Layered structures of hydrated vanadium oxides. Part 5.—Single-crystal structure of Rb0.5V2O5and phase changes of rubidium intercalate

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Abstract
Rb0.5V2O5, an anhydrous phase of the rubidium intercalate, has been synthesized in a hydrothermal VO(OH)2–RbCl system. It crystallizes in the monoclinic system C2/m: a= 11.596(2), b= 3.6908(9), c= 9.723(l)Å, β= 100.93(1)° and Z= 4. A single-crystal study (R/Rw= 0.069/0.079) revealed that the V2O5 layers are isostructural with those of K0.5V2O5 in Part 4 which consist of zigzag chains of edge-sharing VO6 octahedra. The interlayer Rb atom forms an RbO8 rectangular prism with the apical oxygens of the VO6 octahedra in contrast to the KO7 coordination in K0.5 V2O5˙Rb0.5V2O5 with 9.55 Å spacing was oxidized by hydrogen peroxide to a hydrated phase, Rb0.4V2O5˙0.8H2O with 10.85 Å spacing. This compound was reduced by rubidium iodide to a less hydrated phase, Rb0.4V2O5·0.5H2O with 10.41 Å spacing, rather than to Rb0.5V2O5. Interlayer sites for monovalent cations in anhydrous phases are suggested to be correlated with cationic sizes and contents.

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