32) Watanabe, M.; Togo, M.; Sanui, K.; Ogata, N.; Kobayoshi, T.; (33) The numbers in parentheses represent standard deviations (34) Armand, M. B.; Duclot, M. J.; Rigaud, Ph. Solid State Zonics (29) Hartman, J. R.; Wolf, R. E.; Foxman, B. M.; Cooper, S. R. J. Am. Chem. SOC. 1983,105, 131-132. (30) Ashworth, R. S.; Prout, C. K.; Domenicano, A.; Vaciago, A.; J. Chem. SOC. A 1968, 93-104. (31) Domenicano, A.; Scaramuzza, L.; Vaciago, A.; Ashworth, R. S.; Ohtaki, Z. Macromolecules 1984,17, 2908-2912. determined from multiple experiments. Prout, C. K. J. Chem. SOC. A 1968, 866-869.ABSTRACT A series of poly(di-n-allcylsilanes) having hexyl, heptyl, and octyl side chains have been investigated by spectroscopic methods. Whereas the UV spectrum provided information about the electronic structure of the polymer backbone, IR and Raman methods have been used to characterize the molecular conformation of both the main and side chains. These structural studies were correlated with results from thermal analyses and X-ray diffraction measurements. A mechanism involving the melting of the n-alkyl side chains with a subsequent disordering of the polymer backbone is proposed.