Poly[[diaqua-μ6-succinato-di-μ5-succinato-didysprosium(III)] mono­hydrate]

Wei Xu; Hai-Sheng Chang; Xia-Xia Guo

doi:10.1107/S1600536811024330

. 2011 Jun 30;67(Pt 7):m998. doi: 10.1107/S1600536811024330

Poly[[diaqua-μ₆-succinato-di-μ₅-succinato-didysprosium(III)] monohydrate]

Wei Xu ^a,^*, Hai-Sheng Chang ^a, Xia-Xia Guo ^a

PMCID: PMC3152080 PMID: 21836969

Abstract

The title compound, {[Dy₂(C₄H₄O₄)₃(H₂O)₂]·H₂O}_n, is isostructural with other lanthanide succinates of the same formula. The Dy^III atom is nine-coordinated in a tricapped trigonal–prismatic environment by eight O atoms, derived from six carboxylate groups and a water molecule. One of the independent succinate anions is located about a crystallographic inversion center and the uncoordinated water molecule lies on a twofold axis. The crystal structure comprises edge-shared DyO₉ polyhedra linked by succinate bridges, forming a three-dimensional network architecture. Intra- and intermolecular O—H⋯O hydrogen bonds are present in the crystal structure.

Related literature

For related compounds, see: Perles et al. (2004 ▶); Serpaggi & Ferey (1999 ▶); He et al. (2007 ▶); Seguatni et al. (2004 ▶); Zhou et al. (2005 ▶); Cui et al. (2005 ▶); Yu et al. (2006 ▶); Li (2007 ▶).

Experimental

Crystal data

[Dy₂(C₄H₄O₄)₃(H₂O)₂]·H₂O
M _r = 727.26
Monoclinic,
a = 19.981 (4) Å
b = 7.7616 (16) Å
c = 13.868 (3) Å
β = 121.49 (3)°
V = 1834.0 (9) Å³
Z = 4
Mo Kα radiation
μ = 8.17 mm⁻¹
T = 293 K
0.45 × 0.20 × 0.14 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.154, T _max = 0.319
8691 measured reflections
2093 independent reflections
2016 reflections with I > 2σ(I)
R _int = 0.018

Refinement

R[F ² > 2σ(F ²)] = 0.016
wR(F ²) = 0.038
S = 1.09
2093 reflections
133 parameters
H-atom parameters constrained
Δρ_max = 0.78 e Å⁻³
Δρ_min = −0.73 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004 ▶); 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 datablock(s) global, I. DOI: 10.1107/S1600536811024330/vm2100sup1.cif

e-67-0m998-sup1.cif^{(16.7KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811024330/vm2100Isup2.hkl

e-67-0m998-Isup2.hkl^{(103KB, 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
O7—H7A⋯O3ⁱ	0.85	2.07	2.878 (3)	158
O7—H7B⋯O2ⁱⁱ	0.85	1.86	2.710 (3)	174
O8—H8W⋯O7	0.85	2.17	2.949 (4)	153

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

Acknowledgments

This project was supported by the Scientific Research Fund of Zhejiang Provincial Education Department (grant No. Y201017782). Thanks are also extended to the K. C. Wong Magna Fund of Ningbo University.

supplementary crystallographic information

Comment

There is considerable interest in the study of coordination frameworks with suitable rigid multidentate ligands. Especially those having long chain dicarboxylates present interesting behavior owing to their conformational flexibility and coordination diversity. Lanthanide ions exhibit high affinity for oxygen and diverse coordination modes. In an attempt to further understand the formation of lanthanide–organic framework materials, we present here the hydrothermal synthesis and crystal structure of a new Ln–succinate complex, (I).

The title compound, (I), is isostructural with the known Ln–succinate complexes where Ln = Y and La (Perles et al., 2004), Pr (Serpaggi & Ferey, 1999), Nd (He et al., 2007), Sm (Seguatni et al., 2004), Gd (Zhou et al., 2005), Tb (Cui et al., 2005), Ho (Yu et al., 2006), and Er (Li, 2007) analogs, but it represents the first reported succinate coordination polymer of dysprosium (III).

The asymmetric unit in (I) comprises a Dy atom, one and a half succinate anions, a coordinated water molecule and half an uncoordinated water molecule (Fig. 1). The complete second succinate dianion, containing O5 and O6, is generated from the half-ion by inversion and the uncoordinated water molecule O atom is located on a twofold axis. The Dy^III ion is nine-coordinated within a tricapped trigonal-prismatic geometry defined by eight O atoms, derived from six carboxylate anions, and a water molecule. The crystal structure comprises edge–sharing DyO₈(OH₂) polyhedra forming chains along the b–axis direction by sharing one edge with each neigboring polyhedron. The Dy···Dy distance within chains is 4.046 (1) Å. These chains are in turn linked via succinate bridges, forming a three-dimensional framework (Fig. 2.). Intra- and intermolecular O–H···O hydrogen bonds are present in the crystal structure (Table 1).

Experimental

A mixture of Dy(NO₃)₃.7H₂O (0.1316 g, 0.30 mmol), succinic acid (0.0354 g, 0.30 mmol), 1,10-phenanthroline (0.0595 g, 0.30 mmol), water (10 ml) was adjusted to a pH = 5.25 by NaOH solution. The mixture was sealed in a Teflon-lined stainless steel reactor and heated at 443 K for 3 d. After the reaction system had cooled slowly to room temperature, a small quantity of colourless crystals was isolated.