A novel partly substituted dithiocarboxyl β-cyclodextrin and its metal complexes (Cu 2 + , Co 2 + and Ni 2 + ) were synthesized and characterized by means of IR, UV, 1 H NMR, MS, electron spin resonance, cyclic voltammetry and transmission electron microscope. The results indicate that some hydroxyls of C2 of anhydroglucose unit have been modified by carbon disulphide and the functional β-cyclodextrin complexes show properties of both metal and cyclodextrin. The novel functional material made by the partly substituted β-cyclodextrin exhibits stable electrochemical activity and paramagnetism.