Tetra-quinolinium ditelluro(VI)octa-vanadate(V) octa-hydrate.

In the title compound, (C9H8N)4[Te2V8O28]·8H2O, the com-plete heteropolyanion is generated by a crystallographic inversion centre. One of the two quniolinium ions forms an N-H⋯Op (p = polyoxidometallate) hydrogen bond and the other an N-H⋯Ow (w = water) hydrogen bond. The water mol-ecules further link the components by O-H⋯Op and O-H⋯Ow hydrogen bonds. A number of C-H⋯O inter-actions and aromatic π-π stacking inter-actions [shortest centroid-centroid separation = 3.541 (7) Å] are also observed. Together, these generate a three-dimensional network.

Related literature

For applications of polyoxidometallates, see: Fukuda & Yamase (1997 ▶); Rajakumar et al. (2000 ▶); Folbergrova & Mares (1987 ▶); Fantus et al. (1995 ▶). For bond-valence calculations, see: Brown & Altermatt (1985 ▶). For geometrical features in related structures, see: Lee et al. (2008 ▶); Joo et al. (2011 ▶); Strukan et al. (1997 ▶); Konaka et al. (2008 ▶, 2011 ▶); Evans et al. (1966 ▶); Hemissi et al. (2010 ▶).

Experimental

Crystal data

(C9H8N)4[Te2V8O28]·8H2O

M = 1775.50

Triclinic,

a = 10.907 (3) Å

b = 11.302 (3) Å

c = 13.169 (2) Å

α = 106.45 (4)°

β = 107.71 (4)°

γ = 105.34 (4)°

V = 1369.4 (6) Å3

Z = 1

Ag Kα radiation

λ = 0.56087 Å

μ = 1.28 mm−1

T = 295 K

0.19 × 0.15 × 0.09 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: analytical (Alcock, 1970 ▶) T min = 0.561, T max = 0.725

16455 measured reflections

13245 independent reflections

6549 reflections with I > 2σ(I)

R int = 0.045

2 standard reflections every 120 min intensity decay: 4%

Refinement

R[F 2 > 2σ(F 2)] = 0.115

wR(F 2) = 0.308

S = 1.05

13245 reflections

385 parameters

20 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 3.11 e Å−3

Δρmin = −2.28 e Å−3

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1996 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶) and DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: WinGX (Farrugia, 2012 ▶).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536813027347/hb7146sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813027347/hb7146Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C9H8N)4[Te2V8O28]·8H2O	Z = 1
Mr = 1775.50	F(000) = 868
Triclinic, P1	Dx = 2.153 Mg m−3
Hall symbol: -P 1	Ag Kα radiation, λ = 0.56087 Å
a = 10.907 (3) Å	Cell parameters from 25 reflections
b = 11.302 (3) Å	θ = 9–11°
c = 13.169 (2) Å	µ = 1.28 mm−1
α = 106.45 (4)°	T = 295 K
β = 107.71 (4)°	Rectangular, yellow
γ = 105.34 (4)°	0.19 × 0.15 × 0.09 mm
V = 1369.4 (6) Å3

Enraf–Nonius CAD-4 diffractometer	6549 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.045
Graphite monochromator	θmax = 28.0°, θmin = 2.3°
non–profiled ω scans	h = −18→17
Absorption correction: analytical (Alcock, 1970)	k = −18→18
Tmin = 0.561, Tmax = 0.725	l = −3→22
16455 measured reflections	2 standard reflections every 120 min
13245 independent reflections	intensity decay: 4%

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)] = 0.115	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.308	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ2(Fo2) + (0.0978P)2 + 22.5177P] where P = (Fo2 + 2Fc2)/3
13245 reflections	(Δ/σ)max < 0.001
385 parameters	Δρmax = 3.11 e Å−3
20 restraints	Δρmin = −2.28 e Å−3

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.

