(Ethano­lato-κO)[N′-(3-meth­oxy-2-oxidobenzyl­idene-κO 2)benzo­hydrazidato-κ2 N′,O]oxidovanadium(V)

Xiao-Hua Chen; Qiong-Jie Wu; Li-Juan Chen; Ming-Xing Yang

doi:10.1107/S1600536812032229

. 2012 Jul 21;68(Pt 8):m1101–m1102. doi: 10.1107/S1600536812032229

(Ethanolato-κO)[N′-(3-methoxy-2-oxidobenzylidene-κO ²)benzohydrazidato-κ² N′,O]oxidovanadium(V)

Xiao-Hua Chen ^a,^*, Qiong-Jie Wu ^b, Li-Juan Chen ^c, Ming-Xing Yang ^c

PMCID: PMC3414151 PMID: 22904758

Abstract

In the title complex, [V(C₁₅H₁₂N₂O₄)(C₂H₅O)O], the V^V ion is coordinated by an oxide O atom, an ethanolate anion and two O atoms and one N atom from the tridentate benzohydrazidate dianion in a distorted square-pyramidal geometry; the V atom is displaced by 0.4748 (8) Å from the basal plane towards the axial oxide O atom. An intramolecular O—H⋯N hydrogen bond occurs in the benzohydrazidate ligand. Weak intermolecular C—H⋯O hydrogen bonding is present in the crystal.

Related literature

For general background to the coordination chemistry and biochemisty of vanadium, see: Deng et al. (2007 ▶); Monfared et al. (2011 ▶); Sutradhar et al. (2006 ▶). For related structures, see: Chen et al. (2004 ▶); Liu et al. (2006 ▶); Ghosh et al. (2007 ▶); Seena et al. (2008 ▶). For the synthesis, see: Gao et al. (1998 ▶); Huang et al. (2010 ▶).

Experimental

Crystal data

[V(C₁₅H₁₂N₂O₄)(C₂H₅O)O]
M _r = 396.27
Monoclinic,
a = 15.808 (5) Å
b = 6.606 (2) Å
c = 16.693 (8) Å
β = 94.107 (16)°
V = 1738.6 (12) Å³
Z = 4
Mo Kα radiation
μ = 0.61 mm⁻¹
T = 293 K
0.37 × 0.25 × 0.13 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (TEXRAY; Molecular Structure Corporation, 1999 ▶) T _min = 0.834, T _max = 0.924
15371 measured reflections
3968 independent reflections
3243 reflections with I > 2σ(I)
R _int = 0.041

Refinement

R[F ² > 2σ(F ²)] = 0.038
wR(F ²) = 0.105
S = 1.08
3968 reflections
237 parameters
H-atom parameters constrained
Δρ_max = 0.34 e Å⁻³
Δρ_min = −0.22 e Å⁻³

Data collection: TEXRAY (Molecular Structure Corporation, 1999 ▶); cell refinement: TEXRAY; data reduction: TEXSAN (Molecular Structure Corporation, 1999 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEX (McArdle, 1995 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812032229/xu5587sup1.cif

e-68-m1101-sup1.cif^{(21.2KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812032229/xu5587Isup2.hkl

e-68-m1101-Isup2.hkl^{(194.5KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

V1—N1	2.1029 (15)
V1—O1	1.8325 (14)
V1—O3	1.9453 (14)
V1—O5	1.5762 (15)
V1—O6	1.7423 (13)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H4B⋯N2	0.82	1.86	2.581 (2)	147
C8—H8A⋯O4ⁱ	0.93	2.31	3.236 (2)	177

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Symmetry code: (i) Inline graphic .

Acknowledgments

The authors are grateful for financial support from the Foundation of Fujian Educational Committee, China (grant No. JB10007).

supplementary crystallographic information

Comment

In the recent years, the coordination chemistry and biochemisty of vanadium has received considerable attention (Deng et al., 2007; Monfared et al., 2011; Sutradhar et al., 2006). Generally, a tridentate hydrazone ligand is coordinated to the vanadium through O and N atoms, similar to those of the biological system. So, it is important to intensively study the relation ship of the syntheses and structural properties of vanadium hydrazone complexes.

In the title complex, [VO(C₁₅H₁₂N₂O₄)(C₂H₅O)], the V^V ion exists in a distorted square-pyramidal coordination geometry. Three donor atoms (O1, O3 and N1) of the hydrozone ligand and O6 atom from the ethanol group define the coordination basal plane, with a maximum mean plane deviation of 0.030 (1) Å. The V atom is displaced towards the axial oxo O atom by 0.4748 (8) Å from the basal plane. Bond distances (Table 1) and bond angles around V1 atom are compared with those in reported oxovanadium complexes (Chen et al., 2004; Seena et al., 2008; Liu et al.,2006; Ghosh et al., 2007). In the crystal structure there are the intramolecular O—H···N hydrogen bonding and intermolecular C—H···O hydrogen bonding (Table 2).

Experimental

VO(acac)₂ (acac = acetylacetonate) was synthesized according to the reported method of Gao et al. (1998). The synthesis of the hydrazone ligand has already been reported in the literature (Huang et al., 2010).

The title compound was prepared by reacting H₂L (0.1 mmol) with VO(acac)₂ (0.1 mmol) in ethanol solvent with stirring. The solution was filtered and allowed to stand at room temperature for one week, and dark-red crystals of complex (I) were obtained.