0.0161 (8)0.0010 (8)0.0169 (8)
O190.050 (1)0.086 (2)0.035 (1)0.007 (1)0.0150 (9)0.031 (1)
O200.0211 (7)0.0196 (7)0.049 (1)0.0053 (6)0.0043 (7)0.0136 (7)
O210.0189 (7)0.0251 (8)0.046 (1)0.0050 (6)0.0105 (7)0.0176 (7)
O220.0222 (8)0.0317 (9)0.058 (1)0.0065 (7)0.0102 (8)0.0224 (8)
O230.0319 (8)0.0350 (9)0.0369 (9)0.0112 (7)0.0128 (7)0.0187 (7)
Li10.041 (2)0.032 (2)0.029 (2)0.011 (2)0.007 (2)0.007 (2)
Geometric parameters (Å, º) top
V1—O11.594 (1)Na1—O182.435 (2)
V1—O21.841 (2)Na2—O172.320 (2)
V1—O52.014 (2)Na2—O182.338 (2)
V1—O81.907 (2)Na2—O192.304 (2)
V1—O92.335 (1)Na2—O202.469 (2)
V1—O101.843 (2)Na2—O212.365 (2)
V2—O21.863 (1)Na2—O222.627 (2)
V2—O31.603 (2)O1—Na12.495 (2)
V2—O41.967 (1)O4—V41.983 (2)
V2—O62.024 (1)O5—V12.014 (2)
V2—O92.236 (1)O6—V22.024 (1)
V2—O111.799 (2)O9—V32.137 (1)
V3—O41.956 (2)Li1—O201.989 (5)
V3—O51.700 (1)Li1—O211.957 (4)
V3—O61.871 (2)Li1—O221.943 (5)
V3—O92.099 (1)Li1—O231.926 (5)
V3—O92.137 (1)O15—H10.9099
V3—O121.685 (2)O15—H20.8562
V4—O41.983 (2)O16—H30.7264
V4—O62.026 (1)O16—H40.8431
V4—O71.616 (2)O17—H50.8800
V4—O81.789 (1)O17—H60.7824
V4—O92.218 (2)O18—H70.9001
V4—O131.843 (2)O18—H80.8967
V5—O92.309 (1)O19—H90.8755
V5—O101.825 (1)O19—H100.8534
V5—O111.893 (2)O20—H110.7711
V5—O122.056 (1)O20—H120.8796
V5—O131.856 (2)O21—H130.7312
V5—O141.603 (2)O21—H140.9135
Na1—O12.495 (2)O22—H150.8778
Na1—O142.366 (2)O22—H160.7915
Na1—O152.349 (2)O23—H170.9425
Na1—O162.373 (2)O23—H180.8316
Na1—O172.391 (2)
O2—V1—O1102.45 (8)O14—V5—O10104.24 (7)
O5—V1—O1100.94 (8)O13—V5—O11154.19 (7)
O8—V1—O1102.70 (8)O12—V5—O1182.00 (6)
O9—V1—O1175.59 (7)O14—V5—O11101.34 (9)
O10—V1—O1103.37 (8)O13—V5—O1284.35 (6)
V1—O1—Na1165.3 (1)O14—V5—O1299.51 (7)
V1—O2—V2114.48 (7)O14—V5—O13102.45 (9)
O5—V1—O285.31 (7)V5—O14—Na1169.4 (1)
O8—V1—O2153.82 (5)O14—Na1—O182.08 (6)
O9—V1—O278.19 (5)O15—Na1—O1100.99 (7)
O10—V1—O292.30 (7)O16—Na1—O1165.59 (8)
V1—O5—V3111.64 (8)O17—Na1—O186.07 (6)
O8—V1—O582.89 (6)O18—Na1—O172.77 (7)
O9—V1—O574.72 (5)Na1—O1—V1165.3 (1)
O10—V1—O5155.51 (5)O15—Na1—O1485.26 (7)
V1—O8—V4115.07 (8)O16—Na1—O1495.90 (7)
O9—V1—O876.18 (5)O17—Na1—O14166.61 (7)
