Hexakis(tetra­aqua­sodium) deca­vanadate(V) dihydrate

Nilsson, J.; Nordlander, E.; Behrens, U.; Rehder, D.

doi:10.1107/S1600536810010251

inorganic compounds

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ISSN: 2056-9890

Volume 66| Part 4| April 2010| Pages i30-i31

doi:10.1107/S1600536810010251

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Hexakis(tetraaquasodium) decavanadate(V) dihydrate

Jessica Nilsson,^a Ebbe Nordlander,^a Ulrich Behrens ^b and Dieter Rehder ^b ^*

^aInorganic Chemistry Research Group, Chemical Physics, Center for Chemistry and Chemical Engineering, Lund University, SE-22100 Lund, Sweden, and ^bChemistry Department, University of Hamburg, D-20146 Hamburg, Germany
^*Correspondence e-mail: rehder@chemie.uni-hamburg.de

(Received 9 March 2010; accepted 18 March 2010; online 24 March 2010)

The title compound, {[Na(H₂O)₄]₆[V₁₀O₂₈]·2H₂O}_n, crystallized from a H₂O/THF/CH₃CN solution (pH ca 6) containing equimolar amounts of NaVO₃ and N-(2-hydroxybenzyl)-N-(2-picolyl)glycine. In the crystal structure, the decavanadate [V₁₀O₂₈]⁶⁻ anion ( $[\overline1]$ symmetry) is coordinated, via four terminal oxide ligands of V centres, to two dinuclear [{Na(H₂O)₃}₂(μ-H₂O)₂]²⁺ units. Interconnection of these aquasodium-ion-sandwiched decavanadates to chains parallel to [001] is effected by μ-[{Na(H₂O)₃}₂(μ-H₂O)₂]²⁺ units, bridging adjacent decavanadates via O=V. The structure is consolidated by an extensive network of O—H⋯O hydrogen bonds.

Related literature

Decavanadates with hydrated inorganic cations (Na⁺, K⁺), though with different molecular and supramolecular arrangements from that in the title structure, have been reported by, for example, Durif et al. (1980 ); Matias et al. (2000 ); Lee & Joo (2003 ); Wang et al. (2003 ); Guo & Yao (2007 ). More common are deca- and other polyoxidovanadates with organic counter-ions such as glycyl-glycinium (Crans et al., 1994 ) or cryptands and related macrocyclic O_xN₂ cations (Farahbakhsh et al., 1998 ; Wang et al., 2003). For the impact of decavanadates as building blocks for supermolecular assemblies, see: Ferreira da Silva et al. (2003 ). For the interaction of decavanadate with reverse micelles, see: Baruah et al. (2006 ).

Experimental

Crystal data

[Na(H₂O)₄]₆[V₁₀O₂₈]·2H₂O
M_r = 1563.76
Triclinic, $[P \overline 1]$
a = 9.6144 (9) Å
b = 11.7260 (11) Å
c = 11.8691 (11) Å
α = 92.446 (1)°
β = 113.582 (1)°
γ = 100.274 (1)°
V = 1197.01 (19) Å³
Z = 1
Mo Kα radiation
μ = 2.05 mm⁻¹
T = 100 K
0.50 × 0.24 × 0.10 mm

Data collection

Bruker SMART diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005 ) T_min = 0.428, T_max = 0.822
7584 measured reflections
5049 independent reflections
4621 reflections with I > 2σ(I)
R_int = 0.010

Refinement

R[F² > 2σ(F²)] = 0.022
wR(F²) = 0.057
S = 1.06
5049 reflections
396 parameters
39 restraints
H-atom parameters constrained
Δρ_max = 0.36 e Å⁻³
Δρ_min = −0.42 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O15—H15B⋯O19ⁱ	0.84 (2)	2.04 (2)	2.862 (2)	169 (3)
O16—H16B⋯O18ⁱⁱ	0.84 (2)	1.99 (2)	2.820 (2)	171 (2)
O17—H17A⋯O13ⁱⁱ	0.84 (2)	1.99 (2)	2.816 (2)	166 (3)
O17—H17B⋯O10ⁱ	0.84 (2)	2.01 (2)	2.837 (2)	168 (3)
O18—H18A⋯O4ⁱⁱⁱ	0.84 (3)	1.98 (3)	2.815 (2)	176 (2)
O18—H18B⋯O22^iv	0.84 (2)	2.01 (2)	2.822 (2)	164 (2)
O19—H19A⋯O5ⁱ	0.84 (2)	1.97 (2)	2.804 (2)	175 (2)
O20—H20A⋯O14^v	0.84 (2)	2.02 (2)	2.846 (2)	170 (2)
O20—H20B⋯O6^vi	0.84 (2)	1.91 (2)	2.724 (2)	164 (2)
O22—H22A⋯O27^v	0.84 (2)	1.93 (2)	2.752 (2)	168 (2)
O23—H23B⋯O7^vii	0.84 (2)	1.86 (2)	2.694 (2)	173 (2)
O25—H25A⋯O23^viii	0.84 (2)	1.88 (2)	2.706 (2)	170 (3)
O25—H25B⋯O27^ix	0.84 (2)	1.99 (2)	2.810 (3)	167 (2)
O26—H26A⋯O21^viii	0.84 (2)	1.97 (2)	2.796 (2)	167 (3)
Symmetry codes: (i) -x, -y+1, -z; (ii) -x+1, -y+1, -z; (iii) x, y, z-1; (iv) -x, -y, -z; (v) x-1, y, z; (vi) -x, -y, -z+1; (vii) -x+1, -y, -z+1; (viii) -x+1, -y, -z; (ix) -x+2, -y, -z.

