{2-[(2-Amino­cyclo­hex­yl)imino­meth­yl]phenolato}dioxidovanadium(V)

Xin-Zhi Sun

doi:10.1107/S1600536812011592

. 2012 Mar 24;68(Pt 4):m476. doi: 10.1107/S1600536812011592

{2-[(2-Aminocyclohexyl)iminomethyl]phenolato}dioxidovanadium(V)

Xin-Zhi Sun ^a,^*

PMCID: PMC3343864 PMID: 22589838

Abstract

In the title dioxidovanadium complex, [V(C₁₃H₁₇N₂O)O₂], the V^V atom is in a square-based pyramidal coordination: the basal plane is defined by the phenolate O, imine N and amine N atoms of the tridentate Schiff base ligand, and by one oxide O atom. The apical position is occupied by the other oxide O atom. In the crystal, molecules are connected by N—H⋯O and N—H⋯(O,O) hydrogen bonds, forming a tetramer.

Related literature

For related structures and their proporties, see: Agarwal & Prasad (2006 ▶); Chohan & Sumrra (2010 ▶); Huo et al. (2004 ▶); Jing et al. (2005 ▶); Lodyga-Chruscinska et al. (2008 ▶); Xie et al. (2004 ▶); Yuan et al. (2009 ▶).

Experimental

Crystal data

[V(C₁₃H₁₇N₂O)O₂]
M _r = 300.23
Tetragonal,
a = 19.120 (9) Å
c = 15.421 (3) Å
V = 5638 (4) Å³
Z = 16
Mo Kα radiation
μ = 0.71 mm⁻¹
T = 298 K
0.23 × 0.20 × 0.20 mm

Data collection

Bruker SMART 1000 CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2000 ▶) T _min = 0.854, T _max = 0.871
19404 measured reflections
2537 independent reflections
1487 reflections with I > 2σ(I)
R _int = 0.172

Refinement

R[F ² > 2σ(F ²)] = 0.099
wR(F ²) = 0.203
S = 1.08
2537 reflections
172 parameters
H-atom parameters constrained
Δρ_max = 0.44 e Å⁻³
Δρ_min = −0.30 e Å⁻³

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812011592/hb6676sup1.cif

e-68-0m476-sup1.cif^{(16.4KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812011592/hb6676Isup2.hkl

e-68-0m476-Isup2.hkl^{(124.9KB, hkl)}

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

Table 1. Selected bond lengths (Å).

V1—O2	1.607 (5)
V1—O3	1.621 (5)
V1—O1	1.900 (5)
V1—N2	2.095 (5)
V1—N1	2.137 (6)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2B⋯O2ⁱ	0.90	2.26	3.099 (7)	155
N2—H2B⋯O3ⁱ	0.90	2.55	3.229 (7)	133
N2—H2A⋯O3ⁱⁱ	0.90	2.07	2.948 (7)	166

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Symmetry codes: (i) Inline graphic ; (ii) .

Acknowledgments

The author acknowledges the Qingdao Agricultural University for financial support.

supplementary crystallographic information

Comment

Oxovanadium complexes with Schiff bases have been received much attention in bioinorganic chemistry (Chohan & Sumrra, 2010; Agarwal & Prasad, 2006; Lodyga-Chruscinska et al., 2008; Yuan et al., 2009). In this paper, the title new dioxovanadium(V) complex, (I), is reported.

In the title dioxovanadium complex, Fig. 1, the V atom is in a square pyramidal coordination. The basal plane of the square pyramid is defined by one phenolate O, one imine N, and one amine N atoms of a Schiff base ligand, and by one oxo O atom. The apical position of the square pyramid is occupied by the other oxo O atom. The bond lengths (Table 1) are comparable to those observed in similar oxovanadium complexes (Xie et al., 2004; Jing et al., 2005; Huo et al., 2004). In the crystal, adjacent molecules are linked through N–H···O and N—H···(O,O) hydrogen bonds (Table 2) to form a tetramer (Fig. 2).

Experimental

To a MeOH solution (30 ml) of salicylaldehyde (0.122 g, 1.0 mmol) was added a MeOH solution (20 ml) of cyclohexane-1,2-diamine (0.114 g, 1.0 mmol) with stirring. To the above mixture was added a MeOH solution (10 ml) of VO(acac)₂ (0.265 g, 1.0 mmol) with stirring. The mixture was refluxed for 1 h, affording a clear yellow solution. This was allowed to stand at room temperature for a week and block-shaped single crystals were obtained by slow evaporation.