O10—V1—O888.91 (7)O18—Na1—O1495.67 (8)
V1—O9—V285.88 (4)O16—Na1—O1593.03 (6)
V1—O9—V386.84 (5)O17—Na1—O1590.94 (7)
V1—O9—V486.42 (5)O18—Na1—O15173.44 (7)
V1—O9—V582.99 (4)O17—Na1—O1697.12 (6)
O10—V1—O980.93 (5)O18—Na1—O1693.33 (7)
V1—O9—V3171.07 (7)Na1—O17—Na292.07 (7)
V1—O10—V5114.05 (7)O18—Na1—O1786.70 (8)
O6—V2—O287.81 (6)Na1—O18—Na290.55 (8)
O9—V2—O280.41 (6)O18—Na2—O1790.67 (8)
O11—V2—O294.26 (7)O19—Na2—O17111.36 (9)
O3—V2—O2102.12 (7)O20—Na2—O1793.17 (7)
O4—V2—O2154.70 (7)O21—Na2—O17157.35 (7)
O6—V2—O399.58 (8)O19—Na2—O1897.34 (8)
O9—V2—O3174.60 (7)O20—Na2—O1897.19 (7)
O11—V2—O3103.55 (8)O21—Na2—O18105.73 (8)
O4—V2—O3100.22 (7)O20—Na2—O19151.2 (1)
O6—V2—O476.86 (5)O21—Na2—O1982.45 (8)
O9—V2—O476.38 (5)O21—Na2—O2069.72 (6)
O11—V2—O491.90 (6)Na2—O20—Li178.1 (1)
V2—O4—V3107.18 (7)Na2—O21—Li181.3 (2)
V2—O4—V4101.48 (6)O1—Na1—O1482.08 (6)
V2—O6—V3108.35 (8)O1—Na1—O1786.07 (6)
O9—V2—O675.64 (6)O1—Na1—O1872.77 (7)
O11—V2—O6155.77 (7)O4—V4—O676.47 (6)
V2—O6—V498.10 (6)O4—V4—O799.44 (8)
V2—O9—V392.51 (6)O4—V4—O891.02 (6)
V2—O9—V4169.81 (6)O4—V4—O976.64 (6)
V2—O9—V586.37 (5)O5—V1—O285.31 (7)
O11—V2—O980.90 (6)O5—V1—O882.89 (6)
V2—O9—V393.43 (6)O5—V1—O974.72 (5)
V2—O11—V5114.80 (8)O5—V1—O1100.94 (8)
O9—V3—O479.93 (6)O6—V2—O287.81 (6)
V3—O4—V4107.56 (6)O6—V2—O476.86 (5)
O12—V3—O495.21 (7)O6—V2—O975.64 (6)
O5—V3—O494.93 (7)O6—V2—O399.58 (8)
O6—V3—O4155.49 (6)O9—V3—O586.65 (6)
O9—V3—O479.16 (6)O9—V3—O681.26 (6)
O9—V3—O5164.38 (7)O9—V3—O479.16 (6)
O12—V3—O5107.46 (7)O9—V3—O977.91 (5)
V3—O5—V1111.64 (8)O20—Li1—O2188.9 (2)
O6—V3—O598.51 (7)O20—Li1—O2299.3 (2)
O9—V3—O586.65 (6)O20—Li1—O23106.8 (2)
V3—O6—V4107.10 (6)O21—Li1—O22100.4 (2)
O9—V3—O681.67 (5)O21—Li1—O23129.9 (3)
O12—V3—O6100.14 (7)O22—Li1—O23122.3 (2)
V3—O6—V2108.35 (8)H1—Na1—O1498.0343
O9—V3—O681.26 (6)H2—Na1—O1470.1226
V3—O9—V3102.09 (5)H3—Na1—O14106.3757
V3—O9—V493.14 (5)H4—Na1—O1495.0635
V3—O9—V588.08 (5)H5—Na1—O14168.2916
O12—V3—O987.79 (6)H6—Na1—O14153.6421
O9—V3—O977.91 (5)H7—Na1—O1483.7865
V3—O9—V3102.09 (5)H8—Na1—O1493.9078
V3—O9—V493.72 (5)Na1—O15—H1111.2957
O12—V3—O9165.31 (5)Na1—O15—H2110.3156