Data collection: SMART (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810010251/br2141sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810010251/br2141Isup2.hkl

checkCIF report

Comment top

Decavanadates H_nV₁₀O₂₈^(6-n)- (n = 0-3) form in aqueous solutions containing vanadates (mainly mono- and diprotonated mono- and divanadate, cyclic tetra- and pentavanadate) at a pH < 6.3 and sufficiently high concentrations (> ca. 1 mM, depending on the ionic strength of the medium). In the pH range 4.5 to 6.3, HV₁₀O₂₈^5- is the major species, coexistent with minor amounts of V₁₀O₂₈^6-. Stabilisation by organic counter-ions can extend the range of stability of decavanadates into the alkaline regime (Wang et al., 2003). The centro-symmetric decavanadate contains three distinct types of vanadium centres: The eight peripheral vanadium ions, Va [O=V(µ-O)₂(µ₃-O)₂(µ₆-O)] and Vb [O=V(µ-O)₄(µ₆-O)] carry one terminal and five bridging oxido ligands, while the two central Vc type vanadium ions are hexa-coordinated by bridging oxygens.

The title compound shows a unique interaction between the decavanadate and dinuclear aquasodium counterions: The structure comprises a discrete non-protonated decavanadate anion [V₁₀O₂₈]^6-, sandwiched by two [{Na(H₂O)₃}₂(µ-H₂O)₂]²⁺ cations via aqua ligands, and further connected to chains by bridging [{Na(H₂O)₃}₂(µ-H₂O)₂]²⁺ cations (Figs. 1, 2 and 3). The sandwiching dinuclear aquasodium cations coordinate to the oxido ligands O1 and O2 of the four Va type vanadium ions (V2 and V3) of the decavanadate, while two opposed O=Vb groups (O3=V4) participate in the chain construction; the second O=Vb group, O14=V5, is not involved in direct bonding. The oxygen O14 is, however, hydrogen bonded to the aqua ligand H20a (O14···H20a = 2.017 Å). In addition, there are two molecules of water of hydration (O27) which are hydrogen bonded to one of the aqua ligands (H27b···O25 = 1.912 Å) and weakly hydrogen bonded to the doubly bridging O9 of decavanadate (H27a···O9 = 2.197 Å).

Related literature top

Decavanadates with hydrated inorganic cations (Na⁺, K⁺), though with different molecular and supramolecular arrangements from that in the title structure, have been reported by, for example, Durif et al. (1980); Matias et al. (2000); Lee & Joo (2003); Wang et al. (2003); Guo & Yao (2007). More common are deca- and other polyoxidovanadates with organic counter-ions such as glycyl-glycinium (Crans et al., 1994) or cryptands and related macrocyclic O_xN₂ cations (Farahbakhsh et al., 1998; Wang et al., 2003). For the impact of decavanadates as building blocks for supermolecular assemblies, see: Ferreira da Silva et al. (2003). For the interaction of decavanadate with reverse micelles, see: Baruah et al. (2006).

Experimental top

NaVO₃ (0.07 g, 0.55 mmol) and N-(2-hydroxibenzyl)-N-(2-picolyl)-glycine (H₂L; 0.15 g, 0.55 mmol) were dissolved in 10 ml of deionised water/THF 9:1 and stirred at room temp. for three hours. The ⁵¹V NMR showed the presence of H₂VO₄^-, H₂V₂O₇^2-, V₄O₁₂^4-, V₅O₁₅^5- and an oxidovanadium complex of L^2-. The solvent volume was reduced to 3 ml, layered with CH₃CN, and kept at 8 °C. Yellow crystals of the title compound formed within a week.

Computing details top

Data collection: SMART (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. An ORTEP view (50% probability level; hydrogen atoms omitted) of the decavanadate(6-) anion with its sandwiching and bridging [{Na(H₂O)₃}₂(µ-H₂O)₂]²⁺ counter-ions.
	Fig. 2. Polygonal representation of a three-membered chain section. The decavanadates are shown in blue, the [{Na(H₂O)₃}₂(µ-H₂O)₂]²⁺ counter-ions in yellow.
	Fig. 3. Detail view of the µ-[{Na(H₂O)₃}₂(µ-H₂O)₂]²⁺ unit connecting two decavanadates via O4 and O4a.

Hexakis(tetraaquasodium) decavanadate(V) dihydrate top

Crystal data top

[Na(H₂O)₄]₆[V₁₀O₂₈]·2H₂O	Z = 1
M_r = 1563.76	F(000) = 780
Triclinic, P1	D_x = 2.169 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.6144 (9) Å	Cell parameters from 4566 reflections
b = 11.7260 (11) Å	θ = 4.7–55.9°
c = 11.8691 (11) Å	µ = 2.05 mm⁻¹
α = 92.446 (1)°	T = 100 K
β = 113.582 (1)°	Block, orange
γ = 100.274 (1)°	0.50 × 0.24 × 0.10 mm
V = 1197.01 (19) Å³

Data collection top

Bruker SMART diffractometer	5049 independent reflections
Radiation source: fine-focus sealed tube	4621 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.010
ω–scan	θ_max = 27.5°, θ_min = 2.8°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −11→12
T_min = 0.428, T_max = 0.822	k = −14→15
7584 measured reflections	l = −15→8

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.022	H-atom parameters constrained
wR(F²) = 0.057	w = 1/[σ²(F_o²) + (0.0224P)² + 1.1216P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.001
5049 reflections	Δρ_max = 0.36 e Å⁻³
396 parameters	Δρ_min = −0.42 e Å⁻³
39 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0004 (2)

Crystal data top

[Na(H₂O)₄]₆[V₁₀O₂₈]·2H₂O	γ = 100.274 (1)°
M_r = 1563.76	V = 1197.01 (19) Å³
Triclinic, P1	Z = 1
a = 9.6144 (9) Å	Mo Kα radiation
b = 11.7260 (11) Å	µ = 2.05 mm⁻¹
c = 11.8691 (11) Å	T = 100 K
α = 92.446 (1)°	0.50 × 0.24 × 0.10 mm
β = 113.582 (1)°

