Studies of the oxovanadium(IV)-oxalate system: Syntheses and crystal structures of binuclear (Ph4P)2[(VO)2(H2O) 2(C2O4)3]·4H2O and of the one-dimensional chain material, (Ph4P) [VOCl(C2O4)]

José Salta, Charles J. O'Connor, Sichu Li, Jon Zubieta

Research output: Contribution to journalArticle

26 Scopus citations

Abstract

The hydrothermal reactions of (Ph4P)[VO2Cl2] and H2C2O4 at 150 and 125 °C yield (Ph4P)2[V2O2(H2O) 2(C2O4)3]·4H2O (1) and (Ph4P) [VOCl(C2O4)] (2), respectively. The structure of the molecular anion of 1 consists of a binuclear unit of oxovanadium(IV) octahedra bridged by a bisbidentate oxalate group. The {VO6} coordination geometry at each vanadium site is defined by a terminal oxo group, an aquo ligand, and four oxygen donors - two from the bisbidentate bridging oxalate and two from the terminal bidentate oxalate. The structure of 2 consists of discrete Ph4P+ cations occupying regions between {[VOCl(C2O4)]-} spiral chains. The structure of the one-dimensional anionic chain exhibits V(IV) octahedra bridged by bisbidentate oxalate groups. Crystal data: 1·4H2O, monoclinic P21/n, a=12.694(3), b=12.531 (3), c=17.17(3) Å, β=106.32(2)°, V=2621.3(13) Å3,Z=2,Dcalc=1.501 g cm-3, structure solution and refinement converged at a conventional residual of 0.0518; 2, tetragonal P43, a=12.145(2), c=15.991(3) Å, V=2358.7(12) Å3, Z=4, R=0.0452.

Original languageEnglish (US)
Pages (from-to)303-310
Number of pages8
JournalInorganica Chimica Acta
Volume250
Issue number1-2 PART I
DOIs
StatePublished - Sep 1996

Keywords

  • Crystal structures
  • Hydrothermal synthesis
  • One-dimensional chain complexes
  • Oxalate complexes
  • Oxovanadium complexes

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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