Dieuropium(III) tri­sulfate octahydrate: a redetermination at 120 K

Sarangarajan, T.R.; Panchanatheswaran, K.; Low, J.N.; Glidewell, C.

doi:10.1107/S160053680402608X

inorganic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 60| Part 11| November 2004| Pages i142-i144

https://doi.org/10.1107/S160053680402608X

Dieuropium(III) trisulfate octahydrate: a redetermination at 120 K

Thanjavur Ramabhadran Sarangarajan,^a Krishnaswamy Panchanatheswaran,^b ^* John N. Low ^c ‡ and Christopher Glidewell ^d

^aSchool of Chemical and Biotechnology, Shanmuga Arts, Science, Technology and Research Academy (SASTRA), Tirumalaisamudram, Thanjavur 613 402, India, ^bDepartment of Chemistry, Bharathidasan University, Tiruchirappalli, Tamil Nadu 620 024, India, ^cDepartment of Chemistry, University of Aberdeen, Meston Walk, Old Aberdeen AB24 3UE, Scotland, and ^dSchool of Chemistry, University of St Andrews, Fife KY16 9ST, Scotland
^*Correspondence e-mail: panch_45@yahoo.co.in

(Received 5 October 2004; accepted 14 October 2004; online 30 October 2004)

The title compound, Eu₂(SO₄)₃·8H₂O, crystallizes in space group C2/c, with one of the anions lying on a twofold rotation axis and the other in a general position, and is best formulated as [Eu(H₂O)_4/1(SO₄)_3/3(SO₄)_1/2]₂, where one of the anions lies across a twofold axis. The coordination environment of Eu^III consists of four water molecules and four sulfate ions. All the water molecules and sulfate ions are involved in hydrogen-bonding interactions. The structure is similar to that previously determined at 293 K [Wei & Zheng (2003 ). Z. Kristallogr. New Cryst. Struct. 218, 277–278], but the cell parameters and the interatomic distances are more precise in the present determination.

Comment

Hydrated lanthanide(III) sulfates can adopt a number of different compositions, namely M₂(SO₄)₃·9H₂O, M₂(SO₄)₃·8H₂O, M₂(SO₄)₃·5H₂O and M₂(SO₄)₃·4H₂O, and the octahydrated sulfates of lanthanides Ln^III exist as coordination polymers in which sulfate ions act as bridging bidentate and tridentate ligands; the presence of four coordinated water molecules leads to a coordination number of eight for the lanthanide ion (Wickleder, 2002 ). The unit-cell dimensions for hydrated europium(III) sulfate were reported many years ago (Geller, 1957 ), and the crystal structure, in space group C2/c, has recently been reported using data collected at 293 K (Wei & Zheng, 2003).

We report here the structure at 120 K. The similarity of the unit-cell dimensions and atomic coordinates at 293 and 120 K indicates that the same phase has been utilized in all of these studies. The aims of the present investigation are the determination of more precise metrical parameters and the determination of the extent of hydration. The structure (Table 1 and Fig. 1) indicates the presence of octacoordinate europium, with distorted square antiprismatic coordination by four water molecules, one O atom from a sulfate ion in the μ₂ bonding mode and three O atoms from three different anions in the μ₃ bonding mode. The triply bridging anions lie in general positions, while the doubly bridging anions lie on twofold rotation axes.

Compound (I) is, in fact, isostructural not only with yttrium(III) sulfate octahydrate (Held & Wickleder, 2003 ) but also with the analogous lanthanide sulfates Ln₂(SO₄)₃·8H₂O, where Ln is Ce (Junk et al., 1999 ), Pr (Ahmed Farag et al., 1981 ), Nd (Bartl & Rodek, 1983 ), Sm (Podberezskaya & Borisov, 1976 ), Dy (Junk et al., 1999), Er (Wickleder, 1999 ), Yb (Hiltunen & Niinistö, 1976 ) or Lu (Junk et al., 1999). The coordination polymer in this structure is most readily envisaged as inversion-related pairs of chains comprising alternating cations and triply bridging anions, themselves generated by translation along the [010] direction, which are then linked into sheets by the doubly bridging anions. The coordination-polymer sheets are linked by hydrogen bonds (Table 2) into a continuous three-dimensional framework structure. As noted for the yttrium analogue (Held & Wickleder, 2003), one of the S—O bonds in the triply bridging anion is significantly longer than the others (Table 1).

