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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 10| October 2011| Page m1398
https://doi.org/10.1107/S1600536811037184

Di-μ-chlorido-bis­­[diaceto­nitrile­chlorido­oxidovanadium(IV)]

Dalibor Dastych,a* Pavel Rotter,b Gabriel Demob and Lenka Dastychováa

aDepartment of Chemistry, Faculty of Technology, Tomas Bata University in Zlin, Nam. T. G. Masaryka 275 Zlin, 762 72, Czech Republic, and bDepartment of Chemistry, Faculty of Science, Masaryk University, Kamenice 5 Brno–Bohunice, 625 00, Czech Republic
*Correspondence e-mail: dastych@gmail.com

(Received 18 August 2011; accepted 13 September 2011; online 17 September 2011)

The title compound, [V2Cl4O2(CH3CN)4], is a centrosymmetric dinuclear VIV complex associated with four mol­ecules of acetonitrile. The coordination around both VIV atoms is essentially square-planar, involving three Cl atoms and one O atom [maximum deviation = 0.017 (3) Å for the O atom]. The augmented octahedral coordination of the metal atom is completed by the N atoms of acetonitrile ligands. The VIV atoms are linked by two Cl atoms, acting as bridging atoms. The crystal studied was a non-merohedral twin with a ratio of the two twin components of 0.8200 (3):0.1800 (3). Although Cl and O atoms are present as potential acceptors in the title compound, no hydrogen bonds were observed in the crystal structure.

Related literature

For the biological activity of vanadium(IV) compounds, see: D'Cruz et al. (2003[D'Cruz, O. J., Dong, Y. H. & Uckun, F. M. (2003). Biochem. Biophys. Res. Commun. 302, 253-264.]); Lopez et al. (1976[Lopez, V., Stevens, T. & Lindquist, R. N. (1976). Arch. Biochem. Biophys. 175, 31-38.]); Lu et al. (2001[Lu, B., Enni, D., Lai, R., Bogdanovic, E., Nikolov, R., Salamon, L., Fantus, C., Le-Tien, H. & Fantus, I. G. (2001). J. Biol. Chem. 276, 35589-35598.]); Shi et al. (1996[Shi, X., Wang, P., Jiang, H., Mao, Y., Ahmed, N. & Dalal, N. (1996). Ann. Clin. Lab. Sci. 26, 39-49.]). For Ziegler–Natta catalysts, see: Hagen et al. (2002[Hagen, H., Boersma, J. & van Koten, G. (2002). Chem. Soc. Rev. 31, 357-364.]). For the synthesis of chloridooxidovanadium(IV) complexes, see: du Preez & Sadle (1967[Preez, J. G. H. du & Sadle, F. G. (1967). Inorg. Chim. Acta, 1, 202-204.]); Homden et al. (2009[Homden, D., Redshaw, C., Warford, L., Hughes, D. L., Wright, J. A., Dale, S. H. & Elsegood, M. R. J. (2009). Dalton Trans. pp. 8900-8910.]); Kern (1962[Kern, R. J. (1962). J. Inorg. Nucl. Chem. 24, 1105-1109.]); Papoutsakis et al. (2004[Papoutsakis, D., Ichimura, A. S., Young, V. G., Jackson, J. E. & Nocera, D. G. (2004). Dalton Trans. pp. 224-228.]); Priebsch & Rehder (1990[Priebsch, W. & Rehder, D. (1990). Inorg. Chem. 29, 3013-3019.]).

[Scheme 1]

Experimental

Crystal data

  • [V2Cl4O2(C2H3N)4]

  • Mr = 439.90

  • Triclinic, [P \overline 1]

  • a = 7.0242 (6) Å

  • b = 8.1388 (6) Å

  • c = 8.7118 (5) Å

  • α = 86.536 (6)°

  • β = 66.806 (7)°

  • γ = 74.374 (7)°

  • V = 440.28 (6) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.67 mm−1

  • T = 120 K

  • 0.30 × 0.20 × 0.15 mm
Data collection

  • Oxford Diffraction Xcalibur Sapphire2 diffractometer

  • Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis RED and CrysAlis CCD. Oxford Diffraction Ltd, Yarnton, England.]) Tmin = 0.804, Tmax = 1.000

