1,4-Diazo­niabi­cyclo­[2.2.2]­octane aqua­bis­(oxalato-κ2O,O′)copper(II) dihydrate

Keene, T.D.; Hursthouse, M.B.; Price, D.J.

doi:10.1107/S1600536804005033

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 60| Part 4| April 2004| Pages m378-m380

https://doi.org/10.1107/S1600536804005033

1,4-Diazoniabicyclo[2.2.2]octane aquabis(oxalato-κ²O,O′)copper(II) dihydrate

Tony D. Keene,^a Michael B. Hursthouse ^a and Daniel J. Price ^a ^*

^aSchool of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, England
^*Correspondence e-mail: daniel.price@soton.ac.uk

(Received 1 March 2004; accepted 4 March 2004; online 20 March 2004)

The title compound, (C₆H₁₄N₂)[Cu(C₂O₄)₂(H₂O)]·2H₂O, crystallizes in the space group P $[\overline 1]$ . In the solid state, the [Cu(ox)₂(H₂O)]²⁻ units (ox is oxalate, C₂O₄) dimerize to give a tetragonally distorted CuO₆ coordination environment. Extensive hydrogen bonding between the oxalate, the coordinated water, the 1,4-diazoniabicyclo[2.2.2]octane dications ([dabcoH₂]²⁺) and the water of crystallization determines the crystal packing.

Comment

Blue crystals of the title compound, (I), were obtained by a slow diffusion technique in an aqueous gel. This ionic compound crystallizes in the triclinic space group P $[\overline 1]$ , with two formula units per unit cell. The structure of (I) contains [Cu(ox)₂(H₂O)]²⁻ (ox is oxalate, C₂O₄) units, in which the Cu^II ion is coordinated by two chelating oxalate ions in a planar geometry, and the coordinated water molecule forms a long axial contact [Cu1—O1W 2.344 (7) Å]. These units dimerize through one of the coordinating O atoms of the oxalate (Fig. 1 and Table 1), resulting in a Cu1⋯Cu1ⁱ separation of 3.818 (8) Å [symmetry code: (i) −x, 1 − y, 1 − z]. The long Cu1—O3ⁱ contact of 2.906 (10) Å gives an idea of the weakness of the dimerization interaction.

The number of hydrogen-bond acceptor sites in (I) is greater than the number of potential hydrogen-bond donating groups. We note that all D—H groups are involved in hydrogen bonding, and that there are seven different (near) linear and one bifurcated hydrogen-bond interactions (Table 2). Neighbouring [Cu(ox)₂(H₂O)]₂⁴⁻ units are directly hydrogen-bonded into chains. These chains are hydrogen-bonded through the water of crystallization, resulting in an extensive three-dimensional network (Fig. 2). The unsymmetric bifurcated hydrogen bond between the oxalate and 1,4-diazoniabicyclo[2.2.2]octane ([dabcoH₂]²⁺) is a motif seen in almost all other compounds containing [dabcoH₂]²⁺ and ox²⁻ (Vaidhyanathan et al., 2001 ; Lee & Wang, 1999 ; Malfant et al., 1990 ), although we note that this hydrogen-bonding pattern is not uncommon in oxalate compounds.

As described previously (Keene et al., 2003 , 2004 ), discrete mono- and dinuclear metal oxalate species may be formed when the bridging potential of the oxalate is reduced. This can be achieved either through the use of capping ligands or by a high concentration of the oxalate dianion, in both cases resulting in coordinatively saturated complexes. The large Jahn–Teller effect in Cu^II makes the structural chemistry of copper oxalate compounds different from that of other 3d transition metals. In particular, a displacement of the labile axial water molecules during crystallization is commonly observed, and a polycatenation process results in chains of [Cu(ox)₂]₂²ⁿ⁻ in the solid state. Very few examples of isolated [Cu(ox)₂(H₂O)₂]²⁻ (Insausti et al., 1994 ; Keene et al., 2004) or dimerized species (Savel'eva et al., 1992 ) have been observed in the solid state. In the case of (I), the extensive hydrogen-bonded network stabilizes the discrete dimerization of the copper bisoxalate dianions, to give isolated [Cu(ox)₂(H₂O)]₂⁴⁻ units.

