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In the title compound, the centrosymmetric polyanion consists of ten VO
6 edge-sharing distorted octahedra. Each of the two Li
+ cations is surrounded by six water molecules in a distorted octahedral arrangement. The V
V distances are in the range 3.078 (5)–3.101 (5) Å and the four types of V—O bond lengths are in the range 1.601 (2)–2.361 (2) Å. The title compound is isostructural with (NH
4)
4Na
2[V
10O
28]·10H
2O and K
4Na
2[V
10O
28]·10H
2O. It provides the first example of a decavanadate salt of a lithium cation.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (V-O) = 0.002 Å
- R factor = 0.030
- wR factor = 0.093
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT480_ALERT_4_C Long H...A H-Bond Reported H6 .. O14 .. 2.62 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 5
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
H4 N
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5
H2 O
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. # 7
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 8
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 9
Li
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
10 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
9 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.
Crystal data top
(NH4)4Li2[V10O28]·10H2O | Z = 1 |
Mr = 1223.61 | F(000) = 604 |
Triclinic, P1 | Dx = 2.439 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.523 (2) Å | Cell parameters from 25 reflections |
b = 10.272 (2) Å | θ = 2–27° |
c = 11.110 (2) Å | µ = 2.80 mm−1 |
α = 68.42 (2)° | T = 293 K |
β = 87.05 (2)° | Hexagonal, orange |
γ = 67.80 (2)° | 0.58 × 0.29 × 0.14 mm |
V = 833.1 (3) Å3 | |
Data collection top
Diffractomètre CAD-4 | 3387 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.002 |
Graphite monochromator | θmax = 27.0°, θmin = 2.0° |
ω/2θ scans | h = −10→0 |
Absorption correction: ψ scan (North et al., 1968) | k = −13→12 |
Tmin = 0.392, Tmax = 0.676 | l = −14→14 |
7758 measured reflections | 2 standard reflections every 120 min |
3628 independent reflections | intensity decay: 1% |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.093 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0537P)2 + 0.7843P] where P = (Fo2 + 2Fc2)/3 |
3628 reflections | (Δ/σ)max = 0.004 |
298 parameters | Δρmax = 0.73 e Å−3 |
