The syntheses and characterization of two new redox active cyclam ligands ferrocenylmethyl-(6-methyl-1,4,8,11-tetraazacyclotetradec-6-yl)-amine (L 3 ) and 1,1Ј-ferrocenylmethyl-bis(6-methyl-1,4,8,11-tetraazacyclotetradec-6-yl)-amine (L 4 ) are reported. The compounds each possess a ferrocenyl group bearing one (L 3 ) or two (L 4 ) appended macrocycles linked by their exocyclic amino groups and the crystal structures of both compounds have been determined. Anion binding of L 3 and L 4 was investigated by electrochemical titrations where H-bonding to each macrocycle causing a shift in the Fc ϩ/0 redox potential was used as a reporter of guest binding. The Zn II complex of L 3 has also been isolated and characterized structurally. These compounds were analysed for their capacity to electrochemically recognize anions in both aqueous and non-aqueous solution. We have found that L 3 , L 4 and [ZnL 3 ] 2ϩ sense Cl Ϫ and AcO Ϫ anions in MeCN-CH 2 Cl 2 , a function that is lost in aqueous solution.