Figure 1
The asymmetric unit and selected symmetry equivalents of (I

), showing the dimerization of the [Cu(ox)₂(H₂O)]²⁻ unit. Displacement ellipsoids are drawn at the 50% probability level. Some H atoms have been omitted for clarity. Primed atoms are generated by the symmetry operation (−x, 1 − y, 1 − z).

Figure 2
Hydrogen-bonding interactions (dashed lines) between [Cu(ox)₂(H₂O)]₂⁴⁻ clusters and the water of crystallization, viewed along the b axis.

Experimental

Single crystals of (I) were synthesized by a gel-crystallization technique. CuSO₄·5H₂O (100 mg, 0.40 mmol) was dissolved in distilled water (18 ml). Tetramethoxysilane (2 ml) was added and the mixture stirred until monophasic, then allowed to set in a test tube. A solution of 1,4-diazoniabicyclo[2.2.2]octane bis(hydrogenoxalate) (200 mg, 0.68 mmol) was added to the top of the gel. After two weeks, light-blue crystals of (I) had formed in the gel. IR (KBr, diffuse reflectance, cm⁻¹): 3450 s (O—H stretch), 2823 s (C—H stretch), 2650 s (N—H stretch), 1681 s and 1658 s (oxalate), 1412 s (oxalate), 1291 s, 1059 s, 850 s, 801 s, 607 m, 540 m, 495 m; UV/VIS/NIR (diffuse reflectance, cm⁻¹): 14 400 (d-d), 35 700 (oxalate).

Crystal data

(C₆H₁₄N₂)[Cu(C₂O₄)₂(H₂O)]·2H₂O
M_r = 407.82
Triclinic, $[P\overline 1]$
a = 9.3847 (7) Å
b = 9.4884 (6) Å
c = 9.6936 (5) Å
α = 62.150 (4)°
β = 81.987 (4)°
γ = 87.868 (3)°
V = 755.36 (9) Å³
Z = 2
D_x = 1.793 Mg m⁻³
Mo Kα radiation
Cell parameters from 9717 reflections
θ = 2.9–27.5°
μ = 1.51 mm⁻¹
T = 167 (2) K
Block, blue
0.42 × 0.12 × 0.08 mm

Data collection

Nonius KappaCCD area-detector diffractometer
φ and ω scans
Absorption correction: multi-scan (SORTAV; Blessing, 1997 ) T_min = 0.696, T_max = 0.886
7866 measured reflections
3465 independent reflections
3018 reflections with I > 2σ(I)
R_int = 0.060
θ_max = 27.6°
h = −10 → 12
k = −12 → 12
l = −11 → 12

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.040
wR(F²) = 0.103
S = 1.05
3465 reflections
241 parameters
H atoms treated by a mixture of independent and constrained refinement
w = 1/[σ²(F_o²) + (0.0396P)² + 0.8532P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max < 0.001
Δρ_max = 0.53 e Å⁻³
Δρ_min = −0.71 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Cu1—O6	1.9366 (18)
Cu1—O3	1.9458 (19)
Cu1—O3ⁱ	2.9058 (18)
Cu1—O1	1.9584 (18)
Cu1—O8	1.9617 (17)
Cu1—O1W	2.343 (2)
Symmetry code: (i) -x,1-y,1-z.

Table 2
Hydrogen-bonding geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯O2W	0.91	1.84	2.698 (4)	157
N2—H2⋯O4ⁱⁱ	0.91	1.90	2.690 (3)	144
N2—H2⋯O2ⁱⁱ	0.91	2.28	2.978 (5)	133
O2W—H21⋯O8ⁱⁱⁱ	0.87 (2)	1.95 (2)	2.819 (5)	178 (2)
O2W—H22⋯O3W^iv	0.87 (2)	2.36 (2)	3.201 (4)	163 (2)
O3W—H31⋯O5	0.88 (4)	1.95 (4)	2.770 (6)	155 (4)
O1W—H11⋯O7ⁱⁱⁱ	0.87 (3)	1.98 (3)	2.837 (5)	169 (3)
O1W—H12⋯O3W^v	0.875 (18)	1.942 (19)	2.800 (6)	166.1 (16)
O3W—H32⋯O2^vi	0.87 (3)	1.88 (3)	2.703 (6)	157 (3)
Symmetry codes: (ii) 1+x,y,1+z; (iii) 1-x,1-y,1-z; (iv) 1-x,2-y,1-z; (v) x,y,z-1; (vi) -x,2-y,1-z.