Some of the lanthanides, such as europium, can also exhibit lower oxidation states in sulfate salts. Thus, for example, europium(II) sulfate has been shown to be anhydrous and to crystallize in space group Pnma (Mayer et al., 1964 ). Accordingly, the oxidation state of europium in (I) was further confirmed by bond valence sum calculations (Brown, 1992 , 2002 ). A total valence of 3.016 for europium was obtained using the observed Eu—O bond lengths (Table 1) and a bond valence parameter of 2.036 Å for europium (Trzesowska et al., 2004 ).

Figure 1
ORTEP diagram of (I

), showing the coordination geometry around europium, with 50% probability ellipsoids. [Symmetry codes: (a) −x, y, ½ − z; (b) ½ − x, ½ − y, 1 − z; (c) ½ − x, $[3 \over 2]$ − y, 1 − z.]

Figure 2
Crystal structure of (I

), showing the sulfate coordination.

Figure 3
Packing diagram of (I

), viewed along the c axis.

Experimental

The title compound was obtained during the attempted preparation of a complex between 2,5-diketopiperazine and europium sulfate, in which 2,5-diketopiperazine (0.228 g, 2 mmol) was heated with europium sulfate (0.736 g, 1 mmol) in water (30 ml). The latter was obtained by the action of sulfuric acid on europium oxide. The crystallization of europium sulfate from solution is facilitated in the presence of other ligands (Held & Wickleder, 2003; Wei & Zheng, 2003).

Crystal data

Eu₂(SO₄)₃·8H₂O
M_r = 736.26
Monoclinic, C2/c
a = 13.5029 (3) Å
b = 6.7601 (1) Å
c = 18.2628 (3) Å
β = 102.2610 (13)°
V = 1629.02 (5) Å³
Z = 4
D_x = 3.002 Mg m⁻³
Mo Kα radiation
Cell parameters from 1869 reflections
θ = 3.1–27.5°
μ = 8.12 mm⁻¹
T = 120 (2) K
Block, colourless
0.10 × 0.08 × 0.06 mm

Data collection

Bruker–Nonius KappaCCD diffractometer with FR591 rotating anode
φ and ω scans
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ) T_min = 0.477, T_max = 0.616
11 784 measured reflections
1869 independent reflections
1805 reflections with I > 2σ(I)
R_int = 0.037
θ_max = 27.5°
h = −17 → 17
k = −8 → 8
l = −22 → 23

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.019
wR(F²) = 0.054
S = 1.26
1869 reflections
114 parameters
H-atom parameters constrained
w = 1/[σ²(F_o²) + (0.0218P)² + 6.1179P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max = 0.002
Δρ_max = 0.71 e Å⁻³
Δρ_min = −1.32 e Å⁻³

Table 1
Selected interatomic distances(Å)

Eu1—O1	2.450 (3)
Eu1—O2	2.390 (2)
Eu1—O3	2.505 (2)
Eu1—O4	2.350 (3)
Eu1—O11	2.384 (2)
Eu1—O13	2.461 (2)
Eu1—O14	2.336 (2)
Eu1—O21	2.339 (2)
S1—O11ⁱ	1.473 (2)
S1—O12	1.459 (3)
S1—O13	1.499 (2)
S1—O14ⁱⁱ	1.463 (2)
S2—O21	1.470 (2)
S2—O22	1.478 (2)
Symmetry codes: (i) $[{\script{1\over 2}}-x,{\script{3\over 2}}-y,1-z]$ ; (ii) $[{\script{1\over 2}}-x,{\script{1\over 2}}-y,1-z]$ .

