abstract
A novel crystalline organic-inorganic hybrid oxovanadium(V) phosphate complex, {[V2O4(Phen)(2)(PO4)](2)VO(OH)}(3/4) {[V2O4(Phen)(2)(HPO4)](2)}(1/4) center dot 4.5H(2)O (where Phen = 1,10-phenanthroline), was isolated using the hydrothermal synthetic approach, and characterised structurally using thermal (TG and DSC) and CHN elemental analysis, vibrational spectroscopy (IR and Raman), single crystal X-ray diffraction and solid-state NMR. The structure contains two similar binuclear dioxovanadium(V) moieties, with all V5+ centres in a highly distorted octahedral coordination geometry. These are further bridged via a fifth V5+ centre, in a highly distorted tetrahedral coordination geometry, leading to the formation of a pentanuclear moiety. Individual complexes close-pack in the solid-state via offset pi-pi (between neighbouring phenanthroline residues) and hydrogen bonding interactions (with the water molecules of crystallisation). V-51 and P-31 solid-state NMR proved unequivocally the presence of these two coordination environments for the V5+ centres. (c) 2005 Elsevier B.V. All rights reserved.
keywords
COORDINATED ORGANONITROGEN LIGANDS; CAMBRIDGE STRUCTURAL DATABASE; HYDROTHERMAL SYNTHESIS; CRYSTAL-STRUCTURE; MAGNETIC-PROPERTIES; HYBRID MATERIALS; VANADIUM-OXIDE; PHEN; BOROPHOSPHATE; FRAGMENTS
subject category
Chemistry
authors
Mafra, L; Paz, FAA; Shi, FN; Fernandez, C; Trindade, T; Klinowski, J; Rocha, J
our authors
Fa-Nian Shi
Researcher
Filipe Alexandre Almeida Paz
Principal Researcher
João Rocha
Full Professor
Luís Mafra
Principal Researcher