27 restraints | Δρmin = −0.66 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
V3 | −0.03155 (5) | 0.20246 (4) | 0.76577 (4) | 0.01855 (12) | |
V5 | −0.19029 (4) | 0.49582 (4) | 0.51993 (3) | 0.01428 (11) | |
V1 | −0.02585 (5) | 0.50699 (4) | 0.25496 (4) | 0.01668 (11) | |
V2 | 0.12201 (5) | 0.21415 (4) | 0.50094 (4) | 0.01760 (11) | |
V4 | 0.32561 (5) | 0.21174 (4) | 0.72571 (4) | 0.01966 (12) | |
O14 | 0.1543 (2) | 0.11711 (19) | 0.40905 (18) | 0.0265 (4) | |
O13 | 0.0062 (2) | 0.4034 (2) | 0.16808 (17) | 0.0255 (4) | |
O11 | −0.1150 (2) | 0.0954 (2) | 0.86590 (18) | 0.0283 (4) | |
O12 | 0.5177 (2) | 0.1143 (2) | 0.79525 (19) | 0.0307 (4) | |
O7 | 0.0146 (2) | 0.12448 (18) | 0.63355 (16) | 0.0196 (3) | |
O9 | −0.2405 (2) | 0.36342 (18) | 0.64300 (15) | 0.0181 (3) | |
O6 | −0.2477 (2) | 0.63680 (18) | 0.20142 (16) | 0.0200 (3) | |
O8 | 0.3274 (2) | 0.13104 (18) | 0.59840 (16) | 0.0214 (3) | |
O10 | −0.3738 (2) | 0.62103 (18) | 0.42493 (16) | 0.0196 (3) | |
O5 | −0.0629 (2) | 0.35420 (18) | 0.83419 (15) | 0.0195 (3) | |
O4 | 0.1983 (2) | 0.11273 (18) | 0.82694 (16) | 0.0211 (3) | |
O2 | −0.1040 (2) | 0.37831 (17) | 0.41414 (15) | 0.0161 (3) | |
O3 | −0.1837 (2) | 0.61531 (17) | 0.61806 (15) | 0.0160 (3) | |
O1 | 0.06631 (18) | 0.37359 (17) | 0.60696 (15) | 0.0151 (3) | |
OW1 | −0.3151 (3) | 0.4887 (3) | 0.9863 (2) | 0.0353 (5) | |
H1 | −0.252 (4) | 0.438 (4) | 0.947 (3) | 0.042* | |
H2 | −0.261 (4) | 0.507 (4) | 1.031 (3) | 0.042* | |
OW2 | −0.4780 (3) | 0.4875 (3) | 0.2343 (2) | 0.0390 (5) | |
H3 | −0.559 (3) | 0.532 (4) | 0.268 (3) | 0.047* | |
H4 | −0.407 (4) | 0.527 (4) | 0.222 (4) | 0.047* | |
OW3 | 0.1814 (3) | −0.1963 (2) | 0.7628 (3) | 0.0423 (5) | |
H5 | 0.121 (4) | −0.103 (2) | 0.735 (4) | 0.051* | |
H6 | 0.114 (4) | −0.237 (3) | 0.760 (4) | 0.051* | |
OW4 | −0.4618 (3) | 0.8005 (3) | 0.7201 (2) | 0.0408 (5) | |
H7 | −0.503 (4) | 0.890 (2) | 0.681 (3) | 0.049* | |
H8 | −0.386 (4) | 0.752 (3) | 0.688 (3) | 0.049* | |
OW5 | 0.4213 (3) | −0.1985 (3) | 0.9710 (2) | 0.0405 (5) | |
H9 | 0.338 (4) | −0.118 (3) | 0.943 (3) | 0.049* | |
H10 | 0.408 (4) | −0.255 (3) | 1.040 (2) | 0.049* | |
N1 | 0.3241 (3) | −0.2048 (3) | 0.5094 (2) | 0.0289 (5) | |
H11 | 0.265 (4) | −0.113 (2) | 0.468 (3) | 0.035* | |
H12 | 0.389 (4) | −0.252 (3) | 0.467 (3) | 0.035* | |
H13 | 0.367 (4) | −0.201 (4) | 0.573 (2) | 0.035* | |
H14 | 0.245 (3) | −0.232 (4) | 0.537 (3) | 0.035* | |