Table 2
Hydrogen-bonding geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H11⋯O3ⁱ	0.84	2.08	2.910 (3)	170
O1—H12⋯O13ⁱⁱ	0.84	2.06	2.771 (3)	143
O2—H21⋯O12ⁱⁱⁱ	0.84	1.87	2.704 (4)	171
O2—H22⋯O22^iv	0.84	1.99	2.814 (3)	169
O3—H31⋯O22	0.84	1.96	2.759 (3)	159
O3—H32⋯O13ⁱⁱⁱ	0.84	2.16	2.994 (3)	170
O4—H41⋯O12^v	0.84	1.93	2.748 (4)	163
O4—H42⋯O22^vi	0.84	1.97	2.788 (4)	165
Symmetry codes: (i) $[{\script{1\over 2}}-x,{\script{1\over 2}}-y,1-z]$ ; (ii) $[{\script{1\over 2}}-x,{\script{3\over 2}}-y,1-z]$ ; (iii) -x,1-y,1-z; (iv) x,1+y,z; (v) $[x,1-y,z-{\script{1\over 2}}]$ ; (vi) $[{\script{1\over 2}}+x,{\script{1\over 2}}+y,z]$ .

All H atoms were located in difference maps and then allowed to ride on their parent atoms, with O—H distances of 0.84 Å and with U_iso(H) = 1.2U_eq(O).

Data collection: COLLECT (Hooft, 1999 ); cell refinement: DENZO (Otwinowski & Minor, 1997 ) and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: OSCAIL (McArdle, 2003 ) and SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: OSCAIL and SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003 ); software used to prepare material for publication: SHELXL97 and PRPKAPPA (Ferguson, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S160053680402608X/lh6289sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S160053680402608X/lh6289Isup2.hkl

Computing details top

Data collection: COLLECT (Hooft, 1999); cell refinement: DENZO (Otwinowski & Minor, 1997) and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: OSCAIL and SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97 and PRPKAPPA (Ferguson, 1999).

Dieuropium trisulfate octahydrate top

Crystal data top

[Eu₂(SO₄)₃(H₂O)₈]	F(000) = 1400
M_r = 736.26	D_x = 3.002 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1869 reflections
a = 13.5029 (3) Å	θ = 3.1–27.5°
b = 6.7601 (1) Å	µ = 8.12 mm⁻¹
c = 18.2628 (3) Å	T = 120 K
β = 102.2610 (13)°	Plate, colourless
V = 1629.02 (5) Å³	0.10 × 0.08 × 0.06 mm
Z = 4

Data collection top

Bruker-Nonius 95mm CCD camera on κ-goniostat diffractometer	1869 independent reflections
Radiation source: Bruker–Nonius FR591 rotating anode	1805 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
Detector resolution: 9.091 pixels mm^-1	θ_max = 27.5°, θ_min = 3.1°
φ & ω scans	h = −17→17
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	k = −8→8
T_min = 0.477, T_max = 0.616	l = −22→23
11784 measured reflections

