Protonation of Fe(CO)3NO−Na+ (I) or Fe(CO)2(NO)L−Na+ (VIII, L P(C6H5)3) with trifluoroacetic acid and excess L yields the new hydrido complex HFe(CO)(NO)L2 (V), which is reduced with sodium amalgam to yield the nucleophilic compound Fe(CO)(NO)L2−Na+ (IX) and converted back to VIII under CO. Protonation of V with HBF4 and excess L under CO yield the dicarbonyl cation (CO)2Fe(NO)L2+ BF4−.