Data collection top

Bruker SMART diffractometer	5049 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2005)	4621 reflections with I > 2σ(I)
T_min = 0.428, T_max = 0.822	R_int = 0.010
7584 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.022	39 restraints
wR(F²) = 0.057	H-atom parameters constrained
S = 1.06	Δρ_max = 0.36 e Å⁻³
5049 reflections	Δρ_min = −0.42 e Å⁻³
396 parameters

Special details top

Experimental. Crystals were grown from a solution of sodiumvanadate in water-THF-methanol

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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. O—H lengths were fixed to 0.84 A, H—O—H angles to 104.5 degrees.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
V1	0.32866 (3)	0.49894 (2)	0.49773 (3)	0.00662 (7)
V2	0.36691 (3)	0.43084 (2)	0.25206 (3)	0.00734 (7)
V3	0.52081 (3)	0.31293 (2)	0.62715 (3)	0.00707 (7)
V4	0.22632 (3)	0.24259 (2)	0.37700 (3)	0.00789 (7)
V5	0.54694 (3)	0.24381 (3)	0.38087 (3)	0.00819 (7)
Na1	0.68380 (9)	0.20347 (7)	−0.04171 (7)	0.01458 (16)
Na2	0.00968 (8)	−0.06905 (6)	0.36995 (7)	0.01258 (15)
Na3	0.20510 (8)	0.51845 (6)	−0.09634 (7)	0.01183 (15)
O1	0.30955 (15)	0.47278 (11)	0.11639 (11)	0.0112 (3)
O2	0.57790 (15)	0.27004 (11)	0.76214 (12)	0.0117 (3)
O3	0.06723 (14)	0.14613 (11)	0.33464 (12)	0.0116 (3)
O4	0.43595 (14)	0.44985 (10)	0.65664 (11)	0.0074 (2)
O5	0.30505 (14)	0.54867 (10)	0.34087 (11)	0.0078 (2)
O6	0.32409 (14)	0.22657 (10)	0.54530 (11)	0.0089 (2)
O7	0.60556 (14)	0.22842 (10)	0.54878 (11)	0.0089 (2)
O8	0.47848 (14)	0.32382 (10)	0.24227 (11)	0.0091 (2)
O9	0.19622 (14)	0.32182 (10)	0.23905 (11)	0.0091 (2)
O10	0.17201 (14)	0.38447 (10)	0.44432 (11)	0.0092 (2)
O11	0.35146 (14)	0.16030 (10)	0.34055 (11)	0.0093 (2)
O12	0.45138 (13)	0.38945 (10)	0.44775 (11)	0.0072 (2)
O13	0.72840 (14)	0.38759 (11)	0.45042 (11)	0.0091 (2)
O14	0.63150 (15)	0.15212 (11)	0.34249 (12)	0.0134 (3)
O15	0.08001 (15)	0.64704 (12)	−0.03043 (12)	0.0139 (3)
O16	0.43615 (15)	0.66748 (12)	−0.03469 (12)	0.0136 (3)
O17	0.13702 (16)	0.61325 (13)	−0.27889 (12)	0.0163 (3)
O18	0.31590 (15)	0.38521 (11)	−0.16898 (12)	0.0128 (3)
O19	−0.03436 (15)	0.37867 (12)	−0.19183 (12)	0.0139 (3)
O20	−0.18096 (15)	−0.01604 (11)	0.42273 (12)	0.0117 (3)
O21	0.76870 (16)	0.15411 (13)	0.15731 (13)	0.0178 (3)
O22	−0.20085 (16)	−0.14460 (12)	0.17792 (13)	0.0178 (3)
O23	0.23048 (15)	−0.07292 (11)	0.33278 (12)	0.0128 (3)
O24	0.01105 (16)	−0.26635 (12)	0.41579 (13)	0.0163 (3)
O25	0.83366 (19)	0.08376 (13)	−0.08832 (14)	0.0236 (3)
O26	0.47074 (19)	0.03597 (14)	−0.12596 (16)	0.0294 (4)
O27	0.8411 (2)	−0.14147 (13)	−0.03821 (14)	0.0281 (4)
H15A	0.0004 (18)	0.657 (2)	−0.0896 (15)	0.0406 (17)*
H15B	0.055 (3)	0.642 (2)	0.0294 (14)	0.0406 (17)*
H16A	0.459 (3)	0.670 (2)	−0.0956 (14)	0.0406 (17)*
H16B	0.509 (2)	0.646 (2)	0.0210 (16)	0.0406 (17)*
H17A	0.178 (2)	0.601 (3)	−0.3279 (17)	0.0406 (17)*
H17B	0.0421 (8)	0.605 (3)	−0.3240 (18)	0.0406 (17)*
H18A	0.349 (3)	0.402 (2)	−0.2226 (19)	0.0406 (17)*
H18B	0.273 (3)	0.3144 (7)	−0.187 (2)	0.0406 (17)*
H19A	−0.112 (2)	0.404 (2)	−0.2358 (18)	0.0406 (17)*
H19B	−0.020 (3)	0.334 (2)	−0.2412 (17)	0.0406 (17)*
H20A	−0.238 (2)	0.0307 (16)	0.391 (2)	0.0406 (17)*
H20B	−0.241 (2)	−0.0771 (13)	0.423 (3)	0.0406 (17)*
H21A	0.8521 (17)	0.131 (2)	0.191 (2)	0.0406 (17)*
H21B	0.785 (3)	0.2171 (14)	0.201 (2)	0.0406 (17)*
H22A	−0.202 (3)	−0.148 (2)	0.1070 (11)	0.0406 (17)*
H22B	−0.279 (2)	−0.118 (2)	0.170 (2)	0.0406 (17)*
H23A	0.287 (2)	−0.0058 (9)	0.351 (2)	0.0406 (17)*
H23B	0.287 (2)	−0.1167 (16)	0.373 (2)	0.0406 (17)*
H24A	0.0900 (17)	−0.291 (2)	0.460 (2)	0.0406 (17)*
H24B	−0.0612 (19)	−0.304 (2)	0.431 (2)	0.0406 (17)*
H25A	0.824 (3)	0.085 (2)	−0.1616 (8)	0.0406 (17)*
H25B	0.9284 (10)	0.109 (2)	−0.0442 (18)	0.0406 (17)*
H26A	0.410 (3)	−0.0259 (12)	−0.128 (3)	0.0406 (17)*
H26B	0.519 (3)	0.015 (2)	−0.166 (2)	0.0406 (17)*
H27A	0.804 (3)	−0.1880 (16)	−0.1037 (13)	0.0406 (17)*
H27B	0.827 (3)	−0.0763 (10)	−0.061 (2)	0.0406 (17)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.00643 (14)	0.00731 (14)	0.00662 (14)	0.00154 (11)	0.00308 (11)	0.00185 (11)
V2	0.00903 (14)	0.00742 (14)	0.00493 (14)	0.00141 (11)	0.00236 (11)	0.00133 (10)
V3	0.00797 (14)	0.00698 (14)	0.00611 (14)	0.00169 (11)	0.00257 (11)	0.00235 (10)
V4	0.00671 (14)	0.00731 (14)	0.00883 (15)	0.00045 (11)	0.00281 (11)	0.00129 (11)
V5	0.00842 (14)	0.00770 (14)	0.00935 (15)	0.00218 (11)	0.00441 (12)	0.00113 (11)
Na1	0.0139 (4)	0.0171 (4)	0.0115 (4)	0.0026 (3)	0.0042 (3)	0.0041 (3)
Na2	0.0119 (4)	0.0134 (3)	0.0121 (4)	0.0025 (3)	0.0049 (3)	0.0001 (3)
Na3	0.0108 (3)	0.0148 (3)	0.0101 (4)	0.0029 (3)	0.0044 (3)	0.0030 (3)
O1	0.0128 (6)	0.0117 (6)	0.0076 (6)	0.0016 (5)	0.0031 (5)	0.0019 (5)
O2	0.0140 (6)	0.0114 (6)	0.0107 (6)	0.0031 (5)	0.0055 (5)	0.0040 (5)
O3	0.0094 (6)	0.0107 (6)	0.0129 (6)	0.0007 (5)	0.0032 (5)	0.0025 (5)
O4	0.0078 (6)	0.0085 (6)	0.0068 (6)	0.0017 (5)	0.0041 (5)	0.0017 (4)
O5	0.0076 (6)	0.0093 (6)	0.0063 (6)	0.0020 (5)	0.0026 (5)	0.0022 (4)
O6	0.0081 (6)	0.0089 (6)	0.0095 (6)	0.0004 (5)	0.0037 (5)	0.0028 (5)
O7	0.0101 (6)	0.0080 (6)	0.0096 (6)	0.0026 (5)	0.0046 (5)	0.0023 (5)
O8	0.0107 (6)	0.0101 (6)	0.0078 (6)	0.0022 (5)	0.0051 (5)	0.0013 (5)
O9	0.0088 (6)	0.0087 (6)	0.0083 (6)	0.0010 (5)	0.0026 (5)	0.0013 (5)
O10	0.0072 (6)	0.0107 (6)	0.0095 (6)	0.0014 (5)	0.0034 (5)	0.0019 (5)
O11	0.0105 (6)	0.0080 (6)	0.0093 (6)	0.0015 (5)	0.0040 (5)	0.0013 (5)
O12	0.0078 (6)	0.0081 (5)	0.0066 (6)	0.0017 (5)	0.0038 (5)	0.0023 (4)
O13	0.0084 (6)	0.0117 (6)	0.0085 (6)	0.0030 (5)	0.0043 (5)	0.0027 (5)
O14	0.0154 (7)	0.0131 (6)	0.0150 (7)	0.0057 (5)	0.0085 (5)	0.0029 (5)
O15	0.0127 (6)	0.0182 (7)	0.0114 (7)	0.0040 (5)	0.0053 (5)	0.0026 (5)
O16	0.0102 (6)	0.0210 (7)	0.0104 (6)	0.0048 (5)	0.0045 (5)	0.0038 (5)
O17	0.0118 (6)	0.0279 (8)	0.0114 (7)	0.0073 (6)	0.0057 (5)	0.0055 (6)
O18	0.0137 (7)	0.0141 (6)	0.0124 (7)	0.0023 (5)	0.0073 (5)	0.0025 (5)
O19	0.0105 (6)	0.0175 (7)	0.0132 (7)	0.0040 (5)	0.0040 (5)	0.0021 (5)
O20	0.0114 (6)	0.0105 (6)	0.0141 (7)	0.0019 (5)	0.0060 (5)	0.0039 (5)
O21	0.0152 (7)	0.0238 (7)	0.0142 (7)	0.0064 (6)	0.0049 (6)	0.0050 (6)
O22	0.0181 (7)	0.0187 (7)	0.0145 (7)	0.0034 (6)	0.0046 (6)	0.0019 (6)
O23	0.0132 (6)	0.0101 (6)	0.0160 (7)	0.0040 (5)	0.0060 (5)	0.0039 (5)
O24	0.0136 (7)	0.0182 (7)	0.0166 (7)	0.0032 (5)	0.0056 (6)	0.0052 (5)
O25	0.0362 (9)	0.0216 (7)	0.0160 (7)	0.0114 (7)	0.0117 (7)	0.0039 (6)
O26	0.0223 (8)	0.0300 (9)	0.0292 (9)	−0.0075 (7)	0.0096 (7)	−0.0008 (7)
O27	0.0489 (10)	0.0138 (7)	0.0126 (7)	−0.0018 (7)	0.0074 (7)	−0.0008 (6)