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)] = 0.019	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.054	H-atom parameters constrained
S = 1.26	w = 1/[σ²(F_o²) + (0.0218P)² + 6.1179P] where P = (F_o² + 2F_c²)/3
1869 reflections	(Δ/σ)_max = 0.002
114 parameters	Δρ_max = 0.71 e Å⁻³
0 restraints	Δρ_min = −1.32 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Eu1	0.167587 (11)	0.47732 (2)	0.392539 (9)	0.00436 (8)
O1	0.34495 (19)	0.5163 (3)	0.45743 (14)	0.0075 (5)
O2	0.01431 (17)	0.6639 (4)	0.35904 (14)	0.0140 (5)
O3	0.04016 (16)	0.2634 (3)	0.43634 (13)	0.0083 (5)
O4	0.2592 (2)	0.5073 (4)	0.29716 (15)	0.0123 (5)
S1	0.21644 (6)	0.52970 (11)	0.58924 (5)	0.00457 (17)
O11	0.20077 (17)	0.8241 (3)	0.39758 (12)	0.0077 (5)
O12	0.16150 (18)	0.5354 (4)	0.64991 (14)	0.0097 (5)
O13	0.14441 (17)	0.5794 (3)	0.51715 (12)	0.0076 (4)
O14	0.24242 (17)	0.1670 (3)	0.41959 (13)	0.0103 (5)
S2	0.0000	0.17534 (16)	0.2500	0.0053 (2)
O21	0.08491 (17)	0.3008 (4)	0.28701 (13)	0.0106 (5)
O22	−0.03310 (19)	0.0515 (3)	0.30707 (14)	0.0089 (5)
H11	0.3814	0.4312	0.4838	0.009*
H12	0.3610	0.6166	0.4845	0.009*
H21	−0.0434	0.6132	0.3549	0.017*
H22	0.0076	0.7843	0.3477	0.017*
H31	0.0064	0.1908	0.4028	0.010*
H32	−0.0066	0.3184	0.4527	0.010*
H41	0.2369	0.4741	0.2524	0.015*
H42	0.3197	0.5429	0.3007	0.015*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Eu1	0.00432 (12)	0.00358 (11)	0.00492 (12)	−0.00052 (5)	0.00041 (8)	−0.00030 (5)
O1	0.0081 (12)	0.0060 (11)	0.0069 (12)	0.0006 (8)	−0.0017 (10)	−0.0003 (8)
O2	0.0059 (11)	0.0084 (12)	0.0258 (14)	−0.0008 (9)	−0.0012 (10)	0.0046 (10)
O3	0.0067 (11)	0.0085 (11)	0.0095 (11)	−0.0019 (9)	0.0008 (9)	−0.0017 (9)
O4	0.0083 (13)	0.0217 (13)	0.0073 (13)	−0.0068 (9)	0.0029 (11)	−0.0032 (9)
S1	0.0046 (4)	0.0032 (4)	0.0057 (4)	−0.0001 (3)	0.0007 (3)	0.0002 (3)
O11	0.0066 (11)	0.0053 (11)	0.0107 (12)	−0.0019 (9)	0.0008 (9)	−0.0003 (9)
O12	0.0072 (13)	0.0157 (12)	0.0066 (13)	−0.0018 (9)	0.0021 (10)	−0.0016 (9)
O13	0.0076 (11)	0.0081 (11)	0.0059 (11)	0.0001 (9)	−0.0010 (9)	0.0001 (9)
O14	0.0115 (12)	0.0029 (11)	0.0158 (12)	0.0019 (9)	0.0012 (9)	−0.0003 (9)
S2	0.0052 (5)	0.0049 (5)	0.0053 (5)	0.000	−0.0004 (4)	0.000
O21	0.0094 (11)	0.0139 (12)	0.0078 (11)	−0.0078 (9)	0.0006 (9)	−0.0041 (9)
O22	0.0104 (12)	0.0071 (11)	0.0091 (12)	−0.0008 (9)	0.0022 (10)	0.0023 (9)

Geometric parameters (Å, º) top

Eu1—O1	2.450 (3)	O3—H31	0.84
Eu1—O2	2.390 (2)	O3—H32	0.84
Eu1—O3	2.505 (2)	O4—H41	0.84
Eu1—O4	2.350 (3)	O4—H42	0.84
Eu1—O11	2.384 (2)	S1—O11ⁱ	1.473 (2)
Eu1—O13	2.461 (2)	S1—O12	1.459 (3)
Eu1—O14	2.336 (2)	S1—O13	1.499 (2)
Eu1—O21	2.339 (2)	S1—O14ⁱⁱ	1.463 (2)
O1—H11	0.84	S2—O21	1.470 (2)
O1—H12	0.84	S2—O21ⁱⁱⁱ	1.470 (2)
O2—H21	0.84	S2—O22	1.478 (2)
O2—H22	0.84	S2—O22ⁱⁱⁱ	1.478 (2)