  • 1550 measured reflections

  • 1550 independent reflections

  • 1432 reflections with I > 2σ(I)
Refinement

  • R[F2 > 2σ(F2)] = 0.031

  • wR(F2) = 0.103

  • S = 1.25

  • 1550 reflections

  • 94 parameters

  • H-atom parameters constrained

  • Δρmax = 0.47 e Å−3

  • Δρmin = −0.51 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis RED and CrysAlis CCD. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis RED and CrysAlis CCD. Oxford Diffraction Ltd, Yarnton, England.]); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]); molecular graphics: Mercury (Macrae et al., 2008[Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.]); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811037184/ru2013sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811037184/ru2013Isup2.hkl

checkCIF report


Comment top

Vanadium(IV) compounds exert biological activity such as inhibition for some phosphatases (D'Cruz et al., 2003; Lopez et al., 1976), modulation of cell's redox potential (Lu et al., 2001) or catalysis of the generation of reactive oxygen species (Shi et al., 1996). The oxovanadium(IV) complexes exhibit rapid selective spermicidal effects and their anti-HIV activity was studied too (D'Cruz et al., 2003). Chlorovanadium(IV) compounds are also used for catalysis in homogenous Ziegler-Natta polymerizations to prepare high-molecular-weight polymers with narrow molecular weight distribution (Hagen et al., 2002).

The dichloro(oxo)vanadium(IV) complex with acetonitrile was prepared for the first time by the reaction of VOCl2 with dry acetonitrile (du Preez et al. , 1967). The structure characteristic of the reaction product was performed only by means of UV, IR and conductivity measurements. The constitution of this reaction product was determined as VOCl2.2.5CH3CN. The only known crystal structure of acetonitrile adduct with dichloro(oxo)vanadium complex is to our knowledge [H3Np-tolyl][VOCl3(MeCN)2], which was prepared by the refluxing of [V(Np-tolyl)Cl3] in acetonitrile (Homden et al., 2009).

It is known a lot of VOCl2 adducts with organic solvents, namely VOCl2.2THF (Kern, 1962) and trans-VOCl2(THF)2(H2O) (Papoutsakis et al., 2004; Priebsch et al., 1990), cis-VOCl2(CH3OH)3 (Papoutsakis et al., 2004), trans-VOCl2(Et2O)2(H2O)2 (Papoutsakis et al., 2004) or VOCl2(HMPA)2 (du Preez et al., 1967). These adducts are presented in the known crystal structures as monomers in all cases (Papoutsakis et al., 2004; Priebsch et al., 1990). All of these complexes pick up very easily to the vanadium coordination sphere water molecules, therefore there are known only as water adducts (Papoutsakis et al., 2004). On this account, it is necessary to keep strictly nonaqueous solution to obtain dichloro(oxo)vanadium complexes without water in the vanadium coordination sphere.

The asymmetric unit of the title compound consists of a single vanadium(IV) complex molecule associated with four molecules of acetonitrile (Fig. 1). Both of chlorine bridge atoms are situated essentially in the same plane with vanadium atoms, as demonstrated by torsion angles V1—Cl1—V1A—Cl1A 0.0° and O1—V1—Cl1—V1A, which is 179.36 (11)°, respectively. The angle describing the triple bond in acetonitrile is N2≡C3—C4 179.6 (4)° and N1≡C1—C2 179.1 (4)°, respectively. The crystal packing is showed in Fig. 2.

Related literature top

For the biological activity of vanadium(IV) compounds, see: D'Cruz et al. (2003); Lopez et al. (1976); Lu et al. (2001); Shi et al. (1996). For Ziegler–Natta catalysts, see: Hagen et al. (2002). For the synthesis of chloridooxidovanadium(IV) complexes, see: du Preez et al. (1967); Homden et al. (2009); Kern (1962); Papoutsakis et al. (2004); Priebsch et al. (1990).

Experimental top

The title compound was obtained by the reaction of VOCl3 with N,N'-bis(trimethylsilyl)urea in acetonitrile. N,N'-bis(trimethylsilyl)urea (3.0 mmol) was dissolved in 100 cm3 of dry acetonitrile at 70 °C. The solutoin of VOCl3 (2.6 mmol) in in dry acetonitrile (50 cm3) was quickly added to the solution of N, N'-bis(trimethylsilyl)urea and the reaction mixture was refluxed for 17 h. The solvent was partially distilled off after the reaction and the total volume was reduced to 25 cm3. Dry CCl4 (25 cm3) was consequently added to the concentrated acetonitrile solution and two liquid phases were formed. Blue crystals of [(µ-Cl)2(VOCl2(CH3CN)2)2] grew up from the surface of the denser phase after 4 days standing at room temperature.