Geometric parameters (Å, º) top

V1—O13ⁱ	1.7061 (12)	V5—O7	1.8682 (13)
V1—O10	1.7071 (12)	V5—O8	1.8722 (13)
V1—O5	1.9130 (12)	V5—O13	2.0609 (13)
V1—O4	1.9237 (12)	V5—O12	2.3278 (12)
V1—O12	2.1042 (12)	V5—V1ⁱ	3.0935 (5)
V1—O12ⁱ	2.1094 (12)	Na1—O21	2.3073 (16)
V1—V4	3.0832 (5)	Na1—O2ⁱⁱ	2.3682 (14)
V1—V5ⁱ	3.0935 (5)	Na1—O25	2.3760 (17)
V2—O1	1.6102 (13)	Na1—O16ⁱⁱⁱ	2.4051 (15)
V2—O8	1.8184 (12)	Na1—O26	2.4108 (17)
V2—O9	1.8393 (12)	Na1—O15ⁱⁱⁱ	2.4205 (16)
V2—O4ⁱ	2.0014 (12)	Na1—Na3ⁱⁱⁱ	3.3703 (11)
V2—O5	2.0110 (12)	Na2—O20	2.3303 (15)
V2—O12	2.2400 (12)	Na2—O23	2.3419 (15)
V2—V3ⁱ	3.0798 (5)	Na2—O22	2.3608 (16)
V2—V5	3.1090 (4)	Na2—O20^iv	2.3926 (15)
V2—V4	3.1173 (4)	Na2—O24	2.4003 (15)
V3—O2	1.6078 (13)	Na2—O3	2.5741 (15)
V3—O6	1.8191 (12)	Na2—Na2^iv	3.5112 (15)
V3—O7	1.8240 (12)	Na3—O18	2.3522 (15)
V3—O4	2.0034 (12)	Na3—O15	2.3730 (15)
V3—O5ⁱ	2.0126 (12)	Na3—O19	2.3831 (15)
V3—O12	2.2414 (12)	Na3—O17	2.3852 (15)
V3—V2ⁱ	3.0798 (5)	Na3—O16	2.3937 (16)
V3—V5	3.1181 (5)	Na3—O1	2.4391 (14)
V4—O3	1.6095 (13)	Na3—Na1ⁱⁱⁱ	3.3704 (11)
V4—O11	1.8333 (12)	O2—Na1^v	2.3682 (14)
V4—O9	1.8640 (13)	O4—V2ⁱ	2.0014 (12)
V4—O6	1.8713 (13)	O5—V3ⁱ	2.0126 (12)
V4—O10	2.0516 (13)	O12—V1ⁱ	2.1094 (12)
V4—O12	2.3337 (12)	O13—V1ⁱ	1.7061 (12)
V4—V5	3.0620 (5)	O15—Na1ⁱⁱⁱ	2.4205 (16)
V5—O14	1.6095 (13)	O16—Na1ⁱⁱⁱ	2.4051 (15)
V5—O11	1.8177 (13)	O20—Na2^iv	2.3926 (15)

