Six new mononuclear [Fe III (L Br,Cl )X]-complexes (L Br,Cl is the dianionic penta-N 3 O 2 -dentate Schiff base ligand N,N'-bis(2'hydroxy-3-bromo-5-chlorobenzylidene)-1,6-diamino-3-azahexane; X: Cl À , N 3 À , NCO À , NCS À , NCSe À , CN À ) were synthesized and their structures, magnetic and electrochemical properties studied. Structure analysis and magnetic measurements showed that [Fe III (L Br,Cl )CN] is in the low spin state and the other five complexes are in high spin states. Furthermore, the trinuclear mixed valent cobalt complex {[Co III (L H,H )CN] 2 [Co II (1-methylimidazole) 3 (H 2 O)]} was prepared and its magnetic behavior studied.