	x	y	z	Uiso*/Ueq
Te1	0.16225 (7)	0.58886 (7)	0.58253 (6)	0.03140 (18)
V1	0.05217 (14)	0.27420 (12)	0.49481 (12)	0.0177 (2)
V2	0.03656 (13)	0.57033 (13)	0.32457 (11)	0.0166 (2)
V3	0.23652 (14)	0.42319 (14)	0.39532 (13)	0.0213 (3)
V4	0.07774 (16)	0.74944 (13)	0.76322 (12)	0.0215 (3)
O1	0.1649 (8)	0.8702 (7)	0.8882 (6)	0.0356 (16)
O2	−0.0552 (6)	0.1678 (5)	0.3401 (5)	0.0198 (10)
O3	0.2094 (6)	0.3145 (6)	0.4763 (5)	0.0209 (11)
O4	0.1186 (7)	0.6932 (7)	0.4925 (6)	0.03140 (18)
O5	0.0293 (7)	0.6753 (6)	0.2649 (6)	0.0261 (12)
O6	−0.0685 (6)	0.4051 (5)	0.2031 (5)	0.0209 (11)
O7	0.0538 (8)	0.1673 (6)	0.5536 (6)	0.0289 (14)
O8	0.1039 (6)	0.2887 (5)	0.2588 (5)	0.0208 (11)
O9	0.3794 (7)	0.4249 (7)	0.3844 (7)	0.0322 (14)
O10	−0.0326 (7)	0.5676 (7)	0.5778 (6)	0.03140 (18)
O11	0.3065 (6)	0.5744 (6)	0.5518 (5)	0.0233 (11)
O12	0.1318 (7)	0.4462 (7)	0.6351 (6)	0.03140 (18)
O13	0.2328 (6)	0.7205 (6)	0.7204 (5)	0.0215 (11)
O14	0.1984 (6)	0.5518 (6)	0.3384 (5)	0.0203 (10)
O1W	0.0759 (8)	0.0847 (6)	0.7344 (6)	0.0335 (15)
H1W1	0.067 (3)	0.118 (3)	0.683 (2)	0.040*
H2W1	0.0671	0.0039	0.7102	0.040*
O2W	1.1818 (11)	0.1180 (8)	1.1089 (9)	0.060 (3)
H1W2	1.176 (13)	0.185 (2)	1.154 (12)	0.072*
H2W2	1.1280	0.0421	1.0989	0.072*
O3W	0.9613 (14)	0.3830 (8)	1.0059 (9)	0.065 (3)
H1W3	0.947 (18)	0.401 (9)	1.068 (8)	0.078*
H2W3	0.9696	0.3095	0.9801	0.078*
O4W	0.9969 (13)	0.1478 (11)	0.9221 (9)	0.067 (3)
H1W4	1.0634 (19)	0.121 (3)	0.936 (5)	0.081*
H2W4	0.947 (3)	0.1236 (17)	0.8506 (12)	0.081*
N1	0.3469 (8)	0.2174 (8)	0.8833 (7)	0.0351 (18)
H1	0.2632	0.1746	0.8307	0.042*
N2	0.4422 (8)	0.7675 (7)	0.4207 (8)	0.0297 (16)
H2	0.3644	0.7027	0.3982	0.036*
C1	0.4842 (14)	0.4522 (13)	0.7670 (11)	0.046 (3)
H1A	0.4551	0.4753	0.7040	0.056*
C2	0.6262 (15)	0.5203 (13)	0.8545 (13)	0.049 (3)
H2A	0.6894	0.5873	0.8470	0.059*
C3	0.6670 (12)	0.4882 (11)	0.9452 (13)	0.047 (3)
H3	0.7581	0.5342	1.0011	0.056*
C4	0.5747 (10)	0.3857 (10)	0.9581 (9)	0.0305 (18)
C5	0.6157 (12)	0.3427 (12)	1.0502 (11)	0.047 (3)
H5	0.7075	0.3808	1.1049	0.056*
C6	0.5166 (14)	0.2435 (13)	1.0568 (11)	0.047 (3)
H6	0.5410	0.2175	1.1186	0.056*
C7	0.3861 (11)	0.1844 (11)	0.9754 (10)	0.039 (2)
H7	0.3207	0.1189	0.9825	0.046*
C8	0.3937 (12)	0.3527 (12)	0.7797 (10)	0.040 (2)
H8	0.3017	0.3089	0.7251	0.048*
C9	0.4371 (9)	0.3171 (9)	0.8717 (8)	0.0274 (17)
C10	0.5429 (11)	0.7920 (10)	0.5154 (10)	0.036 (2)
H10	0.5287	0.7373	0.5553	0.043*
C11	0.6672 (12)	0.8923 (12)	0.5600 (12)	0.048 (3)
H11	0.7361	0.9090	0.6306	0.057*
C12	0.6909 (11)	0.9708 (11)	0.4981 (12)	0.043 (3)
H12	0.7776	1.0383	0.5247	0.052*
C13	0.5836 (10)	0.9467 (8)	0.3967 (11)	0.038 (2)
C14	0.5994 (13)	1.0189 (12)	0.3266 (13)	0.049 (3)
H14	0.6845	1.0867	0.3490	0.059*
C15	0.4871 (19)	0.9884 (14)	0.2232 (16)	0.063 (4)
H15	0.4970	1.0390	0.1793	0.076*
C16	0.3654 (17)	0.8868 (15)	0.1870 (15)	0.066 (4)
H16	0.2949	0.8661	0.1159	0.080*
C17	0.3395 (11)	0.8109 (10)	0.2506 (11)	0.038 (2)
H17	0.2524	0.7452	0.2267	0.046*
C18	0.4533 (9)	0.8398 (8)	0.3537 (9)	0.0289 (18)

