This paper reports a new synthesis of polymers in which macrocyclic bis-l,3-diketones are attached to polystyrene and then complexed with transition metals. Preparation of 22- and 26-membered macrocyclic bis-l,3~diketones was performed by Fe(III)Cl3-induced ring expansion reaction of the corresponding tetrakis(trimethylsilyloxy)tricycloalkanes according to the procedure we reported previously. Treatment of the 22- and 26-membered macrocyclic bis- 1,3-diketones with chloromethylated polystyrene in dimethylformamide in the presence of sodium hydride produced polystyrene with macrocyclic bis-l,3-diketone as pendant groups. As expected, the polystyrene carrying macrocyclic bis-l,3-diketone rings was found to form metal chelated polymer when it was treated with transition metal salts such as copper, nickel, and cobalt. © 1979, Taylor & Francis Group, LLC. All rights reserved.