Refinement top

The investigated crystal was a non-merohedral twin [twin law: rotation of 180° around the [101] direction].. The twin law was determined using TwinRotMat implemented in PLATON (Spek, 2009). The twinning coefficient of the crystal is 0.180040. The description of twin law in transformation matrix is: (0.397 - 0.364 0.603) (0.000 - 1.000 0.000) (1.397 - 0.364 - 0.397) The detwinned data were obtained by HKLF 5 option in the SHELXL97 program (Sheldrick, 2008) and the final refinement was carried out against the detwinned data set.

Structure description top

Vanadium(IV) compounds exert biological activity such as inhibition for some phosphatases (D'Cruz et al., 2003; Lopez et al., 1976), modulation of cell's redox potential (Lu et al., 2001) or catalysis of the generation of reactive oxygen species (Shi et al., 1996). The oxovanadium(IV) complexes exhibit rapid selective spermicidal effects and their anti-HIV activity was studied too (D'Cruz et al., 2003). Chlorovanadium(IV) compounds are also used for catalysis in homogenous Ziegler-Natta polymerizations to prepare high-molecular-weight polymers with narrow molecular weight distribution (Hagen et al., 2002).

The dichloro(oxo)vanadium(IV) complex with acetonitrile was prepared for the first time by the reaction of VOCl2 with dry acetonitrile (du Preez et al. , 1967). The structure characteristic of the reaction product was performed only by means of UV, IR and conductivity measurements. The constitution of this reaction product was determined as VOCl2.2.5CH3CN. The only known crystal structure of acetonitrile adduct with dichloro(oxo)vanadium complex is to our knowledge [H3Np-tolyl][VOCl3(MeCN)2], which was prepared by the refluxing of [V(Np-tolyl)Cl3] in acetonitrile (Homden et al., 2009).

It is known a lot of VOCl2 adducts with organic solvents, namely VOCl2.2THF (Kern, 1962) and trans-VOCl2(THF)2(H2O) (Papoutsakis et al., 2004; Priebsch et al., 1990), cis-VOCl2(CH3OH)3 (Papoutsakis et al., 2004), trans-VOCl2(Et2O)2(H2O)2 (Papoutsakis et al., 2004) or VOCl2(HMPA)2 (du Preez et al., 1967). These adducts are presented in the known crystal structures as monomers in all cases (Papoutsakis et al., 2004; Priebsch et al., 1990). All of these complexes pick up very easily to the vanadium coordination sphere water molecules, therefore there are known only as water adducts (Papoutsakis et al., 2004). On this account, it is necessary to keep strictly nonaqueous solution to obtain dichloro(oxo)vanadium complexes without water in the vanadium coordination sphere.

The asymmetric unit of the title compound consists of a single vanadium(IV) complex molecule associated with four molecules of acetonitrile (Fig. 1). Both of chlorine bridge atoms are situated essentially in the same plane with vanadium atoms, as demonstrated by torsion angles V1—Cl1—V1A—Cl1A 0.0° and O1—V1—Cl1—V1A, which is 179.36 (11)°, respectively. The angle describing the triple bond in acetonitrile is N2≡C3—C4 179.6 (4)° and N1≡C1—C2 179.1 (4)°, respectively. The crystal packing is showed in Fig. 2.

