Abstract: | A novel metallocene catalyst was prepared from the reaction of (η3‐pentamethylcyclopentadienyl)dimethylaluminum (Cp*AlMe2) and titanium(IV) n‐butoxide Ti(OBu)4. The resulting titanocene Cp*Ti(OBu)3 was combined with methylaluminoxane (MAO)/tri‐iso‐butylaluminum (TIBA) to carry out the syndiotactic polymerization of styrene. The resulting syndiotactic polystyrene (sPS) possesses high syndiotacticity according to 13C NMR. Catalytic activity and the molecular weight of the resulting sPSs were discussed in terms of reaction temperature, concentration of MAO, amounts of scavenger TIBA added, and the hydrogen pressure applied during polymerization. |