Monomeric fluoroalkoxyalkyl(phenyl)dichlorosilanes were synthesized with quantitative yields by hydrosilylation of allyl ethers of fluoroalcohols with phenyldichlorosilane with Pt(Ph3Sb)(2)Cl-2 complex as a catalyst. Starting from these monomers, corresponding polysilanes with weight-average molecular weights of 2-3 x 10(4) were obtained by the Wurtz reaction. Increasing the CF2 groups containing two to six monomer units caused the char yields to increase from 3 to 48% at 800 degreesC in air. The emission characteristics of these polysilanes in a chloroform solution were examined. They had a narrow peak at 344 nm with a small Stokes shift (approximate to20 nm). (C) 2003 Wiley Periodicals, Inc.