O13ⁱ—V1—O10	106.37 (6)	O11—V5—V1ⁱ	125.15 (4)
O13ⁱ—V1—O5	96.99 (6)	O7—V5—V1ⁱ	77.89 (4)
O10—V1—O5	97.54 (6)	O8—V5—V1ⁱ	78.58 (4)
O13ⁱ—V1—O4	97.07 (6)	O13—V5—V1ⁱ	31.20 (3)
O10—V1—O4	96.89 (6)	O12—V5—V1ⁱ	42.97 (3)
O5—V1—O4	156.12 (5)	V4—V5—V1ⁱ	91.989 (11)
O13ⁱ—V1—O12	165.75 (6)	O14—V5—V2	135.42 (5)
O10—V1—O12	87.88 (5)	O11—V5—V2	82.17 (4)
O5—V1—O12	80.69 (5)	O7—V5—V2	123.05 (4)
O4—V1—O12	80.93 (5)	O8—V5—V2	32.07 (4)
O13ⁱ—V1—O12ⁱ	87.52 (5)	O13—V5—V2	81.70 (3)
O10—V1—O12ⁱ	166.10 (5)	O12—V5—V2	45.93 (3)
O5—V1—O12ⁱ	80.97 (5)	V4—V5—V2	60.678 (10)
O4—V1—O12ⁱ	80.46 (5)	V1ⁱ—V5—V2	61.445 (11)
O12—V1—O12ⁱ	78.23 (5)	O14—V5—V3	132.95 (5)
O13ⁱ—V1—V4	145.10 (4)	O11—V5—V3	81.93 (4)
O10—V1—V4	38.74 (4)	O7—V5—V3	31.95 (4)
O5—V1—V4	89.49 (4)	O8—V5—V3	123.26 (4)
O4—V1—V4	89.95 (4)	O13—V5—V3	81.33 (4)
O12—V1—V4	49.15 (3)	O12—V5—V3	45.82 (3)
O12ⁱ—V1—V4	127.38 (3)	V4—V5—V3	60.666 (9)
O13ⁱ—V1—V5ⁱ	38.74 (4)	V1ⁱ—V5—V3	61.256 (9)
O10—V1—V5ⁱ	145.11 (4)	V2—V5—V3	91.526 (12)
O5—V1—V5ⁱ	89.73 (4)	O21—Na1—O2ⁱⁱ	172.30 (6)
O4—V1—V5ⁱ	89.25 (4)	O21—Na1—O25	90.19 (6)
O12—V1—V5ⁱ	127.01 (3)	O2ⁱⁱ—Na1—O25	97.51 (6)
O12ⁱ—V1—V5ⁱ	48.78 (3)	O21—Na1—O16ⁱⁱⁱ	83.28 (5)
V4—V1—V5ⁱ	176.157 (13)	O2ⁱⁱ—Na1—O16ⁱⁱⁱ	89.04 (5)
O1—V2—O8	102.98 (6)	O25—Na1—O16ⁱⁱⁱ	171.59 (6)
O1—V2—O9	102.33 (6)	O21—Na1—O26	93.99 (6)
O8—V2—O9	94.90 (6)	O2ⁱⁱ—Na1—O26	86.67 (6)
O1—V2—O4ⁱ	100.68 (6)	O25—Na1—O26	86.32 (6)
O8—V2—O4ⁱ	90.06 (5)	O16ⁱⁱⁱ—Na1—O26	99.38 (6)
O9—V2—O4ⁱ	154.69 (5)	O21—Na1—O15ⁱⁱⁱ	87.34 (5)
O1—V2—O5	100.31 (6)	O2ⁱⁱ—Na1—O15ⁱⁱⁱ	93.26 (5)
O8—V2—O5	154.79 (5)	O25—Na1—O15ⁱⁱⁱ	84.44 (6)
O9—V2—O5	89.42 (5)	O16ⁱⁱⁱ—Na1—O15ⁱⁱⁱ	89.94 (5)
O4ⁱ—V2—O5	76.19 (5)	O26—Na1—O15ⁱⁱⁱ	170.67 (6)
O1—V2—O12	174.83 (6)	O21—Na1—Na3ⁱⁱⁱ	85.15 (4)
O8—V2—O12	80.85 (5)	O2ⁱⁱ—Na1—Na3ⁱⁱⁱ	89.87 (4)
O9—V2—O12	80.63 (5)	O25—Na1—Na3ⁱⁱⁱ	129.08 (5)
O4ⁱ—V2—O12	75.68 (5)	O16ⁱⁱⁱ—Na1—Na3ⁱⁱⁱ	45.25 (4)
O5—V2—O12	75.36 (5)	O26—Na1—Na3ⁱⁱⁱ	144.54 (5)
O1—V2—V3ⁱ	90.43 (5)	O15ⁱⁱⁱ—Na1—Na3ⁱⁱⁱ	44.75 (4)
O8—V2—V3ⁱ	129.81 (4)	O20—Na2—O23	165.69 (6)
O9—V2—V3ⁱ	129.49 (4)	O20—Na2—O22	83.88 (5)
O4ⁱ—V2—V3ⁱ	39.76 (3)	O23—Na2—O22	104.40 (6)
O5—V2—V3ⁱ	40.07 (4)	O20—Na2—O20^iv	83.96 (5)
O12—V2—V3ⁱ	84.43 (3)	O23—Na2—O20^iv	87.70 (5)
O1—V2—V5	135.86 (5)	O22—Na2—O20^iv	167.80 (6)
O8—V2—V5	33.14 (4)	O20—Na2—O24	104.87 (5)
O9—V2—V5	83.38 (4)	O23—Na2—O24	87.28 (5)
O4ⁱ—V2—V5	87.43 (4)	O22—Na2—O24	88.00 (5)
O5—V2—V5	123.65 (4)	O20^iv—Na2—O24	94.22 (5)
O12—V2—V5	48.30 (3)	O20—Na2—O3	84.71 (5)
V3ⁱ—V2—V5	119.735 (13)	O23—Na2—O3	82.43 (5)
O1—V2—V4	135.06 (5)	O22—Na2—O3	99.54 (5)
O8—V2—V4	83.55 (4)	O20^iv—Na2—O3	80.26 (5)
O9—V2—V4	32.92 (4)	O24—Na2—O3	168.48 (5)
O4ⁱ—V2—V4	123.96 (4)	O20—Na2—Na2^iv	42.66 (4)
O5—V2—V4	86.79 (4)	O23—Na2—Na2^iv	128.01 (5)
O12—V2—V4	48.31 (3)	O22—Na2—Na2^iv	126.53 (5)