H atoms bound to C and N atoms were positioned geometrically and refined as riding, with C—H = 0.97 and N—H = 0.91 Å, and with U_iso(H) = 1.2U_eq(parent atom). H atoms bound to O atoms were located in difference maps, but their distances and angles were restrained to literature values.

Data collection: DENZO (Otwinowski & Minor, 1997 ); cell refinement: DENZO and COLLECT (Nonius, 1998 ); data reduction: DENZO and COLLECT; program(s) used to solve structure: SIR92 (Altomare et al., 1993 ) in WinGX (Farrugia, 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ) in WinGX; molecular graphics: DIAMOND (Brandenburg, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536804005033/hb6023sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536804005033/hb6023Isup2.hkl

Computing details top

Data collection: DENZO (Otwinowski & Minor, 1997); cell refinement: DENZO and COLLECT (Nonius, 1998); data reduction: DENZO and COLLECT; program(s) used to solve structure: SIR92 (Altomare et al., 1993) in WinGX (Farrugia, 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) in WinGX; molecular graphics: DIAMOND (Brandenburg, 1999).

(I) top

Crystal data top

(C₆H₁₄N₂)[Cu(C₂O₄)₂(H₂O)]·2H₂O	Z = 2
M_r = 407.82	F(000) = 422
Triclinic, P1	D_x = 1.793 Mg m⁻³
Hall symbol: -P 1	Melting point: N/A K
a = 9.3847 (7) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.4884 (6) Å	Cell parameters from 9717 reflections
c = 9.6936 (5) Å	θ = 2.9–27.5°
α = 62.150 (4)°	µ = 1.51 mm⁻¹
β = 81.987 (4)°	T = 167 K
γ = 87.868 (3)°	Block, blue
V = 755.36 (9) Å³	0.42 × 0.12 × 0.08 mm

Data collection top

Nonius KappaCCD areadetector diffractometer	3018 reflections with I > 2σ(I)
φ and ω scans to fill Ewald sphere	R_int = 0.060
Absorption correction: multi-scan (SORTAV; Blessing, 1997)	θ_max = 27.6°, θ_min = 3.0°
T_min = 0.696, T_max = 0.886	h = −10→12
7866 measured reflections	k = −12→12
3465 independent reflections	l = −11→12

Refinement top

Refinement on F²	9 restraints
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.04	w = 1/[σ²(F_o²) + (0.0396P)² + 0.8532P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.103	(Δ/σ)_max < 0.001
S = 1.05	Δρ_max = 0.53 e Å⁻³
3465 reflections	Δρ_min = −0.71 e Å⁻³
241 parameters

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.

