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Addition of 2,2,6,6-tetramethylpiperidine-N-oxyl (TEMPO) to MCl₃ (M = Fe, Al) results in the formation of MCl₃(η¹-TEMPO) [M = Fe (1), Al (2)]. Both 1 and 2 oxidize alcohols to generate ketones or aldehydes along with the reduced complexes MCl₃(η¹-TEMPOH) [M = Fe (3), Al (4)]. Complexes 1–4 were fully characterized, including analysis by X-ray crystallography. Additionally, control experiments indicated that neither MCl₃ (M = Al, Fe) nor TEMPO are capable of effecting the oxidation of alcohols independently.