Reaction of limonene(tricarbonyl)iron (1) with aryl-lithium reagents gave intermediate acylmetallates, from which, by subsequent alkylation with Et3OBF4 in aqueous solution at 0 °C, the novel complexes (η⁴-C10H16){C(OEt)C6H4Me-o}Fe(CO)2(4) and {(η³-C10H16)C(OEt)Ar}Fe(CO)2(2), Ar = Ph; (3), Ar =p-MeC6H4; (5); Ar =p-MeOC6H4; and (6), Ar =p-CF3C6H4 were obtained, the structures of (3) and (4) having been determined by X-ray crystallography.