A pentanuclear oxovanadium(V) phosphate complex with phenanthroline

作者：Mafra L; Paz FAA; Shi FN; Fernandez C; Trindade T; Klinowski J; Rocha J^*

来源：Inorganic Chemistry Communications, 2006, 9(1): 34-38.

DOI：10.1016/j.inoche.2005.09.036

• oxovanadium phosphate
• organic-inorganic hybrid
• hydrothermal synthesis
• V-51
• P-31
• solid-state NMR
• crystal structure

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.

• 出版日期2006-1