Tetra­aqua­bis(3,5-di-4-pyridyl-1,2,4-triazolato-κN)nickel(II) dihydrate

Lin Yi Dong

doi:10.1107/S1600536809027688

. 2009 Jul 22;65(Pt 8):m962–m963. doi: 10.1107/S1600536809027688

Tetraaquabis(3,5-di-4-pyridyl-1,2,4-triazolato-κN)nickel(II) dihydrate

Lin Yi Dong ^a,^*

PMCID: PMC2977209 PMID: 21583408

Abstract

The Ni^II atom in the title compound, [Ni(C₁₂H₈N₅)₂(H₂O)₄]·2H₂O, lies on a center of inversion and is coordinated by the N atoms of two 3,5-di-4-pyridine-1,2,4-triazolate ligands and by four water O atoms in a slightly distorted octahedral geometry. The coordinated and uncoordinated water molecules interact with the N-heterocycles through O—H⋯N and O—H⋯O hydrogen bonds, generating a three-dimensional supramolecular architecture.

Related literature

For magnetic studies of transition metal complexes with 1,2,4- triazole derivatives, see: Haasnoot (2000 ▶). For 3,5-di-4-pyridine-1,2,4-triazole, see: Zhang et al. (2005 ▶, 2006 ▶). For the synthesis, see: Basu & Dutta (1964 ▶).

Experimental

Crystal data

[Ni(C₁₂H₈N₅)₂(H₂O)₄]·2H₂O
M _r = 611.27
Monoclinic,
a = 7.3390 (15) Å
b = 15.653 (3) Å
c = 11.829 (2) Å
β = 107.20 (3)°
V = 1298.1 (5) Å³
Z = 2
Mo Kα radiation
μ = 0.81 mm⁻¹
T = 293 K
0.43 × 0.27 × 0.21 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.722, T _max = 0.848
10883 measured reflections
2344 independent reflections
2131 reflections with I > 2σ(I)
R _int = 0.034

Refinement

R[F ² > 2σ(F ²)] = 0.036
wR(F ²) = 0.078
S = 1.14
2344 reflections
211 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.26 e Å⁻³
Δρ_min = −0.34 e Å⁻³

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1999 ▶); 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 datablocks I, global. DOI: 10.1107/S1600536809027688/hg2531sup1.cif

e-65-0m962-sup1.cif^{(18.6KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809027688/hg2531Isup2.hkl

e-65-0m962-Isup2.hkl^{(115.2KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2A⋯O3ⁱ	0.82 (3)	2.03 (3)	2.818 (3)	160 (3)
O3—H3A⋯N4ⁱⁱ	0.85 (3)	2.09 (3)	2.939 (3)	172 (3)
O3—H3B⋯N5ⁱⁱⁱ	0.86 (4)	1.94 (4)	2.789 (3)	173 (3)

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

supplementary crystallographic information

Comment

Transition metal complexes with 1,2,4-triazole derivatives as ligands are of great interest as they are the subject of magnetic studies (Haasnoot, 2000). The ligand 3,5-di(4-pyridine)-1,2,4-triazole is of special interest as it contains multi-dentate donor atoms and shows diverse coordination modes. Especially only a few examples about the coordinaiton chemistry of L are reported. Some unusual coordination modes of L also have been reported forming interesting supramolecular isomerism systems (Zhang et al., 2006).

In this work, we synthesized a new compound [Ni(L)₂(H₂O)₄](H₂O)₂ (L = 3,5-di(4-pyridine)-1,2,4-triazolate anions), which is composed of one nickel(II) cation, two L ligand, four coordinated and two lattice water molecules. The nickel(II) cation is six-coordinated in the octahedral geometry. The equatorial site of nickel cation is occupied by four aqua molecules while the axial site is occupied by two nitrogen atoms of two mono-dentate L ligands. The mono-dentate coordination mode of L is different from previously reported di-, tri- or tetra-dentate coordination modes of L (Zhang et al., 2005; Zhang et al., 2006).

O3 acts as both a hydrogen bond donor and a hydrogen bond acceptor. Strong O—H···N and O—H···O hydrogen bonds generated from water molecules and nitrogen atoms of pyridine or triazole groups are also observed resulting in the three-dimensional supramolecular network.

Experimental

The ligand was prepared according to the previous literature (Basu & Dutta, (1964)). [Ni(L)₂(H₂O)₄](H₂O) (I) (L = 3,5- di(4-pyridine)-1,2,4-triazole) was prepared under the hydrothermal conditions. [Ni(ClO₄)₂].6H₂O (0.2 mmol), L (0.2 mmol) and 18 ml water was added to a 25 ml reaction vessel. The reaction vessel was then sealed and subsequently placed in an oven for 140 h at 160°C well shaped green block crystals were obtained and washed with ethanol.