(Methoxo-κO)oxidobis(quinolin-8-olato-κ2 N,O)vanadium(V)

Zhenghua Guo; Lianzhi Li; Chengyuan Wang; Tao Xu; Jinghong Li

doi:10.1107/S1600536809031560

. 2009 Aug 15;65(Pt 9):m1075. doi: 10.1107/S1600536809031560

(Methoxo-κO)oxidobis(quinolin-8-olato-κ² N,O)vanadium(V)

Zhenghua Guo ^a, Lianzhi Li ^a,^*, Chengyuan Wang ^b, Tao Xu ^a, Jinghong Li ^a

PMCID: PMC2969990 PMID: 21577429

Abstract

In the title complex, [V(C₉H₆NO)₂(CH₃O)O], the central V^V atom is coordinated by the O atoms from the oxido and methoxo ligands and the N and O atoms of two bis-chelating quinolin-8-olate ligands, forming a distorted octahedral environment. In the crystal structure, weak intermolecular C—H⋯O hydrogen bonds connect molecules into centrosymmetric dimers which are, in turn, linked by weak C—H⋯π interactions into chains along the b axis.

Related literature

For the properties of vanadium compounds, see: Crans et al. (2004 ▶); Diego et al. (2003 ▶); Thompson & Orvig (2006 ▶). For the structures of oxidovandium complexes see: Hoshina et al. (1998 ▶); Otieno et al. (1996 ▶).

Experimental

Crystal data

[V(C₉H₆NO)₂(CH₃O)O]
M _r = 386.27
Monoclinic,
a = 14.0405 (16) Å
b = 8.0019 (1) Å
c = 15.5920 (18) Å
β = 110.560 (1)°
V = 1640.2 (3) Å³
Z = 4
Mo Kα radiation
μ = 0.63 mm⁻¹
T = 298 K
0.44 × 0.18 × 0.17 mm

Data collection

Bruker SMART 1000 CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.768, T _max = 0.900
7660 measured reflections
2893 independent reflections
1378 reflections with I > 2σ(I)
R _int = 0.102

Refinement

R[F ² > 2σ(F ²)] = 0.072
wR(F ²) = 0.230
S = 1.00
2893 reflections
235 parameters
H-atom parameters constrained
Δρ_max = 0.81 e Å⁻³
Δρ_min = −0.69 e Å⁻³

Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809031560/lh2870sup1.cif

e-65-m1075-sup1.cif^{(21.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809031560/lh2870Isup2.hkl

e-65-m1075-Isup2.hkl^{(142KB, hkl)}

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

Table 1. Selected bond angles (°).

O3—V1—O2	101.9 (2)
O3—V1—O1	91.4 (2)
O2—V1—O1	156.3 (2)
O3—V1—N1	164.3 (2)
O2—V1—N1	85.35 (19)
O1—V1—N1	77.40 (19)
O4—V1—N2	170.1 (2)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C9—H9⋯O4ⁱ	0.93	2.54	3.355 (8)	146
C19—H19B⋯Cgⁱⁱ	0.96	2.84	3.520 (9)	128

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Symmetry codes: (i) Inline graphic ; (ii) . Cg is the centroid of the N2/C10–C14 ring.

Acknowledgments

The authors thank the Natural Science Foundation of Shandong Province (No. Y2004B02) for a research grant.

supplementary crystallographic information

Comment

Vanadium is a biologically essential trace element, encountered in metalloenzymes such as haloperoxidases or nitrogenases. Its coordination chemistry has received increasing attention due to the fact that vanadium compounds in various oxidation states have insulin-mimetic properties (Diego et al., 2003; Crans et al., 2004; Thompson & Orvig, 2006). We report here the synthesis and crystal structure of the title complex.

In the molecular structure (Fig.1.), the central V^V atom is six-coordinated by the O atoms of the oxo and methoxo ligands and the N atoms and O atoms of two 8-hydroxyquinolato ligands, forming a distorted octahedral environment (Table 1). The V=O bond distance is 1.602 (4) Å which is typical for oxovandium complexes (Hoshina et al., 1998; Otieno et al., 1996). The mean planes of the chelated rings defined by N1/C5—C6/O1/V1 and N2/C14—C15/O2/V1 form a dihedral angle of 82.02 (18)°.

In the crystal structure, weak intermolecular C—H···O hydrogen bonds connect molecules into centrosymmetric dimers (Fig. 2) which are, in turn, linked by weak C—H···π interactions into chains along the b axis.

Experimental

8-Hydroxyquinoline (1 mmol, 145.16 mg) was dissolved in hot methanol (10 ml) and added dropwise to a methanol solution (3 ml) of VOSO₄.3H₂O (1 mmol, 225.4 mg). The mixture was then stirred at 323 K for 4 h. The solution was held at room temperature for 15 days, whereupon brown needle crystals suitable for X-ray diffraction were obtained.