The crystal structure of the title compound, poly[deca-μ-aqua-octaaqua-μ-decavanadato-dilithium(I)tetrasodium(I)] [Li
2Na
4(H
2O)
18{V
10O
28}]
n, consists of polymeric chains composed of centrosymmetric [V
10O
28]
6− polyanions with
Ci symmetry linked by [LiNa
2(H
2O)
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 NaO
6 octahedra and one LiO
4 tetrahedron. Hydrogen bonds occur between the polyanion and the cation group, and within the cation group. Intrachain O
W—H
O hydrogen bonds stabilize the polymeric chain structure, while interchain O
W—H
O hydrogen bonds link neighbouring polymeric chains to form the complete supramolecular structure.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (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
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 = 1387.51 | F(000) = 684.00 |
Triclinic, P1 | Dx = 2.326 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.7107 Å |
a = 8.5386 (6) Å | Cell parameters from 5541 reflections |
b = 10.6333 (7) Å | θ = 2.5–27.5° |
c = 11.8912 (6) Å | µ = 2.42 mm−1 |
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-1 | Rint = 0.024 |
ω scans | θmax = 27.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −10→11 |
Tmin = 0.438, Tmax = 0.616 | k = −13→13 |
9308 measured reflections | l = −15→15 |
4471 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.027 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 1.02 | w = 1/[0.001Fo2 + σ(Fo2)]/(4Fo2) |
4467 reflections | (Δ/σ)max < 0.001 |
280 parameters | Δρmax = 0.48 e Å−3 |
Primary atom site location: structure-invariant direct methods | Δρmin = −0.52 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
V1 | 0.78731 (4) | 0.66163 (3) | 0.27151 (3) | 0.01683 (9) | |
V2 | 0.59589 (4) | 0.76990 (3) | 0.07942 (3) | 0.01567 (9) | |
V3 | 0.30870 (4) | 0.51024 (3) | −0.00358 (3) | 0.01229 (9) | |
V4 | 0.50849 (4) | 0.40158 (3) | 0.18695 (3) | 0.01479 (9) | |
V5 | 0.42980 (4) | 0.68105 (3) | 0.26387 (3) | 0.01749 (9) | |
Na1 | 0.2248 (1) | 0.85169 (9) | 0.51660 (8) | 0.0262 (2) | |
Na2 | −0.0062 (1) | 0.7475 (1) | 0.6890 (1) | 0.0418 (3) | |
O1 | 0.9595 (2) | 0.7141 (2) | 0.3711 (1) | 0.0272 (4) | |
O2 | 0.7894 (2) | 0.7920 (1) | 0.1962 (1) | 0.0182 (3) | |
O3 | 0.6315 (2) | 0.9024 (1) | 0.0402 (1) | 0.0252 (4) | |
O4 | 0.3971 (2) | 0.6651 (1) | −0.0493 (1) | 0.0138 (3) | |
O5 | 0.1470 (2) | 0.4454 (1) | −0.1285 (1) | 0.0165 (3) | |
