Two new poly(p-phenylenevinylene) derivatives were prepared by Heck coupling. They contained alternating conjugated segments on the basis of p-distyryl-benzene and flexible nonconjugated spacers. The synthesized polymers P1 and P2 carried two m-terphenyl of four tertbutyl pendants, respectively, per repeat unit. Both polymers were amorphous and exhibited satisfactory thermal stability. Polymer P1 displayed a limited solubility in common organic solvents, whereas P2 dissolved readily in these solvents. The glass-transition temperature values were 128degreesC for PI and 37degreesC for P2. The polymers emitted blue or violet-blue light with photoluminescent maxima at about 445 and 460 nm for solutions and thin films, respectively. The bulky pendants reduced their tendency to form aggregates. (C) 2003 Wiley Periodicals, Inc.