	U11	U22	U33	U12	U13	U23
Te1	0.0292 (3)	0.0266 (3)	0.0309 (3)	0.0036 (2)	0.0090 (2)	0.0112 (2)
V1	0.0244 (6)	0.0124 (5)	0.0195 (6)	0.0075 (4)	0.0102 (5)	0.0092 (5)
V2	0.0188 (5)	0.0153 (5)	0.0169 (6)	0.0046 (4)	0.0073 (5)	0.0100 (5)
V3	0.0195 (6)	0.0223 (6)	0.0271 (7)	0.0087 (5)	0.0126 (5)	0.0129 (5)
V4	0.0271 (7)	0.0146 (5)	0.0144 (6)	0.0031 (5)	0.0058 (5)	0.0018 (4)
O1	0.046 (4)	0.027 (3)	0.017 (3)	0.003 (3)	0.009 (3)	0.000 (2)
O2	0.027 (3)	0.012 (2)	0.019 (3)	0.0035 (19)	0.009 (2)	0.0077 (19)
O3	0.020 (2)	0.022 (3)	0.024 (3)	0.008 (2)	0.009 (2)	0.014 (2)
O4	0.0292 (3)	0.0266 (3)	0.0309 (3)	0.0036 (2)	0.0090 (2)	0.0112 (2)
O5	0.030 (3)	0.025 (3)	0.029 (3)	0.011 (2)	0.011 (3)	0.020 (3)
O6	0.023 (3)	0.011 (2)	0.017 (2)	−0.0030 (18)	0.004 (2)	0.0032 (18)
O7	0.050 (4)	0.018 (3)	0.023 (3)	0.014 (3)	0.016 (3)	0.013 (2)
O8	0.029 (3)	0.017 (2)	0.016 (2)	0.007 (2)	0.009 (2)	0.008 (2)
O9	0.027 (3)	0.042 (4)	0.040 (4)	0.017 (3)	0.022 (3)	0.022 (3)
O10	0.0292 (3)	0.0266 (3)	0.0309 (3)	0.0036 (2)	0.0090 (2)	0.0112 (2)
O11	0.018 (2)	0.025 (3)	0.024 (3)	0.003 (2)	0.008 (2)	0.011 (2)
O12	0.0292 (3)	0.0266 (3)	0.0309 (3)	0.0036 (2)	0.0090 (2)	0.0112 (2)
O13	0.017 (2)	0.019 (2)	0.022 (3)	0.0013 (19)	0.006 (2)	0.008 (2)
O14	0.017 (2)	0.023 (3)	0.019 (3)	0.0009 (19)	0.007 (2)	0.011 (2)
O1W	0.047 (4)	0.022 (3)	0.028 (3)	0.013 (3)	0.009 (3)	0.013 (3)
O2W	0.080 (7)	0.051 (5)	0.058 (6)	0.021 (5)	0.051 (6)	0.013 (5)
O3W	0.110 (9)	0.050 (5)	0.043 (5)	0.027 (6)	0.045 (6)	0.019 (4)
O4W	0.095 (8)	0.075 (7)	0.052 (6)	0.037 (6)	0.045 (6)	0.032 (5)
N1	0.029 (4)	0.030 (4)	0.031 (4)	0.001 (3)	0.001 (3)	0.013 (3)
N2	0.028 (3)	0.016 (3)	0.040 (4)	0.004 (3)	0.012 (3)	0.009 (3)
C1	0.063 (8)	0.053 (7)	0.041 (6)	0.026 (6)	0.027 (6)	0.033 (6)
C2	0.062 (8)	0.040 (6)	0.065 (8)	0.022 (6)	0.045 (7)	0.025 (6)
C3	0.028 (5)	0.033 (5)	0.067 (8)	0.000 (4)	0.021 (5)	0.013 (5)
C4	0.030 (4)	0.030 (4)	0.030 (5)	0.017 (4)	0.007 (4)	0.010 (4)
C5	0.030 (5)	0.042 (6)	0.050 (7)	0.000 (4)	−0.001 (5)	0.024 (5)
C6	0.051 (7)	0.046 (6)	0.043 (6)	0.017 (5)	0.012 (5)	0.025 (5)
C7	0.034 (5)	0.039 (5)	0.037 (5)	0.002 (4)	0.009 (4)	0.024 (4)
C8	0.040 (5)	0.046 (6)	0.028 (5)	0.014 (5)	0.007 (4)	0.016 (4)
C9	0.026 (4)	0.027 (4)	0.030 (4)	0.004 (3)	0.013 (3)	0.016 (3)
C10	0.037 (5)	0.030 (4)	0.043 (6)	0.015 (4)	0.020 (5)	0.012 (4)
C11	0.030 (5)	0.043 (6)	0.059 (8)	0.016 (5)	0.008 (5)	0.014 (6)
C12	0.026 (4)	0.029 (5)	0.065 (8)	0.003 (4)	0.019 (5)	0.013 (5)
C13	0.030 (4)	0.011 (3)	0.064 (7)	−0.001 (3)	0.021 (5)	0.008 (4)
C14	0.039 (6)	0.036 (5)	0.073 (9)	0.002 (4)	0.026 (6)	0.030 (6)
C15	0.098 (12)	0.043 (7)	0.092 (12)	0.033 (8)	0.075 (11)	0.042 (8)
C16	0.063 (9)	0.047 (7)	0.061 (9)	0.028 (7)	0.001 (7)	0.002 (7)
C17	0.034 (5)	0.025 (4)	0.052 (7)	0.006 (4)	0.017 (5)	0.018 (4)
C18	0.025 (4)	0.011 (3)	0.043 (5)	−0.003 (3)	0.018 (4)	0.005 (3)

