Poly[diaqua(μ2-oxalato-κ4 O 1,O 2:O 1′,O 2′)(μ2-pyrazine-2-carboxyl­ato-κ3 N 1,O:O′)cerium(III)]

Yuanlan Wang; Chongchen Wang

doi:10.1107/S1600536808029164

. 2008 Sep 20;64(Pt 10):m1282–m1283. doi: 10.1107/S1600536808029164

Poly[diaqua(μ₂-oxalato-κ⁴ O ¹,O ²:O ^1′,O ^2′)(μ₂-pyrazine-2-carboxylato-κ³ N ¹,O:O′)cerium(III)]

Yuanlan Wang ^a, Chongchen Wang ^b,^*

PMCID: PMC2959293 PMID: 21201029

Abstract

In the hydrothermally synthesized title compound, [Ce(C₅H₃N₂O₂)(C₂O₄)(H₂O)₂]_n, the Ce^III ion is coordinated by four O atoms from two different oxalate ligands, three O atoms from two symmetry-related pyrazine-2-carboxylate ligands, two O atoms from two water melecules and one N atom from a pyrazine-2-carboxylate ligand in a distorted bicapped square-antiprismatic coordination geometry. The oxalate and pyrazine-2-carboxylate ligands bridge the Ce^III ions, forming a two-dimensional structure. In addition, intermolecular O—H⋯O and O—H⋯N hydrogen bonds connect the two-dimensional structure into a three-dimensional network.

Related literature

For background information, see: Eliseeva et al. (2004 ▶); Wang et al. (2007 ▶); Zou et al. (1999 ▶); Zheng et al. (2002 ▶).

Experimental

Crystal data

[Ce(C₅H₃N₂O₂)(C₂O₄)(H₂O)₂]
M _r = 387.27
Triclinic,
a = 8.0298 (7) Å
b = 8.7161 (9) Å
c = 8.8201 (9) Å
α = 115.514 (2)°
β = 101.747 (1)°
γ = 95.999 (1)°
V = 532.38 (9) Å³
Z = 2
Mo Kα radiation
μ = 4.31 mm⁻¹
T = 298 (2) K
0.24 × 0.15 × 0.10 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.424, T _max = 0.672
2790 measured reflections
1858 independent reflections
1760 reflections with I > 2σ(I)
R _int = 0.013

Refinement

R[F ² > 2σ(F ²)] = 0.019
wR(F ²) = 0.049
S = 1.09
1858 reflections
163 parameters
H-atom parameters constrained
Δρ_max = 0.68 e Å⁻³
Δρ_min = −0.94 e Å⁻³

Data collection: SMART (Bruker, 1996 ▶); cell refinement: SAINT (Bruker, 1996 ▶); data reduction: SAINT; 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/S1600536808029164/lh2687sup1.cif

e-64-m1282-sup1.cif^{(20.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808029164/lh2687Isup2.hkl

e-64-m1282-Isup2.hkl^{(91.5KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Ce1—O8	2.506 (2)
Ce1—O4ⁱ	2.521 (2)
Ce1—O5	2.530 (2)
Ce1—O3	2.538 (2)
Ce1—O6ⁱⁱ	2.540 (2)
Ce1—O1	2.578 (2)
Ce1—O7	2.595 (3)
Ce1—O1ⁱⁱⁱ	2.614 (2)
Ce1—N1	2.815 (3)
Ce1—O2ⁱⁱⁱ	2.897 (3)

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

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O5^iv	0.85	2.10	2.836 (4)	145
O7—H7B⋯O2^v	0.85	1.94	2.738 (4)	156
O8—H8A⋯N2^vi	0.85	1.96	2.799 (4)	169
O8—H8B⋯O3ⁱⁱⁱ	0.85	2.05	2.873 (3)	163

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Symmetry codes: (iii) Inline graphic ; (iv) ; (v) ; (vi) .

Acknowledgments

The authors gratefully acknowledge the financial support of the Research Fund of Beijing University of Civil Engineering and Architecture (grant No. 100700502) and the Funding Project for Academic Human Resources Development in Institutions of Higher Learning Under the Jurisdiction of Beijing Municipality (grant No. BJE10016200611).

supplementary crystallographic information

Comment

Rare metal coordination polymers of one-, two- and three-dimensional extended frameworks are an attractive research area because of the diverse structures available (Zheng, 2002; Eliseeva et al., 2004). Pyrazine-2,3-dicaboxylic acid is a good ligand with a versatitle coordination mode, which is widely used in self-assembled polymeric coordination synthesis (Zou et al., 1999; Wang et al., 2007). The title compound, [Ce(C₅H₃N₂O₂)(C₂O₄)(H₂O)₂]_n, was obtained unintentionally as the harvested product of the hydrothermal reaction of pyrazine-2,3-dicaboxylic acid and Ce₂(C₂O₄)₃.10H₂O. We report here the crystal structure of the title compound, a 2-D polymeric structure consisting of pyrazine-2-dicaboxylate and oxalate ligands.

The coordination environment of the Ce^III ion can be described as a distorted bicapped square-antiprism, in which the Ce^III ion is ten-coordinated by four oxygen atoms from two different oxalate ligands, three oxygen atoms from two different pyrazine -2-carboxylic acid ligands, two oxygen atoms from two water molecules, and one nitrogen atom from a pyrazine-2-carboxylate ligand, as shown in the Fig. 1. The oxalate ligands and pyrazine-2-carboxylate ligands bridge Ce^III ions to form a two-dimensional structure. The Ce—O bond lengths range from 2.506 (2) to 2.897 (3) Å. In the crystal structure, intermolecular O—H···O and O—H···N hydrogen bonds connect the two-dimensional structure into a three dimensional network.

Experimental

Colorless block-shaped crystals of the title compound were obtained by a hydrothermal reaction of Ce₂(C₂O₄)₃.10H₂O (0.10 mmol, 0.0710 g), pyrazine-2,3-dicarboxylic acid (0.10 mmol, 0.0168 g) and deionized water (15 ml) in a 23 ml teflon-lined reaction vesset at 423 K for 120 h followed by slow cooling to room temperature (yield 77% based on initial input of pyrazine-2,3-dicarboxylic acid).