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

	x	y	z	U_iso*/U_eq
Cu1	0.15412 (3)	0.65517 (4)	0.42178 (3)	0.01844 (11)
O1W	0.3493 (2)	0.7610 (2)	0.2200 (2)	0.0272 (4)
O8	0.2783 (2)	0.4889 (2)	0.5517 (2)	0.0194 (4)
O2W	0.6147 (2)	0.8080 (3)	0.4064 (2)	0.0287 (5)
O5	0.3221 (2)	0.7258 (2)	0.7332 (2)	0.0255 (4)
O3	0.0787 (2)	0.5310 (2)	0.3337 (2)	0.0214 (4)
O6	0.1949 (2)	0.7605 (2)	0.5422 (2)	0.0200 (4)
O7	0.4125 (2)	0.4410 (2)	0.7398 (2)	0.0229 (4)
O4	−0.0491 (2)	0.5699 (2)	0.1426 (2)	0.0228 (4)
O1	0.0246 (2)	0.8192 (2)	0.3001 (2)	0.0218 (4)
O3W	0.2755 (3)	0.8810 (4)	0.9159 (3)	0.0501 (7)
N1	0.6965 (2)	0.8110 (3)	0.6610 (2)	0.0200 (5)
H1	0.66	0.8363	0.5704	0.024*
O2	−0.1199 (2)	0.8612 (2)	0.1207 (2)	0.0282 (4)
N2	0.7966 (2)	0.7424 (3)	0.9072 (3)	0.0211 (5)
H2	0.8332	0.7169	0.9979	0.025*
C4	0.9168 (3)	0.8005 (4)	0.7740 (3)	0.0284 (6)
H4A	0.986	0.7174	0.7911	0.034*
H4B	0.9656	0.8923	0.7672	0.034*
C2	0.6907 (4)	0.8692 (4)	0.8822 (3)	0.0331 (7)
H2A	0.7377	0.9635	0.8722	0.04*
H2B	0.6151	0.8328	0.9717	0.04*
C5	0.6648 (3)	0.6382 (3)	0.7716 (3)	0.0232 (6)
H5A	0.7069	0.574	0.7235	0.028*
H5B	0.5616	0.617	0.7957	0.028*
C1	0.6263 (3)	0.9093 (3)	0.7327 (3)	0.0221 (5)
H1A	0.5233	0.8865	0.7577	0.027*
H1B	0.6425	1.0218	0.6591	0.027*
C6	0.7282 (3)	0.5964 (3)	0.9210 (3)	0.0258 (6)
H6A	0.653	0.5542	1.0108	0.031*
H6B	0.7995	0.5154	0.9369	0.031*
C3	0.8556 (3)	0.8458 (3)	0.6226 (3)	0.0258 (6)
H3A	0.8749	0.9583	0.551	0.031*
H3B	0.9005	0.7851	0.5718	0.031*
C8	−0.0006 (3)	0.6126 (3)	0.2280 (3)	0.0185 (5)
C9	0.2796 (3)	0.6833 (3)	0.6437 (3)	0.0182 (5)
C10	0.3301 (3)	0.5234 (3)	0.6479 (3)	0.0166 (5)
C7	−0.0364 (3)	0.7803 (3)	0.2126 (3)	0.0194 (5)
H21	0.646 (3)	0.7160 (17)	0.419 (3)	0.028 (9)*
H22	0.646 (4)	0.878 (3)	0.310 (2)	0.046 (11)*
H31	0.262 (4)	0.826 (4)	0.867 (4)	0.047 (11)*
H11	0.427 (2)	0.706 (4)	0.238 (3)	0.032 (9)*
H12	0.337 (3)	0.788 (4)	0.1230 (19)	0.045 (11)*
H32	0.210 (3)	0.953 (3)	0.893 (4)	0.053 (12)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.02148 (18)	0.01728 (18)	0.02011 (18)	0.00559 (12)	−0.00930 (12)	−0.01031 (13)
O1W	0.0246 (10)	0.0295 (11)	0.0250 (10)	0.0103 (8)	−0.0053 (8)	−0.0109 (9)
O8	0.0223 (9)	0.0186 (9)	0.0208 (9)	0.0055 (7)	−0.0095 (7)	−0.0107 (7)
O2W	0.0382 (12)	0.0284 (11)	0.0253 (11)	0.0103 (9)	−0.0119 (9)	−0.0160 (9)
O5	0.0277 (10)	0.0270 (10)	0.0310 (10)	0.0070 (8)	−0.0129 (8)	−0.0194 (9)
O3	0.0256 (10)	0.0193 (9)	0.0239 (9)	0.0066 (7)	−0.0123 (8)	−0.0120 (8)
O6	0.0226 (9)	0.0177 (9)	0.0226 (9)	0.0053 (7)	−0.0109 (7)	−0.0100 (7)
O7	0.0224 (9)	0.0251 (10)	0.0241 (9)	0.0087 (8)	−0.0112 (7)	−0.0123 (8)
O4	0.0267 (10)	0.0228 (10)	0.0246 (10)	0.0050 (8)	−0.0125 (8)	−0.0139 (8)
O1	0.0265 (10)	0.0185 (9)	0.0230 (9)	0.0054 (7)	−0.0099 (8)	−0.0104 (8)
O3W	0.0565 (16)	0.0730 (19)	0.0554 (15)	0.0433 (14)	−0.0380 (13)	−0.0535 (15)
N1	0.0218 (11)	0.0226 (11)	0.0178 (10)	0.0046 (9)	−0.0082 (8)	−0.0101 (9)
O2	0.0349 (11)	0.0229 (10)	0.0307 (10)	0.0104 (8)	−0.0189 (9)	−0.0125 (9)
N2	0.0238 (11)	0.0230 (12)	0.0185 (10)	0.0026 (9)	−0.0079 (9)	−0.0102 (9)
C4	0.0186 (13)	0.0318 (16)	0.0323 (15)	−0.0037 (11)	−0.0058 (11)	−0.0120 (13)
C2	0.0452 (18)	0.0332 (16)	0.0283 (15)	0.0185 (14)	−0.0124 (13)	−0.0198 (13)
C5	0.0223 (13)	0.0196 (13)	0.0314 (14)	0.0029 (10)	−0.0088 (11)	−0.0138 (11)
C1	0.0209 (13)	0.0211 (13)	0.0255 (13)	0.0040 (10)	−0.0066 (10)	−0.0112 (11)
C6	0.0308 (15)	0.0192 (13)	0.0239 (13)	−0.0034 (11)	−0.0055 (11)	−0.0064 (11)
C3	0.0214 (13)	0.0281 (15)	0.0239 (13)	0.0010 (11)	0.0011 (10)	−0.0099 (11)
C8	0.0173 (12)	0.0187 (12)	0.0188 (12)	0.0017 (9)	−0.0036 (9)	−0.0080 (10)
C9	0.0199 (12)	0.0172 (12)	0.0199 (12)	0.0013 (9)	−0.0036 (9)	−0.0103 (10)
C10	0.0152 (11)	0.0183 (12)	0.0164 (11)	0.0019 (9)	−0.0026 (9)	−0.0082 (10)
C7	0.0189 (12)	0.0188 (13)	0.0202 (12)	0.0026 (9)	−0.0037 (10)	−0.0088 (10)

