catena-Poly[[bis­(pyridine-κN)nickel(II)]-μ-oxalato-κ4 O 1,O 2:O 1′,O 2′]

Zhen-Yu Xuan; Yong Che; Yong-Chun Huang

doi:10.1107/S1600536808021703

. 2008 Jul 19;64(Pt 8):m1040. doi: 10.1107/S1600536808021703

catena-Poly[[bis(pyridine-κN)nickel(II)]-μ-oxalato-κ⁴ O ¹,O ²:O ^1′,O ^2′]

Zhen-Yu Xuan ^a,^*, Yong Che ^a, Yong-Chun Huang ^a

PMCID: PMC2961960 PMID: 21203030

Abstract

The title compound, [Ni(C₂O₄)(C₅H₅N)₂]_n, was synthesized under hydro(solvo)thermal conditions. The Ni^II atom, lying on a twofold rotation axis, has an octahedral coordination geometry involving two N atoms from two pyridine ligands and four O atoms from two oxalate ligands. The Ni atoms are connected by the tetradentate bridging oxalate ligands into a one-dimensional zigzag chain.

Related literature

For related literature, see: Lu et al. (1999 ▶); Vaidhyanathan et al. (2002 ▶); Wang et al. (2007 ▶); Yao et al. (2007 ▶).

Experimental

Crystal data

[Ni(C₂O₄)(C₅H₅N)₂]
M _r = 304.93
Monoclinic,
a = 14.357 (3) Å
b = 10.801 (2) Å
c = 8.6669 (17) Å
β = 91.52 (3)°
V = 1343.5 (5) Å³
Z = 4
Mo Kα radiation
μ = 1.45 mm⁻¹
T = 293 (2) K
0.26 × 0.24 × 0.22 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.640, T _max = 0.726
6433 measured reflections
1519 independent reflections
1297 reflections with I > 2σ(I)
R _int = 0.041

Refinement

R[F ² > 2σ(F ²)] = 0.042
wR(F ²) = 0.103
S = 1.04
1519 reflections
87 parameters
H-atom parameters constrained
Δρ_max = 0.73 e Å⁻³
Δρ_min = −0.30 e Å⁻³

Data collection: PROCESS-AUTO (Rigaku, 1998 ▶); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808021703/hy2144sup1.cif

e-64-m1040-sup1.cif^{(12.3KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808021703/hy2144Isup2.hkl

e-64-m1040-Isup2.hkl^{(75KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Ni1—O2ⁱ	2.046 (2)
Ni1—O1	2.0716 (18)
Ni1—N1	2.081 (2)

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O2ⁱ—Ni1—O2ⁱⁱ	168.78 (10)
O2ⁱ—Ni1—O1	89.88 (7)
O2ⁱⁱ—Ni1—O1	81.96 (7)
O1—Ni1—O1ⁱⁱⁱ	86.81 (11)
O2ⁱ—Ni1—N1	94.02 (8)
O2ⁱⁱ—Ni1—N1	93.66 (9)
O1—Ni1—N1	89.92 (9)
O1ⁱⁱⁱ—Ni1—N1	174.81 (8)
N1—Ni1—N1ⁱⁱⁱ	93.61 (13)

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

Acknowledgments

The authors thank Yanbian University for supporting this work.

supplementary crystallographic information

Comment

Much research work has been done on metal–oxalate compounds, in the context of studies of molecular-based magnets and open framework structures (Lu et al., 1999; Yao et al., 2007). The geometrical coordination mode and strength of this ligand provide both rigidity and preferred coordination specificity for metal centers (Vaidhyanathan et al., 2002; Wang et al., 2007). In this paper, we report the hydro(solvo)thermal synthesis and structure of a new one-dimensional nickelous oxalate coordination polymer.

The title compound consists of one Ni^II atom lying on a twofold rotation axis, an oxalate ligand and two coordinated pyridine molecules (Fig. 1). The Ni^II atom exhibits a distorted octahedral geometry, defined by four O atoms of two oxalate ligands and two pyridine N atoms in a cis arrangement. The Ni—O distances are 2.046 (2) and 2.0716 (18) Å, while the O—Ni—O angles show distortions particularly as a result of chelation (Table 1). The tetradentate oxalate ligands link adjacent Ni atoms into a one-dimensional zigzag chain.

Experimental

A mixture of K₂C₂O₄.H₂O (0.037 g, 0.2 mmol), H₃BO₃ (0.013 g, 0.2 mmol), NiCl₂.2H₂O (0.033 g, 0.2 mmol), KOH (0.012 g, 0.2 mmol), pyridine (4 ml) and water (8 ml) in a 25 ml Teflon-lined stainless steel reactor was heated from 298 to 393 K in 2 h and maintained at 393 K for 72 h. After the mixture was cooled to 298 K, blue crystals of the title compound were obtained.