V3ⁱ—V2—V4	119.559 (13)	O20^iv—Na2—Na2^iv	41.30 (3)
V5—V2—V4	58.915 (11)	O24—Na2—Na2^iv	102.74 (5)
O2—V3—O6	103.48 (6)	O3—Na2—Na2^iv	79.83 (4)
O2—V3—O7	102.71 (6)	O18—Na3—O15	176.93 (6)
O6—V3—O7	95.00 (6)	O18—Na3—O19	86.84 (5)
O2—V3—O4	100.39 (6)	O15—Na3—O19	90.19 (5)
O6—V3—O4	89.99 (5)	O18—Na3—O17	93.73 (5)
O7—V3—O4	154.50 (5)	O15—Na3—O17	85.47 (5)
O2—V3—O5ⁱ	99.91 (6)	O19—Na3—O17	89.84 (5)
O6—V3—O5ⁱ	154.60 (5)	O18—Na3—O16	91.43 (5)
O7—V3—O5ⁱ	89.34 (5)	O15—Na3—O16	91.37 (5)
O4—V3—O5ⁱ	76.10 (5)	O19—Na3—O16	170.38 (6)
O2—V3—O12	174.75 (6)	O17—Na3—O16	80.82 (5)
O6—V3—O12	80.41 (5)	O18—Na3—O1	94.70 (5)
O7—V3—O12	80.28 (5)	O15—Na3—O1	86.72 (5)
O4—V3—O12	75.92 (5)	O19—Na3—O1	102.83 (5)
O5ⁱ—V3—O12	75.68 (5)	O17—Na3—O1	165.13 (6)
O2—V3—V2ⁱ	90.00 (5)	O16—Na3—O1	86.74 (5)
O6—V3—V2ⁱ	129.69 (4)	O18—Na3—Na1ⁱⁱⁱ	136.94 (4)
O7—V3—V2ⁱ	129.37 (4)	O15—Na3—Na1ⁱⁱⁱ	45.90 (4)
O4—V3—V2ⁱ	39.71 (4)	O19—Na3—Na1ⁱⁱⁱ	135.65 (4)
O5ⁱ—V3—V2ⁱ	40.03 (3)	O17—Na3—Na1ⁱⁱⁱ	81.97 (4)
O12—V3—V2ⁱ	84.78 (3)	O16—Na3—Na1ⁱⁱⁱ	45.52 (4)
O2—V3—V5	135.29 (5)	O1—Na3—Na1ⁱⁱⁱ	83.50 (4)
O6—V3—V5	83.08 (4)	V2—O1—Na3	174.54 (8)
O7—V3—V5	32.82 (4)	V3—O2—Na1^v	174.33 (8)
O4—V3—V5	124.04 (4)	V4—O3—Na2	132.53 (7)
O5ⁱ—V3—V5	87.26 (4)	V1—O4—V2ⁱ	107.65 (6)
O12—V3—V5	48.14 (3)	V1—O4—V3	107.11 (6)
V2ⁱ—V3—V5	119.925 (12)	V2ⁱ—O4—V3	100.53 (5)
O3—V4—O11	102.05 (6)	V1—O5—V2	107.67 (6)
O3—V4—O9	103.67 (6)	V1—O5—V3ⁱ	107.41 (6)
O11—V4—O9	91.64 (6)	V2—O5—V3ⁱ	99.89 (5)
O3—V4—O6	101.25 (6)	V3—O6—V4	115.52 (6)
O11—V4—O6	91.17 (6)	V3—O7—V5	115.23 (6)
O9—V4—O6	153.74 (5)	V2—O8—V5	114.79 (6)
O3—V4—O10	101.85 (6)	V2—O9—V4	114.65 (6)
O11—V4—O10	156.05 (5)	V1—O10—V4	109.89 (6)
O9—V4—O10	84.06 (5)	V5—O11—V4	114.00 (6)
O6—V4—O10	82.86 (5)	V1—O12—V1ⁱ	101.77 (5)
O3—V4—O12	175.93 (6)	V1—O12—V2	93.61 (5)
O11—V4—O12	81.69 (5)	V1ⁱ—O12—V2	93.48 (5)
O9—V4—O12	77.65 (5)	V1—O12—V3	93.23 (5)
O6—V4—O12	76.94 (5)	V1ⁱ—O12—V3	93.28 (5)
O10—V4—O12	74.37 (5)	V2—O12—V3	169.21 (6)
O3—V4—V5	134.88 (5)	V1—O12—V5	169.98 (6)
O11—V4—V5	32.84 (4)	V1ⁱ—O12—V5	88.26 (4)
O9—V4—V5	84.37 (4)	V2—O12—V5	85.77 (4)
O6—V4—V5	83.93 (4)	V3—O12—V5	86.05 (4)
O10—V4—V5	123.22 (4)	V1—O12—V4	87.85 (4)
O12—V4—V5	48.85 (3)	V1ⁱ—O12—V4	170.38 (6)
O3—V4—V1	133.22 (5)	V2—O12—V4	85.91 (4)
O11—V4—V1	124.69 (4)	V3—O12—V4	86.02 (4)
O9—V4—V1	78.79 (4)	V5—O12—V4	82.12 (4)
O6—V4—V1	78.18 (4)	V1ⁱ—O13—V5	110.05 (6)
O10—V4—V1	31.37 (3)	Na3—O15—Na1ⁱⁱⁱ	89.35 (5)
O12—V4—V1	43.00 (3)	Na3—O15—H15A	111.5 (18)
V5—V4—V1	91.854 (11)	Na1ⁱⁱⁱ—O15—H15A	119.1 (19)
O3—V4—V2	135.91 (5)	Na3—O15—H15B	126.4 (18)
O11—V4—V2	81.71 (4)	Na1ⁱⁱⁱ—O15—H15B	105.9 (19)
O9—V4—V2	32.43 (4)	Na3—O16—Na1ⁱⁱⁱ	89.23 (5)
O6—V4—V2	122.73 (4)	Na3—O16—H16A	106.5 (19)
O10—V4—V2	82.14 (4)	Na1ⁱⁱⁱ—O16—H16A	129.7 (17)
