Di-μ1,1-azido-bis­[azido­(5,5′-dimethyl-2,2′-bipyridine)nickel(II)]

Jin Hou

doi:10.1107/S1600536808037902

. 2008 Nov 20;64(Pt 12):m1571. doi: 10.1107/S1600536808037902

Di-μ_1,1-azido-bis[azido(5,5′-dimethyl-2,2′-bipyridine)nickel(II)]

Jin Hou ^a,^*

PMCID: PMC2959945 PMID: 21581175

Abstract

In the title azide-bridged dinuclear centrosymmetric nickel(II) complex, [Ni₂(N₃)₄(C₁₂H₁₂N₂)₂], the Ni^II atom is five-coordinated by two N atoms of the 5,5′-dimethyl-2,2′-bipyridine ligand and three N atoms from three azide ligands in a distorted trigonal–bipyramidal geometry. The Ni⋯Ni distance is 3.2398 (12) Å.

Related literature

For general background, see: Abramo et al. (2002 ▶); Dey et al. (2007 ▶); Jiang et al. (2005 ▶). For related structures, see: Fu et al. (2005 ▶); Song et al. (2007 ▶).

Experimental

Crystal data

[Ni₂(N₃)₄(C₁₂H₁₂N₂)₂]
M _r = 654.01
Monoclinic,
a = 7.938 (2) Å
b = 15.067 (3) Å
c = 11.755 (2) Å
β = 91.650 (2)°
V = 1405.3 (5) Å³
Z = 2
Mo Kα radiation
μ = 1.39 mm⁻¹
T = 298 (2) K
0.13 × 0.10 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.840, T _max = 0.897
11588 measured reflections
3060 independent reflections
2165 reflections with I > 2σ(I)
R _int = 0.063

Refinement

R[F ² > 2σ(F ²)] = 0.056
wR(F ²) = 0.149
S = 1.03
3060 reflections
192 parameters
14 restraints
H-atom parameters constrained
Δρ_max = 0.67 e Å⁻³
Δρ_min = −0.77 e Å⁻³

Data collection: SMART (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; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808037902/ci2712sup1.cif

e-64-m1571-sup1.cif^{(15.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808037902/ci2712Isup2.hkl

e-64-m1571-Isup2.hkl^{(150.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Ni1—N1	2.145 (4)
Ni1—N2	2.081 (4)
Ni1—N3	2.064 (5)
Ni1—N6	2.041 (4)
Ni1—N6ⁱ	2.175 (4)

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Symmetry code: (i) Inline graphic .

supplementary crystallographic information

Comment

Polynuclear complexes play an important role in many fields, such as catalysis and magnetism (Dey et al., 2007; Jiang et al., 2005; Abramo et al., 2002). The main strategy for the design of the polynuclear complexes is to use suitable bridging ligands. In this paper, we report the synthesis and molecular structure of the title azide-bridged dinuclear nickel(II) complex derived from 5,5'-dimethyl-[2,2']bipyridine.

The molecule of the title complex is located on a crystallographic centre of inversion (Fig. 1). The complex contains two NiL (L is 5,5'-dimethyl-[2,2']bipyridine) units connected to each other by two bridging azide ligands. The Ni^II atom in the complex is five-coordinated by two N atoms of 5,5'-dimethyl-[2,2']bipyridine ligand and by three N atoms from three azide ligands in a trigonal-bipyramidal geometry. The bond lengths subtended at the metal center are within normal ranges (Song et al., 2007; Fu et al., 2005). The Ni···Ni distance is 3.2398 (12) Å.

Experimental

5,5'-Dimethyl-[2,2']bipyridine (2 mmol, 368.3 mg), sodium azide (4 mmol, 261.2 mg) and nickel acetate tetrahydrate (2 mmol, 497.8 mg) were dissolved in methanol (100 ml). The mixture was stirred for 30 min at room temperature to give a green solution. The solution was kept still in air for a week, green block-shaped crystals of the title complex were formed.