Te1—O13	1.765 (6)	O12—V2i	2.039 (7)
Te1—O11	1.775 (6)	O1W—H1W1	0.853 (10)
Te1—O12	1.918 (7)	O1W—H2W1	0.845 (5)
Te1—O4	1.941 (7)	O2W—H1W2	0.849 (10)
Te1—O10	2.054 (7)	O2W—H2W2	0.849 (7)
Te1—O10i	2.080 (7)	O3W—H1W3	0.850 (10)
Te1—V4	3.095 (2)	O3W—H2W3	0.844 (7)
Te1—V3	3.105 (2)	O4W—H1W4	0.850 (10)
Te1—V1	3.161 (2)	O4W—H2W4	0.849 (10)
Te1—V2	3.1740 (18)	N1—C7	1.348 (13)
Te1—Te1i	3.220 (3)	N1—C9	1.366 (11)
V1—O7	1.610 (6)	N1—H1	0.8600
V1—O3	1.764 (6)	N2—C10	1.283 (14)
V1—O2	1.840 (6)	N2—C18	1.372 (12)
V1—O12	2.010 (7)	N2—H2	0.8600
V1—O4i	2.037 (7)	C1—C8	1.373 (17)
V1—O10i	2.281 (7)	C1—C2	1.45 (2)
V1—V2i	3.101 (2)	C1—H1A	0.9300
V1—V3	3.107 (2)	C2—C3	1.328 (19)
V2—O5	1.603 (6)	C2—H2A	0.9300
V2—O14	1.793 (6)	C3—C4	1.408 (15)
V2—O6	1.849 (6)	C3—H3	0.9300
V2—O4	2.005 (7)	C4—C9	1.412 (13)
V2—O12i	2.039 (7)	C4—C5	1.423 (15)
V2—O10i	2.285 (7)	C5—C6	1.380 (17)
V2—V1i	3.101 (2)	C5—H5	0.9300
V3—O9	1.604 (7)	C6—C7	1.336 (16)
V3—O8	1.828 (6)	C6—H6	0.9300
V3—O3	1.864 (6)	C7—H7	0.9300
V3—O14	1.895 (6)	C8—C9	1.372 (14)
V3—O11	2.027 (7)	C8—H8	0.9300
V3—O10i	2.380 (7)	C10—C11	1.339 (16)
V3—V4i	3.117 (3)	C10—H10	0.9300
V4—O1	1.602 (7)	C11—C12	1.390 (19)
V4—O8i	1.822 (6)	C11—H11	0.9300
V4—O2i	1.851 (6)	C12—C13	1.379 (18)
V4—O6i	1.905 (6)	C12—H12	0.9300
V4—O13	2.013 (6)	C13—C14	1.413 (17)
V4—O10	2.387 (7)	C13—C18	1.420 (12)
V4—V3i	3.117 (3)	C14—C15	1.40 (2)
O2—V4i	1.851 (6)	C14—H14	0.9300
O4—V1i	2.037 (7)	C15—C16	1.34 (2)
O6—V4i	1.905 (6)	C15—H15	0.9300
O8—V4i	1.822 (6)	C16—C17	1.39 (2)
O10—Te1i	2.080 (7)	C16—H16	0.9300
O10—V1i	2.281 (7)	C17—C18	1.414 (16)
O10—V2i	2.285 (7)	C17—H17	0.9300
O10—V3i	2.380 (7)
O13—Te1—O11	106.2 (3)	O11—V3—Te1	32.64 (17)
O13—Te1—O12	96.4 (3)	O10i—V3—Te1	42.03 (17)
O11—Te1—O12	96.9 (3)	O9—V3—V1	133.6 (3)
O13—Te1—O4	96.4 (3)	O8—V3—V1	81.44 (19)
O11—Te1—O4	96.4 (3)	O3—V3—V1	30.14 (18)
O12—Te1—O4	158.2 (3)	O14—V3—V1	122.84 (18)
O13—Te1—O10	88.1 (3)	O11—V3—V1	82.33 (18)
O11—Te1—O10	165.7 (3)	O10i—V3—V1	46.83 (17)
O12—Te1—O10	81.5 (3)	Te1—V3—V1	61.17 (5)
O4—Te1—O10	81.3 (3)	O9—V3—V4i	134.2 (3)
O13—Te1—O10i	165.8 (3)	O8—V3—V4i	31.3 (2)
O11—Te1—O10i	88.0 (3)	O3—V3—V4i	83.04 (19)
O12—Te1—O10i	81.8 (3)	O14—V3—V4i	83.61 (18)
O4—Te1—O10i	81.4 (3)	O11—V3—V4i	123.93 (18)