O14—Eu1—O21	79.93 (8)	O1—Eu1—S1	62.92 (6)
O14—Eu1—O4	87.81 (8)	O13—Eu1—S1	20.55 (5)
O21—Eu1—O4	70.58 (8)	O3—Eu1—S1	74.07 (5)
O14—Eu1—O11	143.67 (8)	Eu1—O1—H11	126.7
O21—Eu1—O11	125.90 (8)	Eu1—O1—H12	118.4
O4—Eu1—O11	79.62 (8)	H11—O1—H12	99.7
O14—Eu1—O2	147.20 (8)	Eu1—O2—H21	122.9
O21—Eu1—O2	79.78 (8)	Eu1—O2—H22	128.1
O4—Eu1—O2	109.18 (9)	H21—O2—H22	108.9
O11—Eu1—O2	68.68 (8)	Eu1—O3—H31	114.0
O14—Eu1—O1	70.11 (8)	Eu1—O3—H32	118.4
O21—Eu1—O1	134.41 (8)	H31—O3—H32	100.7
O4—Eu1—O1	74.62 (9)	Eu1—O4—H41	124.2
O11—Eu1—O1	73.70 (7)	Eu1—O4—H42	128.6
O2—Eu1—O1	140.48 (8)	H41—O4—H42	107.1
O14—Eu1—O13	100.98 (8)	O12—S1—O14ⁱⁱ	111.97 (14)
O21—Eu1—O13	140.61 (8)	O12—S1—O11ⁱ	110.40 (14)
O4—Eu1—O13	148.41 (8)	O14ⁱⁱ—S1—O11ⁱ	109.58 (13)
O11—Eu1—O13	75.44 (8)	O12—S1—O13	108.74 (14)
O2—Eu1—O13	79.37 (8)	O14ⁱⁱ—S1—O13	107.30 (14)
O1—Eu1—O13	79.97 (8)	O11ⁱ—S1—O13	108.75 (13)
O14—Eu1—O3	73.11 (8)	O12—S1—Eu1	139.49 (10)
O21—Eu1—O3	74.25 (8)	O14ⁱⁱ—S1—Eu1	77.87 (10)
O4—Eu1—O3	142.36 (8)	O11ⁱ—S1—Eu1	101.82 (9)
O11—Eu1—O3	133.73 (7)	S1ⁱ—O11—Eu1	142.72 (14)
O2—Eu1—O3	76.72 (8)	S1—O13—Eu1	124.27 (13)
O1—Eu1—O3	125.08 (8)	S1ⁱⁱ—O14—Eu1	161.88 (15)
O13—Eu1—O3	68.63 (8)	O21—S2—O21ⁱⁱⁱ	109.6 (2)
O14—Eu1—S1	84.02 (6)	O21—S2—O22	108.99 (13)
O21—Eu1—S1	147.46 (6)	O21—S2—O22ⁱⁱⁱ	109.13 (13)
O4—Eu1—S1	137.03 (7)	O22—S2—O22ⁱⁱⁱ	111.0 (2)
O11—Eu1—S1	82.48 (5)	S2—O21—Eu1	149.58 (14)
O2—Eu1—S1	99.91 (6)