For the biological activity of vanadium(IV) compounds, see: D'Cruz et al. (2003); Lopez et al. (1976); Lu et al. (2001); Shi et al. (1996). For Ziegler–Natta catalysts, see: Hagen et al. (2002). For the synthesis of chloridooxidovanadium(IV) complexes, see: du Preez et al. (1967); Homden et al. (2009); Kern (1962); Papoutsakis et al. (2004); Priebsch et al. (1990).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2009); cell refinement: CrysAlis RED (Oxford Diffraction, 2009); data reduction: CrysAlis RED (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Crystal structure of the title compound. Thermal elipsoids are drawn with 50 % probability level, hydrogen atoms are represented as arbitrary spheres.
[Figure 2] Fig. 2. A view of the crystal structure of the title compound showing chains parallel to the ab-plane made up by C—H···Cl and C—H···O weak interactions (dashed lines). Thermal elipsoids are drawn with 50 % probability level.
Di-µ-chlorido-bis[diacetonitrilechloridooxidovanadium(IV)] top
Crystal data top
[V2Cl4O2(C2H3N)4]Z = 1
Mr = 439.90F(000) = 218
Triclinic, P1Dx = 1.659 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.7107 Å
a = 7.0242 (6) ÅCell parameters from 5307 reflections
b = 8.1388 (6) Åθ = 3.3–25.0°
c = 8.7118 (5) ŵ = 1.67 mm−1
α = 86.536 (6)°T = 120 K
β = 66.806 (7)°Block, blue
γ = 74.374 (7)°0.30 × 0.20 × 0.15 mm
V = 440.28 (6) Å3
Data collection top
Oxford Diffraction Xcalibur Sapphire2
diffractometer		1550 independent reflections
Radiation source: Enhance (Mo) X-ray Source1432 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
Detector resolution: 8.4 pixels mm-1θmax = 25.0°, θmin = 3.3°
ω scansh = −7→8
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2009)		k = −9→9
Tmin = 0.804, Tmax = 1.000l = −9→10
1550 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H-atom parameters constrained
S = 1.25 w = 1/[σ2(Fo2) + (0.0397P)2 + 1.0484P]
where P = (Fo2 + 2Fc2)/3
1550 reflections(Δ/σ)max < 0.001
94 parametersΔρmax = 0.47 e Å−3
0 restraintsΔρmin = −0.51 e Å−3
Crystal data top
[V2Cl4O2(C2H3N)4]γ = 74.374 (7)°
Mr = 439.90V = 440.28 (6) Å3
Triclinic, P1Z = 1
a = 7.0242 (6) ÅMo Kα radiation
b = 8.1388 (6) ŵ = 1.67 mm−1
c = 8.7118 (5) ÅT = 120 K
α = 86.536 (6)°0.30 × 0.20 × 0.15 mm
β = 66.806 (7)°
Data collection top
Oxford Diffraction Xcalibur Sapphire2
diffractometer		1550 independent reflections
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2009)		1432 reflections with I > 2σ(I)
Tmin = 0.804, Tmax = 1.000Rint = 0.000
1550 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0310 restraints
wR(F2) = 0.103H-atom parameters constrained
S = 1.25Δρmax = 0.47 e Å−3
1550 reflectionsΔρmin = −0.51 e Å−3
94 parameters
Special details top

