Reaction of [RhCl(NBD)](2) with 2.0 equiv of triphos (triphos = bis(2-diphe
nylphosphinoethyl)phenylphosphine; NBD = bicyclo[2.2.1]hepta-2,5-diene) in
THF solution at room temperature affords [Rh(NBD)(triphos)][Cl] (4a), which
was isolated as [Rh(NBD)(triphos)][SbF6] (4b) in 67% yield. Treatment of 4
b with aqueous formaldehyde in THF solution; at 80 degrees C forms [Rh(CO)(
triphos)][SbF6] (2a), which reversibly binds a second equivalent of CO(g) t
o give [Rh(CO)(2)(triphos)][SbF6] (2b). The complex [Rh(CO)(triphos)][SbF6]
has been found to be an effective aldehyde decarbonylation catalyst for pr
imary and aryl aldehydes at temperatures as low as that of refluxing dioxan
e, with little or no undesirable side products resulting from beta eliminat
ion or radical rearrangement.