Poly[[tetra-μ3-acetato-hexa-μ2-acetato­diaqua-μ2-oxalato-tetra­lanthanum(III)] dihydrate]

Di, W.-J.; Lan, S.-M.; Zhang, Q.; Liang, Y.-X.

doi:10.1107/S1600536811038037

Volume 67
Part 10
Pages m1436-m1437
October 2011

Received 10 August 2011
Accepted 17 September 2011
Online 30 September 2011

Key indicators
Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.005 Å
R = 0.019
wR = 0.042
Data-to-parameter ratio = 14.0
Details

Poly[[tetra-₃-acetato-hexa-₂-acetatodiaqua-₂-oxalato-tetralanthanum(III)] dihydrate]

Wen-Jing Di,^a Shao-Min Lan,^a Qun Zhang ^a and Yun-Xiao Liang ^a ^*

^aState Key Lab. Base of Novel Functional Materials and Preparation Science, Faculty of Materials Science and Chemical Engineering, Ningbo University, Ningbo, Zhejiang, 315211, People's Republic of China
Correspondence e-mail: liangyunxiao@nbu.edu.cn

The title compound, {[La₄(CH₃CO₂)₁₀(C₂O₄)(H₂O)₂]·2H₂O}_n, exhibits a two-dimensional layered structure with the oxalate and acetate ligands acting as bridges. The asymmetric unit contains two crystallographically independent lanthanum(III) ions, half of an oxalate ligand, five acetate ligands, one coordinated water molecule and one uncoordinated water molecule. The coordination numbers of the two La ions are 9 and 10. Adjacent layers of the structure, which extend parallel to (100), are linked by O-HO hydrogen bonds and are also held together by van der Waals interactions between the CH₃ groups of the acetate anions.

Related literature

For properties of lanthanide compounds with metal-organic framework structures, see: Zhu et al. (2006); Deng et al. (2009); Bünzli & Piguet (2005); Zhang et al. (2008). For metal oxalates, see: Kustaryono et al. (2010); Roméro & Trombe (1999); Yu et al. (2006); Ohba et al. (1993). For lanthanide oxalates obtained from oxalate-containing starting materials, see: Zhang et al. (2009); Trombe et al. (2005). For lanthanide oxalates with oxalate formed in the course of the synthesis by decomposition of organic compounds or other unconventional reactions, see: Koner & Goldberg (2009); Li et al. (2003); Min & Lee (2002); Mohapatra et al. (2009). For oxidation of acetate to oxalate, see: Zielinski (1983). For La-O bond lengths, see: Trombe & Roméro (2000); Deng et al. (2009). For coordination modes of acetate groups, see: Zhang et al. (2009); Dan et al. (2006); Koner & Goldberg (2009); Mazurek et al. (1985).

Experimental

Crystal data

[La₄(C₂H₃O₂)₁₀(C₂O₄)(H₂O)₂]·2H₂O
M_r = 653.08
Monoclinic, P 2₁ /c
a = 9.4139 (19) Å
b = 13.310 (3) Å
c = 16.087 (3) Å
= 103.10 (3)°
V = 1963.2 (7) Å³
Z = 4
Mo K radiation
= 4.36 mm^-1
T = 295 K
0.19 × 0.18 × 0.18 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.454, T_max = 0.456
14917 measured reflections
3432 independent reflections
3185 reflections with I > 2(I)
R_int = 0.023

Refinement

R[F² > 2(F²)] = 0.019
wR(F²) = 0.042
S = 1.12
3432 reflections
245 parameters
H-atom parameters constrained
_max = 0.56 e Å^-3
_min = -0.40 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O13-H13AO14	0.82	1.84	2.654 (4)	176
O13-H13BO9ⁱ	0.82	2.01	2.831 (3)	176
O14-H14BO9ⁱⁱ	0.87	2.12	2.921 (4)	152.9
O14-H14AO5ⁱⁱⁱ	0.86	1.90	2.761 (4)	174.3
Symmetry codes: (i) -x+1, -y+2, -z+2; (ii) x-1, y, z; (iii) $[-x, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg & Putz, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: QK2021 ).

Acknowledgements

This work was supported by the Ningbo Natural Science Foundation (grant No. 2009 A610052) and the K. C. Wong Magna Fund in Ningbo University.

References

Brandenburg, K. & Putz, H. (2008). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bünzli, J.-C. G. & Piguet, C. (2005). Chem. Soc. Rev. 34, 1048-1077.
Dan, M., Cheetham, A. K. & Rao, C. N. R. (2006). Inorg. Chem. 45, 8227-8238.
Deng, H., Qiu, Y. C., Li, Y. H., Liu, Z. H. & Guillou, O. (2009). Inorg. Chim. Acta, 362, 1797-1804.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA.
Koner, R. & Goldberg, I. (2009). Acta Cryst. C65, m160-m164.
Kustaryono, D., Kerbellec, N., Calvez, G., Freslon, S., Daiguebonne, C. & Guillou, O. (2010). Cryst. Growth Des. 10, 775-781.
Li, X., Cao, R., Sun, D. F., Shi, Q., Bi, W. H. & Hong, M. C. (2003). Inorg. Chem. Commun. 6, 815-818.
Mazurek, W., Kennedy, B. J., Murray, K. S., O'connor, M. J., Rodgers, J. R., Snow, M. R., Wedd, A. G. & Zwack, P. R. (1985). Inorg. Chem. 24, 3258-3264.
Min, D. & Lee, S. W. (2002). Inorg. Chem. Commun. 5, 978-983.
Mohapatra, S., Vayasmudri, S., Mostafa, G. & Maji, T. K. (2009). J. Mol. Struct. 932, 123-128.
Ohba, M., Tamaki, H., Matsumoto, N. & Okawa, H. (1993). Inorg. Chem. 32, 5385-5390.
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC, The Woodlands, Texas, USA.
Roméro, S. & Trombe, J. C. (1999). Polyhedron, 18, 1653-1659.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Trombe, J. C., Jaud, J. & Galy, J. (2005). J. Solid State Chem. 178, 1094-1103.
Trombe, J. C. & Roméro, S. (2000). Solid State Sci. 2, 279-283.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
Yu, J. H., Hou, Q., Bi, M. H., Lü, Z. L., Zhang, X., Qu, X. J., Lu, J. & Xu, J. Q. (2006). J. Mol. Struct. 800, 69-73.
Zhang, X. J., Xing, Y. H., Han, J., Ge, M. F. & Niu, S. Y. (2008). Z. Anorg. Allg. Chem. 634, 1765-1769.
Zhang, X. J., Xing, Y. H., Wang, C. G., Han, J., Li, J., Ge, M. F., Zeng, X. Q. & Niu, S. Y. (2009). Inorg. Chim. Acta, 362, 1058-1064.
Zhu, W. H., Wang, Z. M. & Gao, S. (2006). Dalton Trans. pp. 765-768.
Zielinski, M. (1983). J. Radioanal. Chem., 80, 237-246.