Diaqua­bis­[4-(4H-1,2,4-triazol-4-yl)benzoato-κ2 O,O′]nickel(II)

Shuzhi Xu; Wenxin Shao; Miao Yu; Guihua Gong

doi:10.1107/S1600536811016643

. 2011 May 7;67(Pt 6):m728. doi: 10.1107/S1600536811016643

Diaquabis[4-(4H-1,2,4-triazol-4-yl)benzoato-κ² O,O′]nickel(II)

Shuzhi Xu ^a,^*, Wenxin Shao ^a, Miao Yu ^a, Guihua Gong ^a

PMCID: PMC3120528 PMID: 21754624

Abstract

In the title compound, [Ni(C₉H₆N₃O₂)₂(H₂O)₂], the Ni^II atom lies on a twofold rotation axis and is six-coordinated by two bidentate chelating 4-(1,2,4-triazol-4-yl)benzoate ligands and two water molecules in a distorted octahedral geometry. Intermolecular O—H⋯N hydrogen bonds link the complex molecules into a two-dimensional network parallel to (010).

Related literature

For general background to the structures and applications of metal complexes, see: Mahata et al. (2009 ▶); Perry et al. (2004 ▶); Qin et al. (2005 ▶); Shi et al. (2009 ▶). For a related structure, see: Zhu (2010 ▶).

Experimental

Crystal data

[Ni(C₉H₆N₃O₂)₂(H₂O)₂]
M _r = 471.06
Monoclinic,
a = 13.5194 (6) Å
b = 9.8480 (5) Å
c = 14.3234 (7) Å
β = 112.293 (1)°
V = 1764.47 (15) Å³
Z = 4
Mo Kα radiation
μ = 1.16 mm⁻¹
T = 296 K
0.28 × 0.24 × 0.22 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.72, T _max = 0.82
4732 measured reflections
1744 independent reflections
1662 reflections with I > 2σ(I)
R _int = 0.021

Refinement

R[F ² > 2σ(F ²)] = 0.030
wR(F ²) = 0.084
S = 1.13
1744 reflections
147 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.31 e Å⁻³
Δρ_min = −0.45 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and Mercury (Macrae et al., 2006 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811016643/hy2427sup1.cif

e-67-0m728-sup1.cif^{(16.4KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811016643/hy2427Isup2.hkl

e-67-0m728-Isup2.hkl^{(84.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Ni1—O1	2.1507 (14)
Ni1—O2	2.1240 (14)
Ni1—O3	2.0453 (16)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3B⋯N2ⁱ	0.78 (2)	2.06 (2)	2.836 (2)	172 (3)
O3—H3A⋯N3ⁱⁱ	0.79 (2)	1.99 (2)	2.768 (2)	169 (3)

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

Acknowledgments

We thank Jilin Business and Technology College for supporting this work.

supplementary crystallographic information

Comment

The construction of novel coordination complexes is the current interest in the field of supramolecular chemistry and crystal engineering stemming from their potential applications as functional materials, as well as their intriguing variety of architectures and topologies (Perry et al., 2004; Qin et al., 2005). Heterocyclic carboxylates have often been used as mono-, bi- or multi-dentate ligands to bind transition metal centers, leading to the formation of moderately robust metal–organic coordination frameworks (Mahata et al., 2009; Shi et al., 2009). In this contribution, we selected 4-(1,2,4-triazol-4-yl)benzoic acid (Htyb) as an organic carboxylate ligand, generating the title compound, which is reported here.

In the title compound, the Ni^II atom lies on a twofold rotation axis and adopts a distorted octahedral coordination geometry, being coordinated by four carboxylate O atoms from two tyb ligands and two water molecules (Fig. 1, Table 1). The Ni—O bond lengths and the O—Ni—O bond angles are in the normal range (Zhu, 2010). Intermolecular O—H···N hydrogen bonds (Table 2) stabilize the structure and give a two-dimensional network (Fig. 2).

Experimental

The synthesis was performed under hydrothermal conditions. A mixture of Ni(CH₃COO)₂.4H₂O (0.2 mmol, 0.05 g), 4-(1,2,4-triazol-4-yl)benzoic acid (0.4 mmol, 0.075 g), NaOH (0.4 mmol, 0.016 g) and H₂O (15 ml) in a 25 ml stainless steel reactor with a Teflon liner was heated from 293 to 443 K in 2 h and a constant temperature was maintained at 443 K for 72 h. After the mixture was cooled to 298 K, green crystals of the title compound were obtained.