O10—Te1—O10i	77.7 (3)	O10i—V3—V4i	49.27 (17)
O13—Te1—V4	37.73 (19)	Te1—V3—V4i	91.29 (7)
O11—Te1—V4	143.9 (2)	V1—V3—V4i	61.01 (5)
O12—Te1—V4	90.4 (2)	O1—V4—O8i	104.6 (3)
O4—Te1—V4	89.0 (2)	O1—V4—O2i	104.4 (3)
O10—Te1—V4	50.4 (2)	O8i—V4—O2i	89.8 (3)
O10i—Te1—V4	128.1 (2)	O1—V4—O6i	103.4 (3)
O13—Te1—V3	144.19 (19)	O8i—V4—O6i	88.9 (3)
O11—Te1—V3	38.0 (2)	O2i—V4—O6i	151.5 (3)
O12—Te1—V3	89.5 (2)	O1—V4—O13	100.9 (3)
O4—Te1—V3	90.3 (2)	O8i—V4—O13	154.4 (3)
O10—Te1—V3	127.7 (2)	O2i—V4—O13	85.6 (3)
O10i—Te1—V3	50.0 (2)	O6i—V4—O13	83.4 (3)
V4—Te1—V3	178.06 (5)	O1—V4—O10	174.8 (4)
O13—Te1—V1	133.8 (2)	O8i—V4—O10	80.5 (3)
O11—Te1—V1	84.6 (2)	O2i—V4—O10	76.5 (2)
O12—Te1—V1	37.4 (2)	O6i—V4—O10	75.3 (2)
O4—Te1—V1	127.5 (2)	O13—V4—O10	74.0 (2)
O10—Te1—V1	85.7 (2)	O1—V4—Te1	133.3 (3)
O10i—Te1—V1	46.1 (2)	O8i—V4—Te1	122.0 (2)
V4—Te1—V1	119.73 (6)	O2i—V4—Te1	78.91 (19)
V3—Te1—V1	59.45 (5)	O6i—V4—Te1	77.73 (19)
O13—Te1—V2	133.6 (2)	O13—V4—Te1	32.45 (17)
O11—Te1—V2	84.3 (2)	O10—V4—Te1	41.54 (17)
O12—Te1—V2	127.7 (2)	O1—V4—V3i	136.0 (3)
O4—Te1—V2	37.1 (2)	O8i—V4—V3i	31.41 (18)
O10—Te1—V2	85.5 (2)	O2i—V4—V3i	81.97 (19)
O10i—Te1—V2	45.95 (19)	O6i—V4—V3i	82.23 (18)
V4—Te1—V2	118.35 (5)	O13—V4—V3i	123.07 (18)
V3—Te1—V2	60.30 (5)	O10—V4—V3i	49.08 (18)
V1—Te1—V2	91.45 (7)	Te1—V4—V3i	90.62 (7)
O13—Te1—Te1i	127.3 (2)	V1—O2—V4i	117.8 (3)
O11—Te1—Te1i	126.5 (2)	V1—O3—V3	117.8 (3)
O12—Te1—Te1i	79.3 (2)	Te1—O4—V2	107.1 (3)
O4—Te1—Te1i	78.9 (2)	Te1—O4—V1i	107.2 (3)
O10—Te1—Te1i	39.14 (19)	V2—O4—V1i	100.2 (3)
O10i—Te1—Te1i	38.5 (2)	V2—O6—V4i	117.7 (3)
V4—Te1—Te1i	89.55 (6)	V4i—O8—V3	117.3 (3)
V3—Te1—Te1i	88.53 (6)	Te1—O10—Te1i	102.3 (3)
V1—Te1—Te1i	60.25 (6)	Te1—O10—V1i	95.2 (3)
V2—Te1—Te1i	60.03 (5)	Te1i—O10—V1i	92.8 (3)
O7—V1—O3	105.3 (3)	Te1—O10—V2i	94.9 (3)
O7—V1—O2	102.9 (3)	Te1i—O10—V2i	93.2 (3)
O3—V1—O2	93.8 (3)	V1i—O10—V2i	167.0 (4)
O7—V1—O12	101.4 (3)	Te1—O10—V3i	169.7 (4)
O3—V1—O12	91.1 (3)	Te1i—O10—V3i	88.0 (2)
O2—V1—O12	152.9 (3)	V1i—O10—V3i	83.6 (2)
O7—V1—O4i	99.3 (3)	V2i—O10—V3i	85.1 (2)
O3—V1—O4i	154.0 (3)	Te1—O10—V4	88.0 (2)
O2—V1—O4i	88.6 (3)	Te1i—O10—V4	169.6 (4)
O12—V1—O4i	75.9 (3)	V1i—O10—V4	85.2 (2)
O7—V1—O10i	172.9 (3)	V2i—O10—V4	86.9 (2)
O3—V1—O10i	81.1 (3)	V3i—O10—V4	81.7 (2)
