The novel cyclometalated Rh(III) complex, [Rh(phpy-K-2 N, C-2 ')2(phen-dione)]PF6, where phpy-K-2 N, C-2 ' is pyridine-2-yl-2-phenyl and phen-dione is 1,10-phenanthroline-5,6-dione has been prepared and characterized by elemental analysis, IR, H-1 NMR, and electronic absorption spectroscopies, cyclic voltammetry, and X-ray crystallography. The crystal structure of [Rh(phpy-K-2 N C-2 ')2(phen-dione)]PF6 center dot CH3CN shows that the coordination geometry around the Rh(111) is a distorted octahedron, with bite angles of 76.13 degrees-81.09 degrees for all three bidentate ligands. (c) 2007 Elsevier B.V. All rights reserved.