A novel metallobridged bis(b-cyclodextrin)s 2[bis(b-CD)s 2] was synthesized and characterized by means of 1 H NMR, IR, element analysis and redox iodometric titration. The fluorescence of metallobridged bis(b-CD)s 2 was weak compared with bis(b-CD)s 1because of the paramagnetism of copper (II) ions.