O2—V1—O10i	79.5 (2)	Te1—O11—V3	109.4 (3)
O12—V1—O10i	75.0 (3)	Te1—O12—V1	107.1 (3)
O4i—V1—O10i	74.0 (3)	Te1—O12—V2i	107.8 (3)
O7—V1—V2i	89.7 (2)	V1—O12—V2i	99.9 (3)
O3—V1—V2i	131.4 (2)	Te1—O13—V4	109.8 (3)
O2—V1—V2i	128.1 (2)	V2—O14—V3	117.5 (3)
O12—V1—V2i	40.4 (2)	H1W1—O1W—H2W1	115 (3)
O4i—V1—V2i	39.5 (2)	H1W2—O2W—H2W2	115 (3)
O10i—V1—V2i	83.69 (19)	H1W3—O3W—H2W3	117 (3)
O7—V1—V3	137.1 (3)	H1W4—O4W—H2W4	115 (3)
O3—V1—V3	32.04 (18)	C7—N1—C9	121.5 (8)
O2—V1—V3	82.40 (18)	C7—N1—H1	119.2
O12—V1—V3	87.9 (2)	C9—N1—H1	119.2
O4i—V1—V3	123.5 (2)	C10—N2—C18	123.0 (8)
O10i—V1—V3	49.57 (18)	C10—N2—H2	118.5
V2i—V1—V3	120.78 (6)	C18—N2—H2	118.5
O7—V1—Te1	136.4 (2)	C8—C1—C2	118.3 (11)
O3—V1—Te1	77.3 (2)	C8—C1—H1A	120.9
O2—V1—Te1	120.50 (18)	C2—C1—H1A	120.9
O12—V1—Te1	35.4 (2)	C3—C2—C1	120.7 (11)
O4i—V1—Te1	79.20 (19)	C3—C2—H2A	119.6
O10i—V1—Te1	41.10 (17)	C1—C2—H2A	119.6
V2i—V1—Te1	61.43 (5)	C2—C3—C4	121.1 (11)
V3—V1—Te1	59.39 (5)	C2—C3—H3	119.4
O5—V2—O14	105.6 (3)	C4—C3—H3	119.4
O5—V2—O6	104.4 (3)	C3—C4—C9	118.3 (10)
O14—V2—O6	93.3 (3)	C3—C4—C5	123.2 (10)
O5—V2—O4	100.4 (3)	C9—C4—C5	118.5 (9)
O14—V2—O4	91.4 (3)	C6—C5—C4	118.8 (10)
O6—V2—O4	152.5 (3)	C6—C5—H5	120.6
O5—V2—O12i	100.0 (3)	C4—C5—H5	120.6
O14—V2—O12i	153.2 (3)	C7—C6—C5	120.7 (11)
O6—V2—O12i	88.1 (3)	C7—C6—H6	119.6
O4—V2—O12i	76.0 (3)	C5—C6—H6	119.6
O5—V2—O10i	172.8 (3)	C6—C7—N1	121.6 (10)
O14—V2—O10i	80.5 (2)	C6—C7—H7	119.2
O6—V2—O10i	78.9 (2)	N1—C7—H7	119.2
O4—V2—O10i	75.1 (3)	C9—C8—C1	120.9 (11)
O12i—V2—O10i	73.5 (3)	C9—C8—H8	119.6
O5—V2—V1i	89.4 (3)	C1—C8—H8	119.6
O14—V2—V1i	131.6 (2)	N1—C9—C8	120.7 (9)
O6—V2—V1i	127.8 (2)	N1—C9—C4	118.7 (8)
O4—V2—V1i	40.3 (2)	C8—C9—C4	120.6 (9)
O12i—V2—V1i	39.7 (2)	N2—C10—C11	123.5 (11)
O10i—V2—V1i	83.49 (19)	N2—C10—H10	118.2
O5—V2—Te1	135.7 (3)	C11—C10—H10	118.2
O14—V2—Te1	77.17 (19)	C10—C11—C12	118.4 (12)
O6—V2—Te1	119.75 (19)	C10—C11—H11	120.8
O4—V2—Te1	35.8 (2)	C12—C11—H11	120.8
O12i—V2—Te1	78.9 (2)	C13—C12—C11	118.9 (10)
O10i—V2—Te1	40.88 (18)	C13—C12—H12	120.6
V1i—V2—Te1	61.38 (5)	C11—C12—H12	120.6
O9—V3—O8	102.9 (3)	C12—C13—C14	122.8 (9)
O9—V3—O3	103.6 (3)	C12—C13—C18	120.4 (10)
O8—V3—O3	91.2 (3)	C14—C13—C18	116.7 (11)
O9—V3—O14	103.5 (3)	C15—C14—C13	120.2 (10)
O8—V3—O14	90.2 (2)	C15—C14—H14	119.9