N2 | 0.2246 (4) | 0.1773 (3) | 0.0729 (2) | 0.0344 (5) | |
H15 | 0.225 (5) | 0.095 (3) | 0.116 (3) | 0.041* | |
H16 | 0.164 (4) | 0.233 (4) | 0.106 (3) | 0.041* | |
H17 | 0.174 (4) | 0.221 (4) | 0.003 (2) | 0.041* | |
H18 | 0.318 (3) | 0.178 (4) | 0.073 (4) | 0.041* | |
Li1 | 0.4379 (6) | −0.3405 (5) | 0.8726 (4) | 0.0273 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V3 | 0.0207 (2) | 0.0161 (2) | 0.0179 (2) | −0.00739 (15) | 0.00407 (15) | −0.00536 (15) |
V5 | 0.01371 (19) | 0.01311 (19) | 0.0165 (2) | −0.00430 (15) | 0.00384 (14) | −0.00729 (15) |
V1 | 0.0209 (2) | 0.01531 (19) | 0.0149 (2) | −0.00545 (15) | 0.00336 (15) | −0.00870 (15) |
V2 | 0.0222 (2) | 0.01204 (19) | 0.0186 (2) | −0.00405 (15) | 0.00439 (15) | −0.00874 (15) |
V4 | 0.0169 (2) | 0.0162 (2) | 0.0210 (2) | −0.00284 (15) | 0.00000 (15) | −0.00517 (16) |
O14 | 0.0346 (10) | 0.0180 (8) | 0.0287 (9) | −0.0069 (7) | 0.0063 (8) | −0.0146 (7) |
O13 | 0.0344 (10) | 0.0255 (9) | 0.0224 (8) | −0.0111 (8) | 0.0063 (7) | −0.0161 (7) |
O11 | 0.0333 (10) | 0.0253 (9) | 0.0259 (9) | −0.0162 (8) | 0.0075 (7) | −0.0049 (7) |
O12 | 0.0218 (9) | 0.0259 (9) | 0.0354 (10) | −0.0016 (7) | −0.0042 (7) | −0.0086 (8) |
O7 | 0.0239 (8) | 0.0137 (7) | 0.0214 (8) | −0.0072 (6) | 0.0037 (6) | −0.0070 (6) |
O9 | 0.0183 (8) | 0.0173 (8) | 0.0194 (8) | −0.0072 (6) | 0.0048 (6) | −0.0076 (6) |
O6 | 0.0215 (8) | 0.0184 (8) | 0.0194 (8) | −0.0063 (6) | 0.0005 (6) | −0.0074 (6) |
O8 | 0.0204 (8) | 0.0145 (7) | 0.0250 (8) | −0.0011 (6) | 0.0029 (6) | −0.0087 (6) |
O10 | 0.0154 (7) | 0.0189 (8) | 0.0226 (8) | −0.0041 (6) | 0.0020 (6) | −0.0085 (7) |
O5 | 0.0240 (8) | 0.0186 (8) | 0.0159 (7) | −0.0078 (6) | 0.0057 (6) | −0.0073 (6) |
O4 | 0.0230 (8) | 0.0162 (8) | 0.0190 (8) | −0.0048 (6) | 0.0008 (6) | −0.0037 (6) |
O2 | 0.0175 (7) | 0.0144 (7) | 0.0181 (7) | −0.0061 (6) | 0.0031 (6) | −0.0082 (6) |
O3 | 0.0171 (7) | 0.0140 (7) | 0.0168 (7) | −0.0038 (6) | 0.0047 (6) | −0.0081 (6) |
O1 | 0.0169 (8) | 0.0128 (7) | 0.0161 (7) | −0.0047 (6) | 0.0040 (6) | −0.0076 (6) |
OW1 | 0.0331 (11) | 0.0443 (12) | 0.0338 (11) | −0.0132 (10) | 0.0087 (9) | −0.0230 (10) |
OW2 | 0.0328 (11) | 0.0545 (14) | 0.0522 (13) | −0.0233 (10) | 0.0210 (10) | −0.0401 (12) |
OW3 | 0.0409 (12) | 0.0234 (10) | 0.0587 (15) | −0.0102 (9) | −0.0017 (11) | −0.0129 (10) |
OW4 | 0.0397 (12) | 0.0358 (11) | 0.0462 (13) | −0.0139 (10) | 0.0227 (10) | −0.0178 (10) |