Geometric parameters (Å, º) top

Cu1—O6	1.9366 (18)	O2—C7	1.228 (3)
Cu1—O3	1.9458 (19)	N2—C2	1.484 (4)
Cu1—O3ⁱ	2.9058 (18)	N2—C4	1.489 (4)
Cu1—O1	1.9584 (18)	N2—C6	1.490 (3)
Cu1—O8	1.9617 (17)	N2—H2	0.91
Cu1—O1W	2.343 (2)	C4—C3	1.515 (4)
O1W—H11	0.87 (3)	C4—H4A	0.97
O1W—H12	0.875 (10)	C4—H4B	0.97
O8—C10	1.278 (3)	C2—C1	1.524 (4)
O2W—H21	0.871 (10)	C2—H2A	0.97
O2W—H22	0.872 (10)	C2—H2B	0.97
O5—C9	1.228 (3)	C5—C6	1.515 (4)
O3—C8	1.278 (3)	C5—H5A	0.97
O6—C9	1.280 (3)	C5—H5B	0.97
O7—C10	1.225 (3)	C1—H1A	0.97
O4—C8	1.221 (3)	C1—H1B	0.97
O1—C7	1.275 (3)	C6—H6A	0.97
O3W—H31	0.88 (4)	C6—H6B	0.97
O3W—H32	0.87 (3)	C3—H3A	0.97
N1—C1	1.489 (3)	C3—H3B	0.97
N1—C5	1.493 (3)	C8—C7	1.555 (4)
N1—C3	1.498 (3)	C9—C10	1.557 (4)
N1—H1	0.91