O3—V3—O14	151.8 (3)	C13—C14—H14	119.9
O9—V3—O11	101.9 (3)	C16—C15—C14	120.6 (13)
O8—V3—O11	155.2 (3)	C16—C15—H15	119.7
O3—V3—O11	84.1 (3)	C14—C15—H15	119.7
O14—V3—O11	83.0 (3)	C15—C16—C17	123.3 (14)
O9—V3—O10i	176.5 (3)	C15—C16—H16	118.3
O8—V3—O10i	80.6 (3)	C17—C16—H16	118.3
O3—V3—O10i	76.5 (2)	C16—C17—C18	116.1 (10)
O14—V3—O10i	76.0 (2)	C16—C17—H17	122.0
O11—V3—O10i	74.7 (2)	C18—C17—H17	122.0
O9—V3—Te1	134.5 (3)	N2—C18—C17	121.4 (8)
O8—V3—Te1	122.6 (2)	N2—C18—C13	115.7 (10)
O3—V3—Te1	77.75 (19)	C17—C18—C13	122.9 (9)
O14—V3—Te1	77.87 (18)
C8—C1—C2—C3	−0.8 (19)	C18—N2—C10—C11	1.8 (17)
C1—C2—C3—C4	1.2 (19)	N2—C10—C11—C12	−2.8 (18)
C2—C3—C4—C9	0.2 (17)	C10—C11—C12—C13	3.2 (18)
C2—C3—C4—C5	176.4 (12)	C11—C12—C13—C14	−178.1 (12)
C3—C4—C5—C6	178.5 (12)	C11—C12—C13—C18	−2.8 (17)
C9—C4—C5—C6	−5.3 (18)	C12—C13—C14—C15	178.9 (12)
C4—C5—C6—C7	3 (2)	C18—C13—C14—C15	3.4 (18)
C5—C6—C7—N1	1 (2)	C13—C14—C15—C16	−3 (2)
C9—N1—C7—C6	−3.1 (18)	C14—C15—C16—C17	4 (2)
C2—C1—C8—C9	−1.1 (19)	C15—C16—C17—C18	−5 (2)
C7—N1—C9—C8	−177.4 (11)	C10—N2—C18—C17	−179.1 (10)
C7—N1—C9—C4	0.7 (16)	C10—N2—C18—C13	−1.1 (14)
C1—C8—C9—N1	−179.5 (11)	C16—C17—C18—N2	−176.9 (10)
C1—C8—C9—C4	2.5 (17)	C16—C17—C18—C13	5.2 (16)
C3—C4—C9—N1	179.9 (10)	C12—C13—C18—N2	1.7 (14)
C5—C4—C9—N1	3.5 (15)	C14—C13—C18—N2	177.3 (10)
C3—C4—C9—C8	−2.0 (15)	C12—C13—C18—C17	179.7 (10)
C5—C4—C9—C8	−178.4 (11)	C14—C13—C18—C17	−4.7 (15)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W1···O2ii	0.85 (1)	1.82 (1)	2.663 (8)	178 (1)
O1W—H1W1···O7	0.85 (1)	1.92 (2)	2.762 (9)	170 (4)
O2W—H1W2···O8iii	0.85 (1)	2.03 (2)	2.842 (10)	159 (4)
O2W—H2W2···O4Wiv	0.85 (1)	2.10 (1)	2.952 (14)	177 (1)
O3W—H2W3···O4W	0.84 (1)	1.91 (1)	2.754 (14)	177 (1)
O3W—H1W3···O6iii	0.85 (1)	1.83 (2)	2.665 (11)	166 (6)
O4W—H2W4···O1Wv	0.85 (1)	2.41 (3)	2.826 (12)	111 (3)
O4W—H1W4···O2W	0.85 (1)	2.26 (5)	2.836 (17)	125 (5)
N1—H1···O1W	0.86	1.85	2.700 (11)	172
N2—H2···O14	0.86	1.88	2.740 (9)	175
C5—H5···O6iii	0.93	2.29	3.180 (13)	160
C6—H6···O13vi	0.93	2.48	3.178 (14)	132
C7—H7···O1vii	0.93	2.56	3.350 (13)	143
C7—H7···O2Wviii	0.93	2.57	3.296 (14)	135
C10—H10···O9ix	0.93	2.51	3.275 (13)	140
C14—H14···O4x	0.93	2.58	3.403 (14)	148
C17—H17···O5	0.93	2.60	3.411 (13)	146

