Wilkinson's catalyst, RhCl(PPh<sub>3</sub>)<sub>3</sub> is a well known and widely used homogeneous hydrogenation catalyst. This catalyst was analyzed by ESCA which revealed that two rhodium species [Rh(I) and Rh(III)] were present, both for commercial preparations and for catalysts prepared in this laboratory. The ratio of Rh(I) to Rh(III) was 3:2 regardless of the source. A different method of synthesizing RhCl(PPh<sub>3</sub>)<sub>3</sub> Wag used and produced a compound having only Rh(I) species. Additional analytical techniques such as elemental analysis, FT-IR, liquid chromatography, and <sup>31</sup>P NMR were used to determine the origin of the higher binding energy peaks when Wilkinson's procedure was used to prepare RhCl(PPh<sub>3</sub>)<sub>3</sub>. Hydrogenation of cyclohexene was also performed to determine the effect of the higher binding energy species on catalytic activity.
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