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Published online by Cambridge University Press: 15 February 2011
Nanometer-sized metal particles have been prepared by chemical and photochemical reduction of homogeneous solutions of metal-organic rhodium(I) compounds. Reduction of [(COD)RhCl]2 with LiBEt3H in THF resulted in the formation of solutions containing crystalline, mono-dispersed Rh particles with average sizes of 2–4nm as determined by TEM and SAXS. The species [(COD)RhH]4 was isolated during the formation of the Rh colloids but was found not to be an intermediate in the reduction of Rh(I) to Rh(0). The catalytic activity of these highly dispersed metals towards pyrene hydrogenation has been investigated. Photochemical reduction of [(ethylene)2Rh(OEt)]2 at room temperature also resulted in formation of Rh as shown by TEM, EDS, ED and X-ray diffraction.