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H2W1⋯O2i	0.85 (1)	1.82 (1)	2.663 (8)	178 (1)
O1W—H1W1⋯O7	0.85 (1)	1.92 (2)	2.762 (9)	170 (4)
O2W—H1W2⋯O8ii	0.85 (1)	2.03 (2)	2.842 (10)	159 (4)
O2W—H2W2⋯O4W iii	0.85 (1)	2.10 (1)	2.952 (14)	177 (1)
O3W—H2W3⋯O4W	0.84 (1)	1.91 (1)	2.754 (14)	177 (1)
O3W—H1W3⋯O6ii	0.85 (1)	1.83 (2)	2.665 (11)	166 (6)
O4W—H2W4⋯O1W iv	0.85 (1)	2.41 (3)	2.826 (12)	111 (3)
O4W—H1W4⋯O2W	0.85 (1)	2.26 (5)	2.836 (17)	125 (5)
N1—H1⋯O1W	0.86	1.85	2.700 (11)	172
N2—H2⋯O14	0.86	1.88	2.740 (9)	175
C5—H5⋯O6ii	0.93	2.29	3.180 (13)	160
C6—H6⋯O13v	0.93	2.48	3.178 (14)	132
C7—H7⋯O1vi	0.93	2.56	3.350 (13)	143
C7—H7⋯O2W vii	0.93	2.57	3.296 (14)	135
C10—H10⋯O9viii	0.93	2.51	3.275 (13)	140
C14—H14⋯O4ix	0.93	2.58	3.403 (14)	148
C17—H17⋯O5	0.93	2.60	3.411 (13)	146

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .