Tetra­quinolinium ditelluro(VI)octa­vanadate(V) octa­hydrate

Toumi, S.; Toumi, S.A.; Rzaigui, M.

doi:10.1107/S1600536813027347

metal-organic compounds

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ISSN: 2056-9890

Volume 69| Part 11| November 2013| Pages m595-m596

doi:10.1107/S1600536813027347

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Tetraquinolinium ditelluro(VI)octavanadate(V) octahydrate

Sirine Toumi,^a ^* Samah Akriche Toumi ^a and Mohamed Rzaigui ^a

^aLaboratoire de chimie des Matériaux, Faculté des Sciences de Bizerte, 7021 Zarzouna Bizerte, Tunisia
^*Correspondence e-mail: samah.akriche@fsb.rnu.tn

(Received 3 October 2013; accepted 4 October 2013; online 12 October 2013)

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

CCDC reference: 964952

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_r = 1775.50
Triclinic, $[P \overline 1]$
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[F² > 2σ(F²)] = 0.115
wR(F²) = 0.308
S = 1.05
13245 reflections
385 parameters
20 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 3.11 e Å⁻³
Δρ_min = −2.28 e Å⁻³

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⋯O4Wⁱⁱⁱ	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⋯O13^v	0.93	2.48	3.178 (14)	132
C7—H7⋯O1^vi	0.93	2.56	3.350 (13)	143
C7—H7⋯O2W^vii	0.93	2.57	3.296 (14)	135
C10—H10⋯O9^viii	0.93	2.51	3.275 (13)	140
C14—H14⋯O4^ix	0.93	2.58	3.403 (14)	148
C17—H17⋯O5	0.93	2.60	3.411 (13)	146
Symmetry codes: (i) -x, -y, -z+1; (ii) x+1, y, z+1; (iii) -x+2, -y, -z+2; (iv) x+1, y, z; (v) -x+1, -y+1, -z+2; (vi) x, y-1, z; (vii) x-1, y, z; (viii) -x+1, -y+1, -z+1; (ix) -x+1, -y+2, -z+1.

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).

Supporting information

CCDC reference: 964952

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

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

checkCIF report

Comment top

The polyoxovanadate materials (POVs) are well established in magnetic, electric and biomedical fields because of their richness structural variety in relation with the vanadium element which can adopt different coordination geometries and variable oxidation states very interesting for redox applications in catalysis and materials science (Fukuda et al., 1997; Rajakumar et al., 2000; Folbergrova et al., 1987; Fantus et al.,1995). Furthermore, this family is dominated by the decavanadates, well known in their protonated forms [H_xV₁₀O₂₈]^{(6 -} ^x^)-. Nevertheless, incorporation of other elements besides vanadium into this structural type has not been reported yet. In particular, substitution of one or more vanadium atoms by Pt^IV (Lee et al., 2008; Joo et al., 2011), Mo^VI(Strukan et al., 1997) and Te^VI (Konaka et al., 2008; Konaka et al., 2011) are investigated and resulted into novel materials with highly promising catalytic properties. To date in our knowledge, only two POVs incorporated one telluric, are known (Konaka et al., 2008). Here, we describe the synthesis and structure of the first ocatavanado-ditellurate ion, [Te₂V₈O₂₈]^4-, which was isolated as the hydrated quinolinium salt (C₉H₈N)₄[Te₂V₈O₂₈]·8H₂O (I). The asymmetric unit of (I) contains one half of a [Te₂V₈O₂₈]^4- anion, two crystallographically independent quinolinium cations and four water molecules. Owing to the inversion symmetry, the whole polyanion is generated, resulting so to the title compound formulae (Fig. 1). The structure of the [Te₂V₈O₂₈]^4- polyanion is basically the same as that of decavanadate, [V₁₀O₂₈]^6- (Evans et al., 1966). In [Te₂V₈O₂₈]^4- anion two of the central V atoms of [V₁₀O₂₈]^6- are replaced with two Te atoms. The valence bond calculation (Brown & Altermatt, 1985) gives effective bond valences of 6.1647 for Te cation and of 5.0743, 5.0068, 5.0574 and 5.063 for the four independent V cations, consistent with their oxidation states Te(+VI) and V(+V). Replacement of central V atom with a heteroatom, has also been observed for [H₂PtV₉O₂₈]^5- (Lee et al.,2008; Joo et al., 2011). As for the decavanadate anion, the [Te₂V₈O₂₈]^4- anion is built up of 10 e dge sharing MO₆ (M = V or Te) octahedra. Within VO₆ octahedra, the V—O distances are also similar to those already observed and depend upon the type of oxo ligand: bond lengths to the terminal oxo oxygen V—Ot are between 1.602 (7) and 1.610 (6) Å, V—O2b bond lengths to the oxygen bonded to two V atoms vary from 1.767 (6) e t 1.864 (6) Å, V—O3b bond lengths to the oxygen bonded to three V atoms are 2.005 (7) and 2.039 (7) and finally, V—O6c bond lengths to the oxygen shared between six V atoms are 2.380 (7) and 2.387 (7) Å. The VO₆ octahedra are significantly distorted, with the bond angles at the V atoms ranging from 73.5 (3) to 176.5 (3)°. The TeO₆ octahedra are less distorted in comparison with VO₆ ocathedra since the Te—O distances vary from 1.765 (6) to 2.080 (7) Å. Similar trends are also observable for similar heteropolyanion (Konaka et al., 2008; Konaka et al., 2011). The quinolinium cations exhibit the typical ranges in bond lengths and angles as found in the related structures (Hemissi et al., 2010).

In the crystal packing, the discrete [Te₂V₈O₂₈]^4- polyanions are hydrogen bonded through clusters of eight water molecules [H₂O]₈ forming layers [Te₂V₈O₂₈(H₂O)₈]_n⁴ⁿ^- stacked along the [100] direction (Fig. 2). With regard to the organic moieties, the two crystallographically independent [C₉H₇—N(1)H]⁺ and [C₉H₇—N(2)H]⁺ cations are interconnected thanks to intermolecular π ···π stacking interactions with centroid-centroid ring separations between 3.54 (8) and 3.90 (7) Å as to develop chains extending along [011] direction. Furthermore, the quinolinium chains and the polyanion sheets are linked thanks to O1W, O2W water molecules and terminal oxygen atoms (O1, O5 and O9) and bridged oxygen atoms (µ 2-O6, µ 2-O13, µ 2-O14 and µ 3-O4) of the polyanion, into a three dimensional network by N—H···O and C—H···O hydrogen bonds with donor—acceptor distances ranging from 2.700 (11) to 3.411 (13) Å.

Related literature top

For applications of polyoxometallates, see: Fukuda et al. (1997); Rajakumar et al. (2000); Folbergrova et al. (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); Konaka et al. (2011); Evans et al. (1966); Hemissi et al. (2010).

Experimental top

Vanadium (V) oxide (1.26 g, 6.93 mmol), quinoline (0.74 ml, 6.16 mmol) and telluric acid Te(OH)₆ (0.36 g, 1.55 mmol) were dissolved in a mixture of 30 ml of distilled water and 10 ml of ethanol and then stirred for 3 h. Yellow single crystals were obtained after one week by slow evaporation at room temperature.

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS (Enraf–Nonius, 1994); 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).

Figures top

	Fig. 1. An ORTEP view of (I) with displacement ellipsoids drawn at the 30% probability level. Hydrogen bonds are represented as dashed lines. [Symmetry code: (i) 1 - x, 1 - y, - z]
	Fig. 2. Structure projection of (I) along the [001] direction. The π ···π stacking interaction are represented as yellow dashed lines and the hydrogen bonds by red ones. The H-atoms not involved in H-bonding are omitted.

Tetraquinolinium ditelluro(VI)octavanadate(V) octahydrate top

Crystal data top

(C₉H₈N)₄[Te₂V₈O₂₈]·8H₂O	Z = 1
M_r = 1775.50	F(000) = 868
Triclinic, P1	D_x = 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

Data collection top

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

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)] = 0.115	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(F_o²) + (0.0978P)² + 22.5177P] where P = (F_o² + 2F_c²)/3
13245 reflections	(Δ/σ)_max < 0.001
385 parameters	Δρ_max = 3.11 e Å⁻³
20 restraints	Δρ_min = −2.28 e Å⁻³

Crystal data top

(C₉H₈N)₄[Te₂V₈O₂₈]·8H₂O	γ = 105.34 (4)°
M_r = 1775.50	V = 1369.4 (6) Å³
Triclinic, P1	Z = 1
a = 10.907 (3) Å	Ag Kα radiation, λ = 0.56087 Å
b = 11.302 (3) Å	µ = 1.28 mm⁻¹
c = 13.169 (2) Å	T = 295 K
α = 106.45 (4)°	0.19 × 0.15 × 0.09 mm
β = 107.71 (4)°

Data collection top

Enraf–Nonius CAD-4 diffractometer	6549 reflections with I > 2σ(I)
Absorption correction: analytical (Alcock, 1970)	R_int = 0.045
T_min = 0.561, T_max = 0.725	2 standard reflections every 120 min
16455 measured reflections	intensity decay: 4%
13245 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.115	20 restraints
wR(F²) = 0.308	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.0978P)² + 22.5177P] where P = (F_o² + 2F_c²)/3
13245 reflections	Δρ_max = 3.11 e Å⁻³
385 parameters	Δρ_min = −2.28 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	U_iso*/U_eq
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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

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···O4W^iv	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···O1W^v	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···O13^vi	0.93	2.48	3.178 (14)	132
C7—H7···O1^vii	0.93	2.56	3.350 (13)	143
C7—H7···O2W^viii	0.93	2.57	3.296 (14)	135
C10—H10···O9^ix	0.93	2.51	3.275 (13)	140
C14—H14···O4^x	0.93	2.58	3.403 (14)	148
C17—H17···O5	0.93	2.60	3.411 (13)	146

Symmetry codes: (ii) −x, −y, −z+1; (iii) x+1, y, z+1; (iv) −x+2, −y, −z+2; (v) x+1, y, z; (vi) −x+1, −y+1, −z+2; (vii) x, y−1, z; (viii) x−1, y, z; (ix) −x+1, −y+1, −z+1; (x) −x+1, −y+2, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W1···O2ⁱ	0.845 (5)	1.819 (5)	2.663 (8)	177.8 (6)
O1W—H1W1···O7	0.853 (10)	1.919 (18)	2.762 (9)	170 (4)
O2W—H1W2···O8ⁱⁱ	0.849 (10)	2.03 (2)	2.842 (10)	159 (4)
O2W—H2W2···O4Wⁱⁱⁱ	0.849 (7)	2.104 (12)	2.952 (14)	177.3 (9)
O3W—H2W3···O4W	0.844 (7)	1.910 (11)	2.754 (14)	177.3 (9)
O3W—H1W3···O6ⁱⁱ	0.850 (10)	1.83 (2)	2.665 (11)	166 (6)
O4W—H2W4···O1W^iv	0.849 (10)	2.41 (3)	2.826 (12)	111 (3)
O4W—H1W4···O2W	0.850 (10)	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···O13^v	0.93	2.48	3.178 (14)	132
C7—H7···O1^vi	0.93	2.56	3.350 (13)	143
C7—H7···O2W^vii	0.93	2.57	3.296 (14)	135
C10—H10···O9^viii	0.93	2.51	3.275 (13)	140
C14—H14···O4^ix	0.93	2.58	3.403 (14)	148
C17—H17···O5	0.93	2.60	3.411 (13)	146

Symmetry codes: (i) −x, −y, −z+1; (ii) x+1, y, z+1; (iii) −x+2, −y, −z+2; (iv) x+1, y, z; (v) −x+1, −y+1, −z+2; (vi) x, y−1, z; (vii) x−1, y, z; (viii) −x+1, −y+1, −z+1; (ix) −x+1, −y+2, −z+1.

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Volume 69| Part 11| November 2013| Pages m595-m596

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