Experimental. empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm

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
xyzUiso*/Ueq
V10.58161 (10)0.06353 (8)0.67541 (8)0.0141 (2)
Cl10.71230 (14)−0.15703 (11)0.46017 (11)0.0172 (2)
Cl20.38000 (14)0.30593 (12)0.85537 (12)0.0201 (2)
O10.7642 (4)−0.0069 (3)0.7454 (3)0.0192 (6)
N20.7440 (5)0.2175 (4)0.5012 (4)0.0197 (7)
C40.9873 (6)0.3945 (5)0.3008 (5)0.0228 (8)
H4A0.89810.50710.29160.034*
H4B1.06450.33510.19010.034*
H4C1.09110.40830.34480.034*
C20.1588 (7)−0.2589 (5)1.0454 (5)0.0241 (9)
H2A0.0118−0.22741.05000.036*
H2B0.1555−0.23851.15630.036*
H2C0.2258−0.38011.01050.036*
N10.3766 (5)−0.0747 (4)0.8326 (4)0.0190 (7)
C30.8514 (6)0.2950 (5)0.4132 (5)0.0193 (8)
C10.2821 (6)−0.1565 (5)0.9263 (5)0.0190 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0142 (3)0.0150 (3)0.0125 (3)−0.0029 (2)−0.0051 (3)−0.0007 (2)
Cl10.0173 (4)0.0172 (5)0.0155 (5)−0.0002 (3)−0.0071 (4)−0.0039 (3)
Cl20.0191 (5)0.0192 (5)0.0197 (5)−0.0014 (4)−0.0066 (4)−0.0054 (4)
O10.0197 (14)0.0202 (14)0.0188 (14)−0.0028 (11)−0.0100 (11)−0.0016 (11)
N20.0180 (16)0.0195 (17)0.0177 (17)−0.0033 (14)−0.0039 (14)−0.0002 (14)
C40.025 (2)0.024 (2)0.020 (2)−0.0099 (17)−0.0079 (17)0.0039 (16)
C20.025 (2)0.024 (2)0.023 (2)−0.0136 (17)−0.0040 (17)0.0005 (17)
N10.0219 (16)0.0209 (17)0.0135 (16)−0.0070 (14)−0.0051 (14)−0.0010 (14)
C30.0182 (19)0.019 (2)0.020 (2)0.0008 (16)−0.0096 (17)−0.0040 (16)
C10.0200 (19)0.0182 (19)0.019 (2)−0.0030 (16)−0.0087 (16)−0.0028 (16)
Geometric parameters (Å, º) top
V1—O11.588 (3)C4—H4A0.9800
V1—N12.085 (3)C4—H4B0.9800
V1—N22.086 (3)C4—H4C0.9800
V1—Cl22.3399 (10)C2—C11.448 (6)
V1—Cl12.3969 (10)C2—H2A0.9800
V1—Cl1i2.6836 (10)C2—H2B0.9800
Cl1—V1i2.6836 (10)C2—H2C0.9800
N2—C31.139 (5)N1—C11.138 (5)
C4—C31.453 (6)
O1—V1—N194.79 (14)C3—N2—V1171.8 (3)
O1—V1—N295.52 (14)C3—C4—H4A109.5
N1—V1—N2169.69 (13)C3—C4—H4B109.5
O1—V1—Cl299.62 (10)H4A—C4—H4B109.5
N1—V1—Cl289.60 (9)C3—C4—H4C109.5
N2—V1—Cl288.90 (9)H4A—C4—H4C109.5
O1—V1—Cl196.44 (10)H4B—C4—H4C109.5
N1—V1—Cl189.01 (9)C1—C2—H2A109.5
N2—V1—Cl189.61 (9)C1—C2—H2B109.5
Cl2—V1—Cl1163.95 (4)H2A—C2—H2B109.5
O1—V1—Cl1i174.92 (10)C1—C2—H2C109.5
N1—V1—Cl1i84.57 (9)H2A—C2—H2C109.5
N2—V1—Cl1i85.15 (9)H2B—C2—H2C109.5
Cl2—V1—Cl1i85.42 (3)C1—N1—V1172.0 (3)
Cl1—V1—Cl1i78.53 (4)N2—C3—C4179.6 (4)
V1—Cl1—V1i101.47 (4)N1—C1—C2179.1 (4)
O1—V1—Cl1—V1i179.36 (11)Cl2—V1—Cl1—V1i−0.47 (16)
N1—V1—Cl1—V1i84.66 (9)Cl1i—V1—Cl1—V1i0.0
N2—V1—Cl1—V1i−85.13 (9)
Symmetry code: (i) −x+1, −y, −z+1.

Experimental details

Crystal data
Chemical formula[V2Cl4O2(C2H3N)4]
Mr439.90
Crystal system, space groupTriclinic, P1
Temperature (K)120
a, b, c (Å)7.0242 (6), 8.1388 (6), 8.7118 (5)
α, β, γ (°)86.536 (6), 66.806 (7), 74.374 (7)
V (Å3)440.28 (6)
Z1
Radiation typeMo Kα
µ (mm−1)1.67
Crystal size (mm)0.30 × 0.20 × 0.15
Data collection
DiffractometerOxford Diffraction Xcalibur Sapphire2
Absorption correctionMulti-scan
(CrysAlis RED; Oxford Diffraction, 2009)
Tmin, Tmax0.804, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections		1550, 1550, 1432
Rint0.000
(sin θ/λ)max (Å−1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.103, 1.25
No. of reflections1550
No. of parameters94
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.47, −0.51

Computer programs: CrysAlis CCD (Oxford Diffraction, 2009), CrysAlis RED (Oxford Diffraction, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009), Mercury (Macrae et al., 2008), SHELXL97 (Sheldrick, 2008).

 

References

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ISSN: 2056-9890
Volume 67| Part 10| October 2011| Page m1398
https://doi.org/10.1107/S1600536811037184
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