Hydrothermal synthesis and structural characterization of the three-dimensional framework solids (NH4) [V2(OH) (PO4)2(H2O)] · H2O and Rb6[(Mo9V3O6) (PO4)10(H2PO4)3(OH) 9] · 8.5H2O

Victoria Soghomonian, Linda A. Meyer, Robert C. Haushalter, Jon Zubieta

Research output: Contribution to journalArticle

15 Scopus citations

Abstract

Hydrothermal synthesis has been employed to prepared two three-dimensional, open-framework solids with tetranuclear metal oxide cores. The reaction of VCl4, H3PO4, 1,3-diaminopropane and H2O in the mole ratio 1:7.4:8.6:1004 at 200°C for 87 h yielded (NH4) [V2(OH) (PO4)2(H2O)] · H2O (1·H2O), while the reaction of Rb2MoO4, Rb2V2O6, vanadium metal, U-Bu4NBr, H3PO4 and H2O in the mole ratio 2:1.1:1:1:145:392 at 240°C for 48 h produced Rb6[(Mo9V3O6)(PO4) 10(H2PO4)3(OH)9] · 8.5H2O (2·8.5H2O). The structure of 1·H2O is constructed from tetranuclear units of edge-and corner-sharing V (III) octahedra linked into a three-dimensional framework through phosphate tetrahedra. Compound 2·8.5H2O exhibits structurally distinct tetranuclear units of edge-and corner-sharing Mo(V) and Mo(III)/V(III) octahedra linked through phosphate tetrahedra into a open-framework solid with hexagonal channels. Both 1·H2O and 2·8.5H2O exhibit microporosity as evidenced by Type I water sorption isotherms. Crystal data: H8O12P2V2 (1·H2O), monoclinic P21/n, a=9.803(2), b=9.688(2), c=9.858(2) Å, β=102.91(3)°, V=912.6(3) Å3; structure solution and refinement converged at 0.0448 for 1481 reflections. H32O75.5P13V3Mo9Rb 6 (2·8.5H2O), hexagonal P63/m, a=16.563(2), c=12.534(3) Å, V=2977.8(7) Å3; R=0.0570 for 3022 reflections.

Original languageEnglish (US)
Pages (from-to)122-129
Number of pages8
JournalInorganica Chimica Acta
Volume275-276
DOIs
StatePublished - Jul 1 1998

Keywords

  • Crystal structures
  • Oxovanadium compounds
  • Phosphate compounds
  • Three-dimensional compounds

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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