OW5 | 0.0469 (13) | 0.0354 (12) | 0.0274 (10) | −0.0041 (10) | 0.0036 (9) | −0.0112 (9) |
N1 | 0.0274 (12) | 0.0274 (11) | 0.0360 (13) | −0.0082 (9) | 0.0039 (10) | −0.0188 (10) |
N2 | 0.0430 (14) | 0.0252 (12) | 0.0261 (12) | −0.0018 (11) | 0.0006 (11) | −0.0115 (10) |
Li1 | 0.032 (2) | 0.024 (2) | 0.032 (2) | −0.0138 (18) | 0.0086 (18) | −0.0145 (18) |
Geometric parameters (Å, º) top
V3—O11 | 1.6009 (18) | O10—V4i | 2.0659 (18) |
V3—O4 | 1.8601 (18) | O5—V1i | 1.8127 (17) |
V3—O7 | 1.8768 (17) | O3—V2i | 2.0036 (17) |
V3—O5 | 1.9012 (17) | O3—V1i | 2.0048 (18) |
V3—O9 | 2.0328 (18) | O1—V5i | 2.1048 (16) |
V3—O1 | 2.3609 (17) | O1—V1i | 2.2333 (15) |
V3—V4 | 3.0858 (9) | OW1—Li1ii | 2.227 (5) |
V3—V5 | 3.1010 (12) | OW1—Li1iii | 2.270 (5) |
V5—O10 | 1.6929 (17) | OW1—H1 | 0.83 (4) |
V5—O9 | 1.7072 (17) | OW1—H2 | 0.81 (4) |
V5—O2 | 1.9139 (16) | OW2—Li1iv | 2.167 (5) |
V5—O3 | 1.9341 (16) | OW2—H3 | 0.83 (4) |
V5—O1i | 2.1048 (16) | OW2—H4 | 0.83 (4) |
V5—O1 | 2.1317 (17) | OW3—Li1 | 2.227 (5) |
V5—V4i | 3.0785 (12) | OW3—H5 | 0.838 (18) |
V1—O13 | 1.6273 (17) | OW3—H6 | 0.84 (4) |
V1—O5i | 1.8127 (17) | OW4—Li1ii | 2.163 (5) |
V1—O6 | 1.8262 (18) | OW4—H7 | 0.797 (17) |
V1—O3i | 2.0048 (18) | OW4—H8 | 0.809 (17) |
V1—O2 | 2.0355 (17) | OW5—Li1 | 2.084 (5) |
V1—O1i | 2.2333 (15) | OW5—H9 | 0.825 (17) |
V1—V2 | 3.0899 (12) | OW5—H10 | 0.805 (17) |
V2—O14 | 1.6198 (17) | N1—H11 | 0.834 (18) |
V2—O8 | 1.8303 (18) | N1—H12 | 0.843 (18) |
V2—O7 | 1.8323 (17) | N1—H13 | 0.826 (18) |
V2—O3i | 2.0036 (17) | N1—H14 | 0.828 (18) |
V2—O2 | 2.0062 (18) | N2—H15 | 0.801 (18) |
V2—O1 | 2.2514 (15) | N2—H16 | 0.80 (4) |
V2—V4 | 3.1010 (9) | N2—H17 | 0.791 (19) |
V4—O12 | 1.6131 (19) | N2—H18 | 0.799 (18) |
V4—O4 | 1.8288 (18) | Li1—OW4v | 2.163 (5) |
V4—O8 | 1.8813 (17) | Li1—OW2iv | 2.167 (5) |
V4—O6i | 1.8992 (17) | Li1—OW1v | 2.227 (5) |
V4—O10i | 2.0659 (18) | Li1—OW1iii | 2.270 (5) |
V4—O1 | 2.3019 (18) | Li1—Li1vi | 3.277 (9) |
V4—V5i | 3.0785 (12) | Li1—H10 | 2.30 (4) |
O6—V4i | 1.8992 (17) | | |
| | | |
O11—V3—O4 | 104.68 (9) | O6i—V4—O10i | 82.92 (7) |
O11—V3—O7 | 102.27 (9) | O12—V4—O1 | 172.12 (8) |
O4—V3—O7 | 90.92 (8) | O4—V4—O1 | 82.93 (7) |
O11—V3—O5 | 103.28 (9) | O8—V4—O1 | 78.63 (7) |
O4—V3—O5 | 89.97 (8) | O6i—V4—O1 | 77.29 (7) |
O7—V3—O5 | 153.32 (7) | O10i—V4—O1 | 74.32 (6) |
O11—V3—O9 | 100.56 (9) | O12—V4—V5i | 129.02 (8) |
O4—V3—O9 | 154.75 (7) | O4—V4—V5i | 126.04 (6) |
O7—V3—O9 | 84.30 (7) | O8—V4—V5i | 79.23 (5) |
O5—V3—O9 | 83.61 (7) | O6i—V4—V5i | 78.39 (5) |
O11—V3—O1 | 174.67 (8) | O10i—V4—V5i | 31.21 (5) |
O4—V3—O1 | 80.65 (7) | O1—V4—V5i | 43.12 (4) |
O7—V3—O1 | 77.06 (6) | O12—V4—V3 | 138.48 (8) |
O5—V3—O1 | 76.78 (6) | O4—V4—V3 | 33.55 (5) |
O9—V3—O1 | 74.11 (6) | O8—V4—V3 | 85.13 (6) |
O11—V3—V4 | 137.57 (7) | O6i—V4—V3 | 84.60 (5) |
O4—V3—V4 | 32.91 (5) | O10i—V4—V3 | 123.71 (5) |
O7—V3—V4 | 82.98 (6) | O1—V4—V3 | 49.39 (4) |
O5—V3—V4 | 83.38 (5) | V5i—V4—V3 | 92.50 (3) |
O9—V3—V4 | 121.86 (5) | O12—V4—V2 | 134.03 (8) |
O1—V3—V4 | 47.75 (4) | O4—V4—V2 | 83.01 (6) |
O11—V3—V5 | 131.32 (7) | O8—V4—V2 | 32.82 (5) |
O4—V3—V5 | 124.01 (6) | O6i—V4—V2 | 123.68 (6) |
O7—V3—V5 | 78.63 (5) | O10i—V4—V2 | 82.01 (5) |
O5—V3—V5 | 78.83 (5) | O1—V4—V2 | 46.40 (4) |
O9—V3—V5 | 30.76 (5) | V5i—V4—V2 | 61.75 (2) |
O1—V3—V5 | 43.36 (4) | V3—V4—V2 | 60.95 (2) |
V4—V3—V5 | 91.10 (3) | V2—O7—V3 | 115.56 (8) |
O10—V5—O9 | 106.88 (9) | V5—O9—V3 | 111.73 (9) |
O10—V5—O2 | 97.52 (8) | V1—O6—V4i | 113.81 (9) |
O9—V5—O2 | 97.11 (8) | V2—O8—V4 | 113.33 (8) |
O10—V5—O3 | 97.18 (8) | V5—O10—V4i | 109.57 (9) |
O9—V5—O3 | 96.58 (7) | V1i—O5—V3 | 114.75 (8) |
O2—V5—O3 | 156.05 (7) | V4—O4—V3 | 113.55 (9) |
O10—V5—O1i | 87.59 (8) | V5—O2—V2 | 108.09 (8) |
O9—V5—O1i | 165.53 (7) | V5—O2—V1 | 107.06 (7) |
O2—V5—O1i | 80.94 (6) | V2—O2—V1 | 99.73 (7) |
O3—V5—O1i | 80.90 (6) | V5—O3—V2i | 107.27 (7) |
O10—V5—O1 | 166.11 (7) | V5—O3—V1i | 107.03 (7) |
O9—V5—O1 | 87.01 (7) | V2i—O3—V1i | 100.86 (8) |
O2—V5—O1 | 80.71 (7) | V5i—O1—V5 | 101.48 (7) |
O3—V5—O1 | 80.48 (7) | V5i—O1—V1i | 94.11 (6) |
O1i—V5—O1 | 78.52 (7) | V5—O1—V1i | 93.00 (6) |
O10—V5—V4i | 39.22 (6) | V5i—O1—V2 | 93.37 (6) |
O9—V5—V4i | 146.09 (6) | V5—O1—V2 | 92.74 (6) |
O2—V5—V4i | 90.26 (5) | V1i—O1—V2 | 169.48 (8) |
O3—V5—V4i | 89.27 (5) | V5i—O1—V4 | 88.51 (6) |
O1i—V5—V4i | 48.37 (5) | V5—O1—V4 | 169.98 (8) |
O1—V5—V4i | 126.89 (5) | V1i—O1—V4 | 86.97 (6) |
O10—V5—V3 | 144.39 (6) | V2—O1—V4 | 85.84 (5) |
O9—V5—V3 | 37.52 (6) | V5i—O1—V3 | 171.37 (8) |
O2—V5—V3 | 89.23 (5) | V5—O1—V3 | 87.14 (6) |
O3—V5—V3 | 89.74 (5) | V1i—O1—V3 | 85.78 (5) |
O1i—V5—V3 | 128.02 (5) | V2—O1—V3 | 85.71 (5) |
O1—V5—V3 | 49.50 (5) | V4—O1—V3 | 82.86 (6) |
V4i—V5—V3 | 176.381 (15) | Li1ii—OW1—Li1iii | 93.56 (17) |
O13—V1—O5i | 103.37 (9) | Li1ii—OW1—H1 | 114 (2) |
O13—V1—O6 | 102.01 (9) | Li1iii—OW1—H1 | 107 (3) |
O5i—V1—O6 | 95.24 (8) | Li1ii—OW1—H2 | 122 (2) |
O13—V1—O3i | 99.89 (8) | Li1iii—OW1—H2 | 105 (3) |
O5i—V1—O3i | 91.14 (8) | H1—OW1—H2 | 111 (3) |
O6—V1—O3i | 155.07 (7) | Li1iv—OW2—H3 | 135 (2) |
O13—V1—O2 | 98.96 (8) | Li1iv—OW2—H4 | 112 (2) |
O5i—V1—O2 | 155.80 (7) | H3—OW2—H4 | 111 (3) |
O6—V1—O2 | 89.09 (8) | Li1—OW3—H5 | 135 (2) |
O3i—V1—O2 | 75.80 (7) | Li1—OW3—H6 | 119 (2) |
O13—V1—O1i | 173.77 (8) | H5—OW3—H6 | 104 (2) |
O5i—V1—O1i | 81.93 (7) | Li1ii—OW4—H7 | 129 (3) |
O6—V1—O1i | 80.54 (7) | Li1ii—OW4—H8 | 113 (2) |
O3i—V1—O1i | 76.53 (6) | H7—OW4—H8 | 117 (3) |
O2—V1—O1i | 75.31 (6) | Li1—OW5—H9 | 113 (3) |
O13—V1—V2 | 89.27 (7) | Li1—OW5—H10 | 95 (3) |
O5i—V1—V2 | 130.69 (6) | H9—OW5—H10 | 111 (3) |
O6—V1—V2 | 128.88 (6) | H11—N1—H12 | 116 (3) |
O3i—V1—V2 | 39.55 (5) | H11—N1—H13 | 102 (3) |
O2—V1—V2 | 39.79 (5) | H12—N1—H13 | 118 (3) |
O1i—V1—V2 | 84.76 (5) | H11—N1—H14 | 97 (3) |
O14—V2—O8 | 103.13 (9) | H12—N1—H14 | 115 (3) |
O14—V2—O7 | 103.93 (9) | H13—N1—H14 | 105 (3) |
O8—V2—O7 | 94.83 (8) | H15—N2—H16 | 105 (4) |
O14—V2—O3i | 98.63 (8) | H15—N2—H17 | 119 (4) |
O8—V2—O3i | 89.92 (8) | H16—N2—H17 | 97 (4) |
O7—V2—O3i | 155.20 (7) | H15—N2—H18 | 112 (4) |
O14—V2—O2 | 99.17 (8) | H16—N2—H18 | 110 (4) |
O8—V2—O2 | 155.40 (7) | H17—N2—H18 | 112 (4) |
O7—V2—O2 | 89.74 (8) | OW5—Li1—OW4v | 86.62 (18) |
O3i—V2—O2 | 76.49 (7) | OW5—Li1—OW2iv | 174.7 (2) |
O14—V2—O1 | 173.25 (8) | OW4v—Li1—OW2iv | 89.48 (18) |
O8—V2—O1 | 81.00 (7) | OW5—Li1—OW1v | 91.73 (19) |
O7—V2—O1 | 80.84 (7) | OW4v—Li1—OW1v | 97.86 (19) |
O3i—V2—O1 | 75.88 (6) | OW2iv—Li1—OW1v | 85.26 (17) |
O2—V2—O1 | 75.88 (6) | OW5—Li1—OW3 | 93.95 (18) |
O14—V2—V1 | 88.49 (7) | OW4v—Li1—OW3 | 87.76 (18) |
O8—V2—V1 | 129.50 (6) | OW2iv—Li1—OW3 | 89.46 (18) |
O7—V2—V1 | 130.22 (6) | OW1v—Li1—OW3 | 172.2 (2) |
O3i—V2—V1 | 39.58 (5) | OW5—Li1—OW1iii | 98.44 (19) |
O2—V2—V1 | 40.49 (5) | OW4v—Li1—OW1iii | 173.3 (2) |
O1—V2—V1 | 84.77 (5) | OW2iv—Li1—OW1iii | 85.73 (17) |
O14—V2—V4 | 136.86 (7) | OW1v—Li1—OW1iii | 86.44 (17) |
O8—V2—V4 | 33.85 (5) | OW3—Li1—OW1iii | 87.50 (17) |
O7—V2—V4 | 83.20 (6) | OW5—Li1—Li1vi | 97.0 (2) |
O3i—V2—V4 | 87.40 (5) | OW4v—Li1—Li1vi | 141.3 (3) |
O2—V2—V4 | 123.63 (5) | OW2iv—Li1—Li1vi | 83.82 (18) |
O1—V2—V4 | 47.76 (4) | OW1v—Li1—Li1vi | 43.74 (12) |
V1—V2—V4 | 119.51 (2) | OW3—Li1—Li1vi | 130.0 (2) |