V3—O9—V186.84 (5)Na1—O16—H3115.8861
V3—O9—V292.51 (6)Na1—O16—H4108.4384
V3—O12—V5109.79 (8)Na1—O17—H5114.6286
V4—O4—V3107.56 (6)Na1—O17—H6123.0022
O8—V4—O491.02 (6)Na1—O18—H7105.2909
O9—V4—O476.64 (6)Na1—O18—H8135.0490
O13—V4—O4155.32 (7)Na2—O17—H5121.5733
V4—O4—V2101.48 (6)Na2—O17—H6106.5964
O6—V4—O476.47 (6)Na2—O18—H7115.6120
O7—V4—O499.44 (8)Na2—O18—H8105.2500
O8—V4—O6155.88 (7)Na2—O19—H9119.8317
O9—V4—O675.49 (5)Na2—O19—H10122.8901
O13—V4—O688.26 (6)Na2—O20—H11114.8626
V4—O6—V298.10 (6)Na2—O20—H12117.0487
O7—V4—O698.78 (6)Na2—O21—H13113.1191
O8—V4—O7103.63 (7)Na2—O21—H14128.1757
O9—V4—O7173.61 (6)H2—O15—H1100.7962
O13—V4—O7102.00 (8)H4—O16—H3115.0966
O9—V4—O881.63 (6)H6—O17—H5100.3715
O13—V4—O895.63 (6)H8—O18—H7104.9681
V4—O9—V393.72 (5)H10—O19—H999.3271
V4—O9—V586.07 (5)H11—O20—Li1125.2203
O13—V4—O980.86 (7)H12—O20—Li1109.0020
V4—O13—V5113.31 (9)H12—O20—H11109.8595
V5—O9—V3169.83 (6)H13—O21—Li1121.3375
O10—V5—O982.03 (6)H14—O21—Li1118.6901
O11—V5—O977.09 (6)H14—O21—H1396.6409
O13—V5—O978.16 (6)H15—O22—Li1133.3027
O12—V5—O974.19 (5)H16—O22—Li1117.9284
O14—V5—O9173.62 (7)H16—O22—H15104.7859
O11—V5—O1091.00 (7)H18—O23—Li1109.6161
O13—V5—O1092.73 (7)H17—O23—Li1117.4397
O12—V5—O10156.14 (7)H18—O23—H1795.5975
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O15—H1···O10i0.911.842.749 (2)170
O15—H2···O16i0.852.012.864 (3)172
O16—H3···O11i0.722.012.738 (2)173
O16—H4···O7ii0.841.962.806 (3)175
O17—H5···O2i0.881.972.843 (2)169
O17—H6···O15iii0.782.012.782 (2)165
O18—H8···O8ii0.891.862.752 (3)168
O19—H9···O13iv0.872.092.913 (3)154
O19—H10···O10v0.852.333.069 (3)144
O20—H11···O3i0.772.002.765 (2)168
O20—H12···O4vi0.881.872.744 (2)172
O21—H13···O13iv0.732.112.828 (2)165
O21—H14···O5vi0.911.882.778 (2)166
O22—H15···O23vii0.872.052.919 (2)166
O22—H16···O7iv0.792.112.882 (2)164
O23—H17···O2viii0.941.872.789 (2)163
O23—H18···O12vi0.832.273.068 (2)159
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y+1, z+1; (iii) x, y+2, z+1; (iv) x, y+1, z+1; (v) x1, y, z; (vi) x, y, z+1; (vii) x, y+2, z+2; (viii) x1, y, z+1.
 

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