O12—V4—V2	45.79 (3)	Na3—O16—H16B	108.6 (19)
V5—V4—V2	60.407 (10)	Na1ⁱⁱⁱ—O16—H16B	114.1 (17)
V1—V4—V2	61.458 (11)	Na3—O17—H17A	118.5 (18)
O14—V5—O11	103.91 (6)	Na3—O17—H17B	116.8 (18)
O14—V5—O7	101.10 (6)	Na3—O18—H18A	120.3 (18)
O11—V5—O7	91.89 (6)	Na3—O18—H18B	120.2 (18)
O14—V5—O8	103.41 (6)	Na3—O19—H19A	116.6 (19)
O11—V5—O8	91.81 (6)	Na3—O19—H19B	103.9 (19)
O7—V5—O8	153.53 (5)	Na2—O20—Na2^iv	96.04 (5)
O14—V5—O13	99.72 (6)	Na2—O20—H20A	128.0 (19)
O11—V5—O13	156.35 (5)	Na2^iv—O20—H20A	107.5 (19)
O7—V5—O13	82.59 (5)	Na2—O20—H20B	108.1 (18)
O8—V5—O13	83.57 (5)	Na2^iv—O20—H20B	110.5 (19)
O14—V5—O12	173.77 (6)	Na1—O21—H21A	122 (2)
O11—V5—O12	82.18 (5)	Na1—O21—H21B	103.8 (19)
O7—V5—O12	77.12 (5)	Na2—O22—H22A	128.5 (18)
O8—V5—O12	77.44 (5)	Na2—O22—H22B	111.2 (18)
O13—V5—O12	74.17 (5)	Na2—O23—H23A	109.7 (19)
O14—V5—V4	137.06 (5)	Na2—O23—H23B	115.3 (19)
O11—V5—V4	33.16 (4)	Na2—O24—H24A	125.2 (18)
O7—V5—V4	84.53 (4)	Na2—O24—H24B	119.5 (17)
O8—V5—V4	84.34 (4)	Na1—O25—H25A	111.3 (19)
O13—V5—V4	123.19 (4)	Na1—O25—H25B	110.5 (19)
O12—V5—V4	49.02 (3)	Na1—O26—H26A	159 (2)
O14—V5—V1ⁱ	130.92 (5)	Na1—O26—H26B	85.0 (17)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y, z−1; (iii) −x+1, −y+1, −z; (iv) −x, −y, −z+1; (v) x, y, z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O15—H15A···O9^vi	0.84 (2)	2.07 (2)	2.912 (2)	178 (2)
O15—H15B···O19^vi	0.84 (2)	2.04 (2)	2.862 (2)	169 (3)
O16—H16A···O8ⁱⁱⁱ	0.84 (2)	2.06 (2)	2.892 (2)	178 (3)
O16—H16B···O18ⁱⁱⁱ	0.84 (2)	1.99 (2)	2.820 (2)	171 (2)
O17—H17A···O13ⁱⁱⁱ	0.84 (2)	1.99 (2)	2.816 (2)	166 (3)
O17—H17B···O10^vi	0.84 (2)	2.01 (2)	2.837 (2)	168 (3)
O18—H18A···O4ⁱⁱ	0.84 (3)	1.98 (3)	2.815 (2)	176 (2)
O18—H18B···O22^vii	0.84 (2)	2.01 (2)	2.822 (2)	164 (2)
O19—H19A···O5^vi	0.84 (2)	1.97 (2)	2.804 (2)	175 (2)
O19—H19B···O24^vii	0.84 (2)	2.23 (2)	3.022 (2)	158 (2)
O20—H20A···O14^viii	0.84 (2)	2.02 (2)	2.846 (2)	170 (2)
O20—H20B···O6^iv	0.84 (2)	1.91 (2)	2.724 (2)	164 (2)
O21—H21A···O3^ix	0.84 (2)	2.06 (2)	2.821 (2)	150 (2)
O21—H21B···O17ⁱⁱⁱ	0.84 (2)	2.03 (2)	2.843 (2)	162 (2)
O22—H22A···O27^viii	0.84 (2)	1.93 (2)	2.752 (2)	168 (2)
O22—H22B···O26^vii	0.84 (2)	2.12 (2)	2.950 (3)	170 (2)
O23—H23A···O11	0.84 (2)	1.96 (2)	2.756 (2)	158 (2)
O23—H23B···O7^x	0.84 (2)	1.86 (2)	2.694 (2)	173 (2)
O24—H24A···O13^x	0.84 (2)	2.19 (2)	3.016 (2)	168 (2)
O24—H24B···O10^iv	0.84 (2)	2.29 (2)	3.072 (2)	155 (2)
O25—H25A···O23^xi	0.84 (2)	1.88 (2)	2.706 (2)	170 (3)
O25—H25B···O27^xii	0.84 (2)	1.99 (2)	2.810 (3)	167 (2)
O26—H26A···O21^xi	0.84 (2)	1.97 (2)	2.796 (2)	167 (3)
O26—H26B···O14^xi	0.84 (3)	2.56 (2)	3.026 (2)	116 (2)
O27—H27A···O9^xi	0.84 (2)	2.20 (2)	2.983 (2)	156 (3)
O27—H27B···O25	0.84 (2)	1.91 (2)	2.739 (2)	169 (2)

