Poly[[μ3-3-(3-pyrid­yl)acrylato-κ3 N:O:O′][μ2-3-(3-pyrid­yl)acrylato-κ3 O,O′:O][μ2-3-(3-pyrid­yl)acrylato-κ2 O:O′)]gadolinium(III)]

Zhi-Hui Qiu; Fu-Pei Liang; Qing-Feng Ruan; Zi-Lu Chen

doi:10.1107/S1600536808012270

. 2008 May 3;64(Pt 6):m766–m767. doi: 10.1107/S1600536808012270

Poly[[μ₃-3-(3-pyridyl)acrylato-κ³ N:O:O′][μ₂-3-(3-pyridyl)acrylato-κ³ O,O′:O][μ₂-3-(3-pyridyl)acrylato-κ² O:O′)]gadolinium(III)]

Zhi-Hui Qiu ^a,^b, Fu-Pei Liang ^a,^*, Qing-Feng Ruan ^c, Zi-Lu Chen ^a

PMCID: PMC2961497 PMID: 21202459

Abstract

In the title compound, [Gd(C₈H₆NO₂)₃]_n, the Gd^III ion is in a bicapped trigonal prismatic coordination environment formed by seven O atoms and one N atom, derived from seven different 3-(3-pyridyl)acrylate (3-PYA) ligands. Gd^III ions are bridged by bidentate and tridentate 3-PYA ligands, resulting in a two-dimensional structure.

Related literature

For related literature, see: Ayyappan et al. (2001 ▶); Gunning & Cahill (2005 ▶); Zhang et al. (2000 ▶) Liu et al. (2006 ▶); Liu et al. (2004 ▶); Zhou et al. (2004 ▶); Li et al. (2007 ▶). For related structures, see: Zhou et al., (2003 ▶).

Experimental

Crystal data

[Gd(C₈H₆NO₂)₃]
M _r = 601.66
Monoclinic,
a = 7.7197 (17) Å
b = 25.646 (6) Å
c = 11.445 (2) Å
β = 95.684 (3)°
V = 2254.8 (8) Å³
Z = 4
Mo Kα radiation
μ = 2.99 mm⁻¹
T = 294 (2) K
0.24 × 0.20 × 0.18 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1998 ▶) T _min = 0.534, T _max = 0.615 (expected range = 0.507–0.584)
12572 measured reflections
4654 independent reflections
3517 reflections with I > 2σ(I)
R _int = 0.048

Refinement

R[F ² > 2σ(F ²)] = 0.037
wR(F ²) = 0.090
S = 1.05
4654 reflections
307 parameters
H-atom parameters constrained
Δρ_max = 2.06 e Å⁻³
Δρ_min = −1.17 e Å⁻³

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); 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 I, global. DOI: 10.1107/S1600536808012270/lh2617sup1.cif

e-64-0m766-sup1.cif^{(25.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808012270/lh2617Isup2.hkl

e-64-0m766-Isup2.hkl^{(228KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Gd1—O4ⁱ	2.305 (3)
Gd1—O2ⁱ	2.305 (3)
Gd1—O1	2.332 (3)
Gd1—O3	2.353 (3)
Gd1—O6ⁱⁱ	2.383 (3)
Gd1—O5	2.440 (3)
Gd1—O6	2.546 (3)
Gd1—N1ⁱⁱⁱ	2.628 (4)

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

Acknowledgments

This work was supported by the Natural Science Foundation of Guangxi (GKJ0639031), People’s Republic of China.

supplementary crystallographic information

Comment

The bifunctional compound 3-pyridylacrylic acid (3-HPYA) is a potential multidentate ligand, and several types of complexes formed with 3-HPYA have been studied (Ayyappan et al., 2001; Gunning & Cahill, 2005; Zhang et al., 2000). Until now, however, only a few crystallographic studies of 4f-block metal complexes of HPYA have been reported (Liu et al.,2006; Liu et al.,2004; Zhou et al.,2004; Zhou et al.,2003; Li et al., 2007).

Here, we report the synthesis and structure of the title complex, [Gd(TPA)₃]_n (I) (Fig.1). The Gd^III ion is eight-coordinated by seven O atoms and one N atom derived from seven different 3-PYA ligands. The topology of (I) is a two-dimensional structure mediated by bridging 3-PYA ligands. Symmetry-related Gd^III centres are bridged by two bidentate and two tridentate 3-PYA ligands, which results in the formation of a one-dimensional chain along a axis (Fig.2). Different chains are connected by tridentate 3-PYA ligands, which results in the formation of a two-dimensional framework parallel to (100) (Fig.3). Gd—O distances are in the range 2.305 (3) to 2.546 (3) Å, and the Gd—N distance is 2.628 (4) Å.

Experimental

A mixture of Gd₂O₃(0.5 mmol), 3-pyridylacrylic acid (2.0 mmol), H₂O(14 ml) was sealed in a 25 ml Teflon-lined stainless reactor and heated at 468 K for six days under autogenous pressure, then followed by slow cooling to room temperature, when a few colourless crystals were obtained. Analysis:found C 47.41,H 3.08,N 7.03%; C₂₄H₂₀GdN₃O₇ requires C 47.45,H 2.97,N 6.92%.