Na2[(VO)2(HPO4)2C2O4].2H2O: crystal structure determination from combined powder diffraction and solid-state NMR

J F Colin; T Bataille; S E Ashbrook; N Audebrand; L Le Pollès; J Y Pivan; E Le Fur

doi:10.1021/ic060483t

Na2[(VO)2(HPO4)2C2O4].2H2O: crystal structure determination from combined powder diffraction and solid-state NMR

Inorg Chem. 2006 Jul 24;45(15):6034-40. doi: 10.1021/ic060483t.

Authors

J F Colin¹, T Bataille, S E Ashbrook, N Audebrand, L Le Pollès, J Y Pivan, E Le Fur

Affiliation

¹ Sciences Chimiques de Rennes, UMR 6226, CNRS-Université de Rennes 1-ENSCR, 35042 Rennes Cedex, France.

PMID: 16842011
DOI: 10.1021/ic060483t

Abstract

The vanadyl oxalatophosphate Na2[(VO)2(HPO4)2C2O4].2H2O has been synthesized by hydrothermal treatment. Its structure has been determined and refined by combining X-ray powder diffraction and solid-state NMR techniques. It crystallizes with monoclinic symmetry in space group P2(1), a = 6.3534(1) A, b = 17.1614(3) A, c = 6.5632(1) A, beta = 106.597(1) degrees . The structure is related to that of (NH4)2[(VO)2(HPO4)2C2O4].5H2O, which was previously reported. The vanadium phosphate framework consists of infinite [(VO)(HPO4)] chains of corner-sharing vanadium octahedra and hydrogenophosphate tetrahedra. The oxalate groups ensure the connection between the chains to form a 2D structure. The sodium ions and the water molecules are located between the anionic [(VO)2(HPO4)2C2O4]2- layers. The thermal decomposition has been studied in situ by temperature-dependent X-ray diffraction and thermogravimetry. It takes place in three stages, where the first two correspond to water removal and the last to the decomposition of the oxalate group and water elimination, leading to the final product NaVOPO4.