O6 | 0.3151 (2) | 0.3544 (1) | 0.0401 (1) | 0.0138 (3) | |
O7 | 0.4710 (2) | 0.2660 (1) | 0.2233 (1) | 0.0225 (4) | |
O8 | 0.7085 (2) | 0.4885 (1) | 0.2831 (1) | 0.0179 (3) | |
O9 | 0.5446 (1) | 0.5739 (1) | 0.1162 (1) | 0.0132 (3) | |
O10 | 0.6422 (2) | 0.7255 (1) | 0.3551 (1) | 0.0193 (3) | |
O11 | 0.4782 (2) | 0.8122 (1) | 0.1877 (1) | 0.0198 (3) | |
O12 | 0.2404 (2) | 0.5991 (1) | 0.1089 (1) | 0.0176 (3) | |
O13 | 0.3961 (2) | 0.5080 (1) | 0.2739 (1) | 0.0173 (3) | |
O14 | 0.3319 (2) | 0.7523 (2) | 0.3546 (1) | 0.0284 (4) | |
O15 | 0.2600 (2) | 1.0422 (2) | 0.4521 (1) | 0.0290 (4) | |
O16 | 0.4808 (2) | 0.9312 (1) | 0.6652 (1) | 0.0291 (4) | |
O17 | 0.0608 (2) | 0.9448 (2) | 0.6432 (2) | 0.0303 (4) | |
O18 | 0.1555 (2) | 0.6484 (2) | 0.5706 (2) | 0.0383 (5) | |
O19 | −0.2580 (3) | 0.6177 (2) | 0.5676 (2) | 0.0551 (7) | |
O20 | 0.2060 (2) | 0.8305 (1) | 0.8840 (2) | 0.0298 (4) | |
O21 | −0.0552 (2) | 0.6102 (2) | 0.8107 (2) | 0.0285 (4) | |
O22 | −0.1331 (2) | 0.8813 (2) | 0.8537 (2) | 0.0358 (5) | |
O23 | 0.0669 (2) | 0.8304 (2) | 1.1090 (2) | 0.0321 (4) | |
Li1 | 0.0023 (5) | 0.7854 (4) | 0.9355 (4) | 0.034 (1) | |
H1 | 0.3040 | 1.1184 | 0.5160 | 0.032* | |
H2 | 0.3360 | 1.0424 | 0.4150 | 0.033* | |
H3 | 0.4931 | 0.9971 | 0.7087 | 0.034* | |
H4 | 0.4981 | 0.8701 | 0.6957 | 0.034* | |
H5 | 0.1117 | 1.0212 | 0.7000 | 0.034* | |
H6 | −0.0223 | 0.9621 | 0.6180 | 0.034* | |
H7 | 0.1000 | 0.5845 | 0.5005 | 0.047* | |
H8 | 0.2114 | 0.6055 | 0.6145 | 0.047* | |
H9 | −0.3278 | 0.5786 | 0.5993 | 0.069* | |
H10 | −0.3240 | 0.6463 | 0.5216 | 0.069* | |
H11 | 0.2581 | 0.9020 | 0.8985 | 0.038* | |
H12 | 0.2702 | 0.7770 | 0.8995 | 0.038* | |
H13 | −0.1388 | 0.5683 | 0.7907 | 0.039* | |
H14 | −0.0028 | 0.5453 | 0.8247 | 0.038* | |
H15 | −0.1177 | 0.9643 | 0.8520 | 0.043* | |
H16 | −0.2298 | 0.8553 | 0.8370 | 0.043* | |
H17 | −0.0150 | 0.8087 | 1.1475 | 0.041* | |
H18 | 0.1230 | 0.7788 | 1.1285 | 0.041* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0150 (2) | 0.0188 (2) | 0.0125 (2) | 0.0008 (1) | 0.0002 (1) | 0.0023 (1) |
V2 | 0.0192 (2) | 0.0104 (2) | 0.0153 (2) | 0.0017 (1) | 0.0030 (1) | 0.0029 (1) |
V3 | 0.0115 (2) | 0.0129 (2) | 0.0124 (2) | 0.0032 (1) | 0.0027 (1) | 0.0039 (1) |
V4 | 0.0173 (2) | 0.0149 (2) | 0.0129 (2) | 0.0031 (1) | 0.0033 (1) | 0.0062 (1) |
V5 | 0.0186 (2) | 0.0177 (2) | 0.0143 (2) | 0.0046 (1) | 0.0059 (1) | 0.0005 (1) |
Na1 | 0.0260 (4) | 0.0274 (5) | 0.0239 (4) | 0.0056 (4) | 0.0081 (4) | 0.0052 (4) |
