Poly-(2,4-hexadiyn-1,6-diol) (PHDO), prepared by NbCl5/(n-Bu)(4)Sn catalyzed metathesis of HDO, was pyrolyzed at various temperatures and electrical and structural properties of resulting polymers were investigated by FT-IR, Laser Raman, CP/MAS C-13-NMR and Xray diffraction methods. The polymer obtained by pyrolysis of PHDO at 800 degrees C showed a conductivity of about 10 S/cm at room temperature. The structure of the polymer seems to be a graphite-like crystal consisting of condensed aromatic layers. (C) 1994 John Wiley & Sons, Inc.