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

Experimental details

Crystal data
Chemical formula	[Na(H₂O)₄]₆[V₁₀O₂₈]·2H₂O
M_r	1563.76
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	9.6144 (9), 11.7260 (11), 11.8691 (11)
α, β, γ (°)	92.446 (1), 113.582 (1), 100.274 (1)
V (Å³)	1197.01 (19)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.05
Crystal size (mm)	0.50 × 0.24 × 0.10

Data collection
Diffractometer	Bruker SMART diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2005)
T_min, T_max	0.428, 0.822
No. of measured, independent and observed [I > 2σ(I)] reflections	7584, 5049, 4621
R_int	0.010
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.022, 0.057, 1.06
No. of reflections	5049
No. of parameters	396
No. of restraints	39
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.36, −0.42

Computer programs: SMART (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O15—H15B···O19ⁱ	0.84 (2)	2.04 (2)	2.862 (2)	169 (3)
O16—H16B···O18ⁱⁱ	0.84 (2)	1.99 (2)	2.820 (2)	171 (2)
O17—H17A···O13ⁱⁱ	0.84 (2)	1.99 (2)	2.816 (2)	166 (3)
O17—H17B···O10ⁱ	0.84 (2)	2.01 (2)	2.837 (2)	168 (3)
O18—H18A···O4ⁱⁱⁱ	0.84 (3)	1.98 (3)	2.815 (2)	176 (2)
O18—H18B···O22^iv	0.84 (2)	2.01 (2)	2.822 (2)	164 (2)
O19—H19A···O5ⁱ	0.84 (2)	1.97 (2)	2.804 (2)	175 (2)
O20—H20A···O14^v	0.84 (2)	2.02 (2)	2.846 (2)	170 (2)
O20—H20B···O6^vi	0.84 (2)	1.91 (2)	2.724 (2)	164 (2)
O22—H22A···O27^v	0.84 (2)	1.93 (2)	2.752 (2)	168 (2)
O23—H23B···O7^vii	0.84 (2)	1.86 (2)	2.694 (2)	173 (2)
O25—H25A···O23^viii	0.84 (2)	1.88 (2)	2.706 (2)	170 (3)
O25—H25B···O27^ix	0.84 (2)	1.99 (2)	2.810 (3)	167 (2)
O26—H26A···O21^viii	0.84 (2)	1.97 (2)	2.796 (2)	167 (3)

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

Acknowledgements

This work was supported by the German Academic Exchange Service (DAAD) and the Swedish Research School in Pharmaceutical Sciences. We thank Oliver Schuster, University of Fribourg, for the preparation of Fig. 2.

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