Na2 | 0.0483 (6) | 0.0382 (6) | 0.0418 (6) | 0.0040 (5) | 0.0171 (5) | 0.0168 (5) |
O1 | 0.0196 (7) | 0.0321 (9) | 0.0231 (8) | −0.0001 (6) | −0.0027 (6) | 0.0073 (7) |
O2 | 0.0177 (7) | 0.0149 (6) | 0.0176 (7) | −0.0006 (5) | 0.0029 (5) | 0.0021 (5) |
O3 | 0.0307 (8) | 0.0148 (7) | 0.0289 (8) | 0.0017 (6) | 0.0061 (7) | 0.0080 (6) |
O4 | 0.0141 (6) | 0.0128 (6) | 0.0151 (6) | 0.0046 (5) | 0.0031 (5) | 0.0050 (5) |
O5 | 0.0123 (6) | 0.0192 (7) | 0.0173 (7) | 0.0034 (5) | 0.0021 (5) | 0.0059 (5) |
O6 | 0.0143 (6) | 0.0130 (6) | 0.0140 (6) | 0.0029 (5) | 0.0036 (5) | 0.0045 (5) |
O7 | 0.0251 (7) | 0.0216 (7) | 0.0246 (8) | 0.0049 (6) | 0.0058 (6) | 0.0141 (6) |
O8 | 0.0170 (7) | 0.0213 (7) | 0.0160 (7) | 0.0047 (5) | 0.0020 (5) | 0.0082 (6) |
O9 | 0.0138 (7) | 0.0116 (6) | 0.0134 (6) | 0.0025 (5) | 0.0029 (5) | 0.0033 (5) |
O10 | 0.0210 (7) | 0.0188 (7) | 0.0136 (6) | 0.0021 (5) | 0.0028 (5) | 0.0004 (5) |
O11 | 0.0238 (7) | 0.0141 (6) | 0.0202 (7) | 0.0058 (5) | 0.0064 (6) | 0.0021 (5) |
O12 | 0.0162 (6) | 0.0189 (7) | 0.0186 (7) | 0.0065 (5) | 0.0060 (5) | 0.0048 (6) |
O13 | 0.0175 (6) | 0.0201 (7) | 0.0155 (7) | 0.0042 (5) | 0.0059 (5) | 0.0063 (5) |
O14 | 0.0297 (8) | 0.0304 (8) | 0.0255 (8) | 0.0123 (7) | 0.0134 (7) | 0.0018 (7) |
O15 | 0.0293 (8) | 0.0248 (8) | 0.0268 (8) | 0.0049 (6) | 0.0063 (7) | −0.0002 (7) |
O16 | 0.0426 (9) | 0.0173 (7) | 0.0254 (8) | 0.0085 (7) | 0.0060 (7) | 0.0049 (6) |
O17 | 0.0276 (8) | 0.0259 (8) | 0.0319 (9) | 0.0088 (7) | 0.0037 (7) | 0.0020 (7) |
O18 | 0.044 (1) | 0.037 (1) | 0.0348 (9) | 0.0161 (8) | −0.0010 (8) | 0.0169 (8) |
O19 | 0.050 (1) | 0.086 (2) | 0.035 (1) | 0.007 (1) | 0.0150 (9) | 0.031 (1) |
O20 | 0.0211 (7) | 0.0196 (7) | 0.049 (1) | 0.0053 (6) | 0.0043 (7) | 0.0136 (7) |
O21 | 0.0189 (7) | 0.0251 (8) | 0.046 (1) | 0.0050 (6) | 0.0105 (7) | 0.0176 (7) |
O22 | 0.0222 (8) | 0.0317 (9) | 0.058 (1) | 0.0065 (7) | 0.0102 (8) | 0.0224 (8) |
O23 | 0.0319 (8) | 0.0350 (9) | 0.0369 (9) | 0.0112 (7) | 0.0128 (7) | 0.0187 (7) |
Li1 | 0.041 (2) | 0.032 (2) | 0.029 (2) | 0.011 (2) | 0.007 (2) | 0.007 (2) |
Geometric parameters (Å, º) top
V1—O1 | 1.594 (1) | Na1—O18 | 2.435 (2) |
V1—O2 | 1.841 (2) | Na2—O17 | 2.320 (2) |
V1—O5 | 2.014 (2) | Na2—O18 | 2.338 (2) |
V1—O8 | 1.907 (2) | Na2—O19 | 2.304 (2) |
V1—O9 | 2.335 (1) | Na2—O20 | 2.469 (2) |
V1—O10 | 1.843 (2) | Na2—O21 | 2.365 (2) |
V2—O2 | 1.863 (1) | Na2—O22 | 2.627 (2) |
V2—O3 | 1.603 (2) | O1—Na1 | 2.495 (2) |
V2—O4 | 1.967 (1) | O4—V4 | 1.983 (2) |
V2—O6 | 2.024 (1) | O5—V1 | 2.014 (2) |
V2—O9 | 2.236 (1) | O6—V2 | 2.024 (1) |
V2—O11 | 1.799 (2) | O9—V3 | 2.137 (1) |
V3—O4 | 1.956 (2) | Li1—O20 | 1.989 (5) |
V3—O5 | 1.700 (1) | Li1—O21 | 1.957 (4) |
V3—O6 | 1.871 (2) | Li1—O22 | 1.943 (5) |
V3—O9 | 2.099 (1) | Li1—O23 | 1.926 (5) |
V3—O9 | 2.137 (1) | O15—H1 | 0.9099 |
V3—O12 | 1.685 (2) | O15—H2 | 0.8562 |
V4—O4 | 1.983 (2) | O16—H3 | 0.7264 |
V4—O6 | 2.026 (1) | O16—H4 | 0.8431 |
V4—O7 | 1.616 (2) | O17—H5 | 0.8800 |
V4—O8 | 1.789 (1) | O17—H6 | 0.7824 |
V4—O9 | 2.218 (2) | O18—H7 | 0.9001 |
V4—O13 | 1.843 (2) | O18—H8 | 0.8967 |
V5—O9 | 2.309 (1) | O19—H9 | 0.8755 |
V5—O10 | 1.825 (1) | O19—H10 | 0.8534 |
V5—O11 | 1.893 (2) | O20—H11 | 0.7711 |
V5—O12 | 2.056 (1) | O20—H12 | 0.8796 |
V5—O13 | 1.856 (2) | O21—H13 | 0.7312 |
V5—O14 | 1.603 (2) | O21—H14 | 0.9135 |
Na1—O1 | 2.495 (2) | O22—H15 | 0.8778 |
Na1—O14 | 2.366 (2) | O22—H16 | 0.7915 |
Na1—O15 | 2.349 (2) | O23—H17 | 0.9425 |
Na1—O16 | 2.373 (2) | O23—H18 | 0.8316 |
Na1—O17 | 2.391 (2) | | |
| | | |
O2—V1—O1 | 102.45 (8) | O14—V5—O10 | 104.24 (7) |
O5—V1—O1 | 100.94 (8) | O13—V5—O11 | 154.19 (7) |
O8—V1—O1 | 102.70 (8) | O12—V5—O11 | 82.00 (6) |
O9—V1—O1 | 175.59 (7) | O14—V5—O11 | 101.34 (9) |
O10—V1—O1 | 103.37 (8) | O13—V5—O12 | 84.35 (6) |
V1—O1—Na1 | 165.3 (1) | O14—V5—O12 | 99.51 (7) |
V1—O2—V2 | 114.48 (7) | O14—V5—O13 | 102.45 (9) |
O5—V1—O2 | 85.31 (7) | V5—O14—Na1 | 169.4 (1) |
O8—V1—O2 | 153.82 (5) | O14—Na1—O1 | 82.08 (6) |
O9—V1—O2 | 78.19 (5) | O15—Na1—O1 | 100.99 (7) |
O10—V1—O2 | 92.30 (7) | O16—Na1—O1 | 165.59 (8) |
V1—O5—V3 | 111.64 (8) | O17—Na1—O1 | 86.07 (6) |
O8—V1—O5 | 82.89 (6) | O18—Na1—O1 | 72.77 (7) |
O9—V1—O5 | 74.72 (5) | Na1—O1—V1 | 165.3 (1) |
O10—V1—O5 | 155.51 (5) | O15—Na1—O14 | 85.26 (7) |
V1—O8—V4 | 115.07 (8) | O16—Na1—O14 | 95.90 (7) |
O9—V1—O8 | 76.18 (5) | O17—Na1—O14 | 166.61 (7) |
O10—V1—O8 | 88.91 (7) | O18—Na1—O14 | 95.67 (8) |
V1—O9—V2 | 85.88 (4) | O16—Na1—O15 | 93.03 (6) |
V1—O9—V3 | 86.84 (5) | O17—Na1—O15 | 90.94 (7) |
V1—O9—V4 | 86.42 (5) | O18—Na1—O15 | 173.44 (7) |
V1—O9—V5 | 82.99 (4) | O17—Na1—O16 | 97.12 (6) |
O10—V1—O9 | 80.93 (5) | O18—Na1—O16 | 93.33 (7) |
V1—O9—V3 | 171.07 (7) | Na1—O17—Na2 | 92.07 (7) |
V1—O10—V5 | 114.05 (7) | O18—Na1—O17 | 86.70 (8) |
O6—V2—O2 | 87.81 (6) | Na1—O18—Na2 | 90.55 (8) |
O9—V2—O2 | 80.41 (6) | O18—Na2—O17 | 90.67 (8) |
O11—V2—O2 | 94.26 (7) | O19—Na2—O17 | 111.36 (9) |
O3—V2—O2 | 102.12 (7) | O20—Na2—O17 | 93.17 (7) |
O4—V2—O2 | 154.70 (7) | O21—Na2—O17 | 157.35 (7) |
O6—V2—O3 | 99.58 (8) | O19—Na2—O18 | 97.34 (8) |
O9—V2—O3 | 174.60 (7) | O20—Na2—O18 | 97.19 (7) |
O11—V2—O3 | 103.55 (8) | O21—Na2—O18 | 105.73 (8) |
O4—V2—O3 | 100.22 (7) | O20—Na2—O19 | 151.2 (1) |
O6—V2—O4 | 76.86 (5) | O21—Na2—O19 | 82.45 (8) |
O9—V2—O4 | 76.38 (5) | O21—Na2—O20 | 69.72 (6) |
O11—V2—O4 | 91.90 (6) | Na2—O20—Li1 | 78.1 (1) |
V2—O4—V3 | 107.18 (7) | Na2—O21—Li1 | 81.3 (2) |
V2—O4—V4 | 101.48 (6) | O1—Na1—O14 | 82.08 (6) |
V2—O6—V3 | 108.35 (8) | O1—Na1—O17 | 86.07 (6) |
O9—V2—O6 | 75.64 (6) | O1—Na1—O18 | 72.77 (7) |
O11—V2—O6 | 155.77 (7) | O4—V4—O6 | 76.47 (6) |
V2—O6—V4 | 98.10 (6) | O4—V4—O7 | 99.44 (8) |
V2—O9—V3 | 92.51 (6) | O4—V4—O8 | 91.02 (6) |
V2—O9—V4 | 169.81 (6) | O4—V4—O9 | 76.64 (6) |
V2—O9—V5 | 86.37 (5) | O5—V1—O2 | 85.31 (7) |
O11—V2—O9 | 80.90 (6) | O5—V1—O8 | 82.89 (6) |
V2—O9—V3 | 93.43 (6) | O5—V1—O9 | 74.72 (5) |
V2—O11—V5 | 114.80 (8) | O5—V1—O1 | 100.94 (8) |
O9—V3—O4 | 79.93 (6) | O6—V2—O2 | 87.81 (6) |
V3—O4—V4 | 107.56 (6) | O6—V2—O4 | 76.86 (5) |
O12—V3—O4 | 95.21 (7) | O6—V2—O9 | 75.64 (6) |
O5—V3—O4 | 94.93 (7) | O6—V2—O3 | 99.58 (8) |
O6—V3—O4 | 155.49 (6) | O9—V3—O5 | 86.65 (6) |
O9—V3—O4 | 79.16 (6) | O9—V3—O6 | 81.26 (6) |
O9—V3—O5 | 164.38 (7) | O9—V3—O4 | 79.16 (6) |
O12—V3—O5 | 107.46 (7) | O9—V3—O9 | 77.91 (5) |
V3—O5—V1 | 111.64 (8) | O20—Li1—O21 | 88.9 (2) |
O6—V3—O5 | 98.51 (7) | O20—Li1—O22 | 99.3 (2) |
O9—V3—O5 | 86.65 (6) | O20—Li1—O23 | 106.8 (2) |
V3—O6—V4 | 107.10 (6) | O21—Li1—O22 | 100.4 (2) |
O9—V3—O6 | 81.67 (5) | O21—Li1—O23 | 129.9 (3) |
O12—V3—O6 | 100.14 (7) | O22—Li1—O23 | 122.3 (2) |
V3—O6—V2 | 108.35 (8) | H1—Na1—O14 | 98.0343 |
O9—V3—O6 | 81.26 (6) | H2—Na1—O14 | 70.1226 |
V3—O9—V3 | 102.09 (5) | H3—Na1—O14 | 106.3757 |
V3—O9—V4 | 93.14 (5) | H4—Na1—O14 | 95.0635 |
V3—O9—V5 | 88.08 (5) | H5—Na1—O14 | 168.2916 |
O12—V3—O9 | 87.79 (6) | H6—Na1—O14 | 153.6421 |
O9—V3—O9 | 77.91 (5) | H7—Na1—O14 | 83.7865 |
V3—O9—V3 | 102.09 (5) | H8—Na1—O14 | 93.9078 |
V3—O9—V4 | 93.72 (5) | Na1—O15—H1 | 111.2957 |
O12—V3—O9 | 165.31 (5) | Na1—O15—H2 | 110.3156 |
V3—O9—V1 | 86.84 (5) | Na1—O16—H3 | 115.8861 |
V3—O9—V2 | 92.51 (6) | Na1—O16—H4 | 108.4384 |
V3—O12—V5 | 109.79 (8) | Na1—O17—H5 | 114.6286 |
V4—O4—V3 | 107.56 (6) | Na1—O17—H6 | 123.0022 |
O8—V4—O4 | 91.02 (6) | Na1—O18—H7 | 105.2909 |
O9—V4—O4 | 76.64 (6) | Na1—O18—H8 | 135.0490 |
O13—V4—O4 | 155.32 (7) | Na2—O17—H5 | 121.5733 |
V4—O4—V2 | 101.48 (6) | Na2—O17—H6 | 106.5964 |
O6—V4—O4 | 76.47 (6) | Na2—O18—H7 | 115.6120 |
O7—V4—O4 | 99.44 (8) | Na2—O18—H8 | 105.2500 |
O8—V4—O6 | 155.88 (7) | Na2—O19—H9 | 119.8317 |
O9—V4—O6 | 75.49 (5) | Na2—O19—H10 | 122.8901 |
O13—V4—O6 | 88.26 (6) | Na2—O20—H11 | 114.8626 |
V4—O6—V2 | 98.10 (6) | Na2—O20—H12 | 117.0487 |
O7—V4—O6 | 98.78 (6) | Na2—O21—H13 | 113.1191 |
O8—V4—O7 | 103.63 (7) | Na2—O21—H14 | 128.1757 |
O9—V4—O7 | 173.61 (6) | H2—O15—H1 | 100.7962 |
O13—V4—O7 | 102.00 (8) | H4—O16—H3 | 115.0966 |
O9—V4—O8 | 81.63 (6) | H6—O17—H5 | 100.3715 |
O13—V4—O8 | 95.63 (6) | H8—O18—H7 | 104.9681 |
V4—O9—V3 | 93.72 (5) | H10—O19—H9 | 99.3271 |
V4—O9—V5 | 86.07 (5) | H11—O20—Li1 | 125.2203 |
O13—V4—O9 | 80.86 (7) | H12—O20—Li1 | 109.0020 |
V4—O13—V5 | 113.31 (9) | H12—O20—H11 | 109.8595 |
V5—O9—V3 | 169.83 (6) | H13—O21—Li1 | 121.3375 |
O10—V5—O9 | 82.03 (6) | H14—O21—Li1 | 118.6901 |
O11—V5—O9 | 77.09 (6) | H14—O21—H13 | 96.6409 |
O13—V5—O9 | 78.16 (6) | H15—O22—Li1 | 133.3027 |
O12—V5—O9 | 74.19 (5) | H16—O22—Li1 | 117.9284 |
O14—V5—O9 | 173.62 (7) | H16—O22—H15 | 104.7859 |
O11—V5—O10 | 91.00 (7) | H18—O23—Li1 | 109.6161 |
O13—V5—O10 | 92.73 (7) | H17—O23—Li1 | 117.4397 |
O12—V5—O10 | 156.14 (7) | H18—O23—H17 | 95.5975 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O15—H1···O10i | 0.91 | 1.84 | 2.749 (2) | 170 |
O15—H2···O16i | 0.85 | 2.01 | 2.864 (3) | 172 |
O16—H3···O11i | 0.72 | 2.01 | 2.738 (2) | 173 |
O16—H4···O7ii | 0.84 | 1.96 | 2.806 (3) | 175 |
O17—H5···O2i | 0.88 | 1.97 | 2.843 (2) | 169 |
O17—H6···O15iii | 0.78 | 2.01 | 2.782 (2) | 165 |
O18—H8···O8ii | 0.89 | 1.86 | 2.752 (3) | 168 |
O19—H9···O13iv | 0.87 | 2.09 | 2.913 (3) | 154 |
O19—H10···O10v | 0.85 | 2.33 | 3.069 (3) | 144 |
O20—H11···O3i | 0.77 | 2.00 | 2.765 (2) | 168 |
O20—H12···O4vi | 0.88 | 1.87 | 2.744 (2) | 172 |
O21—H13···O13iv | 0.73 | 2.11 | 2.828 (2) | 165 |
O21—H14···O5vi | 0.91 | 1.88 | 2.778 (2) | 166 |
O22—H15···O23vii | 0.87 | 2.05 | 2.919 (2) | 166 |
O22—H16···O7iv | 0.79 | 2.11 | 2.882 (2) | 164 |
O23—H17···O2viii | 0.94 | 1.87 | 2.789 (2) | 163 |
O23—H18···O12vi | 0.83 | 2.27 | 3.068 (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) x−1, y, z; (vi) x, y, z+1; (vii) −x, −y+2, −z+2; (viii) x−1, y, z+1. |