O6—Cu1—O3	168.20 (8)	N2—C2—H2B	109.9
O6—Cu1—O1	94.13 (7)	C1—C2—H2B	109.9
O3—Cu1—O1	84.94 (8)	H2A—C2—H2B	108.3
O6—Cu1—O8	84.77 (7)	N1—C5—C6	108.4 (2)
O3—Cu1—O8	95.69 (7)	N1—C5—H5A	110
O1—Cu1—O8	177.59 (7)	C6—C5—H5A	110
O6—Cu1—O1W	98.46 (8)	N1—C5—H5B	110
O3—Cu1—O1W	93.33 (8)	C6—C5—H5B	110
O1—Cu1—O1W	93.02 (7)	H5A—C5—H5B	108.4
O8—Cu1—O1W	89.27 (7)	N1—C1—C2	108.4 (2)
Cu1—O1W—H11	115 (2)	N1—C1—H1A	110
Cu1—O1W—H12	120 (2)	C2—C1—H1A	110
H11—O1W—H12	106.5 (15)	N1—C1—H1B	110
C10—O8—Cu1	112.33 (16)	C2—C1—H1B	110
H21—O2W—H22	107.0 (15)	H1A—C1—H1B	108.4
C8—O3—Cu1	112.38 (16)	N2—C6—C5	109.2 (2)
C9—O6—Cu1	113.35 (16)	N2—C6—H6A	109.8
C7—O1—Cu1	111.87 (17)	C5—C6—H6A	109.8
H31—O3W—H32	106.9 (15)	N2—C6—H6B	109.8
C1—N1—C5	109.7 (2)	C5—C6—H6B	109.8
C1—N1—C3	110.1 (2)	H6A—C6—H6B	108.3
C5—N1—C3	110.7 (2)	N1—C3—C4	108.7 (2)
C1—N1—H1	108.7	N1—C3—H3A	110
C5—N1—H1	108.7	C4—C3—H3A	110
C3—N1—H1	108.7	N1—C3—H3B	110
C2—N2—C4	110.2 (2)	C4—C3—H3B	110
C2—N2—C6	111.3 (2)	H3A—C3—H3B	108.3
C4—N2—C6	109.0 (2)	O4—C8—O3	126.0 (2)
C2—N2—H2	108.7	O4—C8—C7	119.3 (2)
C4—N2—H2	108.7	O3—C8—C7	114.7 (2)
C6—N2—H2	108.7	O5—C9—O6	125.6 (2)
N2—C4—C3	108.8 (2)	O5—C9—C10	119.8 (2)
N2—C4—H4A	109.9	O6—C9—C10	114.5 (2)
C3—C4—H4A	109.9	O7—C10—O8	125.2 (2)
N2—C4—H4B	109.9	O7—C10—C9	119.8 (2)
C3—C4—H4B	109.9	O8—C10—C9	115.0 (2)
H4A—C4—H4B	108.3	O2—C7—O1	126.4 (3)
N2—C2—C1	108.9 (2)	O2—C7—C8	118.2 (2)
N2—C2—H2A	109.9	O1—C7—C8	115.4 (2)
C1—C2—H2A	109.9

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
N1—H1···O2W	0.91	1.84	2.698 (4)	157
N2—H2···O4ⁱⁱ	0.91	1.90	2.690 (3)	144
N2—H2···O2ⁱⁱ	0.91	2.28	2.978 (5)	133
O2W—H21···O8ⁱⁱⁱ	0.87 (2)	1.95 (2)	2.819 (5)	178 (2)
O2W—H22···O3W^iv	0.87 (2)	2.36 (2)	3.201 (4)	163 (2)
O3W—H31···O5	0.88 (4)	1.95 (4)	2.770 (6)	155 (4)
O1W—H11···O7ⁱⁱⁱ	0.87 (3)	1.98 (3)	2.837 (5)	169 (3)
O1W—H12···O3W^v	0.88 (2)	1.94 (2)	2.800 (6)	166 (2)
O3W—H32···O2^vi	0.87 (3)	1.88 (3)	2.703 (6)	157 (3)

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

Acknowledgements

The authors thank the EPSRC for funding of crystallographic facilities and for an Advanced Research Fellowship to DJP.

References

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Volume 60| Part 4| April 2004| Pages m378-m380

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