O12—V4—O4 | 104.94 (9) | OW1iii—Li1—Li1vi | 42.70 (11) |
O12—V4—O8 | 101.23 (9) | OW5—Li1—H10 | 20.4 (5) |
O4—V4—O8 | 92.72 (8) | OW4v—Li1—H10 | 106.4 (6) |
O12—V4—O6i | 101.66 (9) | OW2iv—Li1—H10 | 161.9 (6) |
O4—V4—O6i | 91.28 (8) | OW1v—Li1—H10 | 84.1 (8) |
O8—V4—O6i | 154.89 (7) | OW3—Li1—H10 | 99.5 (8) |
O12—V4—O10i | 97.81 (9) | OW1iii—Li1—H10 | 79.1 (7) |
O4—V4—O10i | 157.23 (7) | Li1vi—Li1—H10 | 78.4 (6) |
O8—V4—O10i | 83.86 (7) | | |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x−1, y+1, z; (iii) −x, −y, −z+2; (iv) −x, −y, −z+1; (v) x+1, y−1, z; (vi) −x+1, −y−1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—H1···O5 | 0.83 (4) | 2.11 (2) | 2.912 (3) | 164 (3) |
OW1—H2···O13vii | 0.81 (4) | 2.44 (3) | 3.130 (3) | 144 (3) |
OW2—H3···O9viii | 0.83 (4) | 2.07 (2) | 2.895 (3) | 178 (4) |
OW2—H4···O6 | 0.83 (4) | 2.03 (4) | 2.851 (3) | 174 (3) |
OW3—H5···O7 | 0.84 (3) | 2.03 (2) | 2.851 (3) | 166 (4) |
OW3—H6···O13iv | 0.84 (4) | 2.20 (2) | 2.985 (3) | 156 (3) |
OW3—H6···O14iv | 0.84 (4) | 2.62 (3) | 3.187 (3) | 126 (3) |
OW4—H7···O8ii | 0.80 (2) | 2.20 (2) | 2.975 (3) | 166 (3) |
OW4—H8···O3 | 0.81 (2) | 2.10 (2) | 2.902 (3) | 176 (4) |
OW5—H9···O4 | 0.83 (2) | 2.11 (2) | 2.890 (3) | 157 (3) |
OW5—H10···OW2ix | 0.81 (2) | 2.59 (2) | 3.305 (4) | 150 (3) |
N1—H11···O14 | 0.83 (2) | 2.04 (2) | 2.848 (3) | 163 (3) |
N1—H12···O10v | 0.84 (2) | 2.08 (2) | 2.866 (3) | 154 (3) |
N1—H12···O9iv | 0.84 (2) | 2.58 (3) | 3.009 (3) | 113 (3) |
N1—H13···OW4v | 0.83 (2) | 2.26 (2) | 3.070 (3) | 167 (3) |
N1—H13···OW3 | 0.83 (2) | 2.58 (3) | 3.028 (4) | 116 (3) |
N1—H14···O2iv | 0.83 (2) | 2.17 (2) | 2.943 (3) | 156 (3) |
N1—H14···O7iv | 0.83 (2) | 2.59 (3) | 3.040 (3) | 115 (3) |
N2—H15···O12x | 0.80 (2) | 2.34 (3) | 2.841 (3) | 121 (3) |
N2—H15···O11iv | 0.80 (2) | 2.41 (3) | 3.113 (3) | 146 (3) |
N2—H16···O13 | 0.80 (3) | 2.09 (2) | 2.884 (3) | 172 (4) |
N2—H17···O6xi | 0.79 (2) | 2.40 (3) | 2.986 (3) | 131 (3) |
N2—H17···O5xii | 0.79 (2) | 2.42 (2) | 3.178 (3) | 160 (3) |
N2—H17···O4xii | 0.79 (2) | 2.54 (3) | 3.076 (3) | 126 (3) |
N2—H18···OW5x | 0.80 (2) | 2.32 (2) | 3.108 (4) | 169 (4) |
Symmetry codes: (ii) x−1, y+1, z; (iv) −x, −y, −z+1; (v) x+1, y−1, z; (vii) x, y, z+1; (viii) −x−1, −y+1, −z+1; (ix) x+1, y−1, z+1; (x) −x+1, −y, −z+1; (xi) −x, −y+1, −z; (xii) x, y, z−1. |
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