O14—Eu1—S1—O12	−108.91 (17)	O2—Eu1—O11—S1ⁱ	−175.9 (2)
O21—Eu1—S1—O12	−48.3 (2)	O1—Eu1—O11—S1ⁱ	16.4 (2)
O4—Eu1—S1—O12	170.80 (18)	O13—Eu1—O11—S1ⁱ	100.0 (2)
O11—Eu1—S1—O12	104.91 (17)	O3—Eu1—O11—S1ⁱ	139.71 (19)
O2—Eu1—S1—O12	38.20 (17)	S1—Eu1—O11—S1ⁱ	80.3 (2)
O1—Eu1—S1—O12	−179.60 (17)	O12—S1—O13—Eu1	−155.83 (14)
O13—Eu1—S1—O12	36.7 (2)	O14ⁱⁱ—S1—O13—Eu1	−34.53 (19)
O3—Eu1—S1—O12	−34.81 (17)	O11ⁱ—S1—O13—Eu1	83.92 (17)
O14—Eu1—S1—O14ⁱⁱ	0.82 (15)	O14—Eu1—O13—S1	34.95 (17)
O21—Eu1—S1—O14ⁱⁱ	61.43 (15)	O21—Eu1—O13—S1	122.42 (16)
O4—Eu1—S1—O14ⁱⁱ	−79.46 (13)	O4—Eu1—O13—S1	−69.0 (2)
O11—Eu1—S1—O14ⁱⁱ	−145.36 (11)	O11—Eu1—O13—S1	−107.93 (16)
O2—Eu1—S1—O14ⁱⁱ	147.93 (11)	O2—Eu1—O13—S1	−178.45 (17)
O1—Eu1—S1—O14ⁱⁱ	−69.87 (11)	O1—Eu1—O13—S1	−32.33 (15)
O13—Eu1—S1—O14ⁱⁱ	146.39 (19)	O3—Eu1—O13—S1	101.77 (16)
O3—Eu1—S1—O14ⁱⁱ	74.93 (11)	O21—Eu1—O14—S1ⁱⁱ	31.0 (5)
O14—Eu1—S1—O11ⁱ	108.59 (11)	O4—Eu1—O14—S1ⁱⁱ	−39.7 (5)
O21—Eu1—S1—O11ⁱ	169.20 (14)	O11—Eu1—O14—S1ⁱⁱ	−108.8 (5)
O4—Eu1—S1—O11ⁱ	28.30 (14)	O2—Eu1—O14—S1ⁱⁱ	83.6 (5)
O11—Eu1—S1—O11ⁱ	−37.59 (14)	O1—Eu1—O14—S1ⁱⁱ	−114.1 (5)
O2—Eu1—S1—O11ⁱ	−104.30 (11)	O13—Eu1—O14—S1ⁱⁱ	170.9 (5)
O1—Eu1—S1—O11ⁱ	37.90 (11)	O3—Eu1—O14—S1ⁱⁱ	107.5 (5)
O13—Eu1—S1—O11ⁱ	−105.84 (19)	S1—Eu1—O14—S1ⁱⁱ	−177.4 (5)
O3—Eu1—S1—O11ⁱ	−177.30 (11)	O21ⁱⁱⁱ—S2—O21—Eu1	88.2 (3)
O14—Eu1—S1—O13	−145.56 (17)	O22—S2—O21—Eu1	−31.1 (3)
O21—Eu1—S1—O13	−84.96 (19)	O22ⁱⁱⁱ—S2—O21—Eu1	−152.5 (3)
O4—Eu1—S1—O13	134.15 (18)	O14—Eu1—O21—S2	88.9 (3)
O11—Eu1—S1—O13	68.25 (17)	O4—Eu1—O21—S2	−179.9 (3)
O2—Eu1—S1—O13	1.54 (17)	O11—Eu1—O21—S2	−119.3 (3)
O1—Eu1—S1—O13	143.74 (17)	O2—Eu1—O21—S2	−65.2 (3)
O3—Eu1—S1—O13	−71.46 (17)	O1—Eu1—O21—S2	137.7 (3)
O14—Eu1—O11—S1ⁱ	11.2 (3)	O13—Eu1—O21—S2	−6.2 (4)
O21—Eu1—O11—S1ⁱ	−117.1 (2)	O3—Eu1—O21—S2	13.7 (3)
O4—Eu1—O11—S1ⁱ	−60.4 (2)	S1—Eu1—O21—S2	27.2 (4)

Symmetry codes: (i) −x+1/2, −y+3/2, −z+1; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···O3ⁱⁱ	0.84	2.08	2.910 (3)	170
O1—H12···O13ⁱ	0.84	2.06	2.771 (3)	143
O2—H21···O12^iv	0.84	1.87	2.704 (4)	171
O2—H22···O22^v	0.84	1.99	2.814 (3)	169
O3—H31···O22	0.84	1.96	2.759 (3)	159
O3—H32···O13^iv	0.84	2.16	2.994 (3)	170
O4—H41···O12^vi	0.84	1.93	2.748 (4)	163
O4—H42···O22^vii	0.84	1.97	2.788 (4)	165

Symmetry codes: (i) −x+1/2, −y+3/2, −z+1; (ii) −x+1/2, −y+1/2, −z+1; (iv) −x, −y+1, −z+1; (v) x, y+1, z; (vi) x, −y+1, z−1/2; (vii) x+1/2, y+1/2, z.

Footnotes

‡Postal address: Department of Electrical Engineering and Physics, University of Dundee, Dundee DD1 4HN, Scotland.

Acknowledgements

X-ray data were collected at the EPSRC X-ray Crystallographic Service, University of Southampton, England; the authors thank the staff for all their help and advice. JNL thanks NCR Self-Service, Dundee, for grants which have provided computing facilities for this work.

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