A diacetylene, 6-(2-pyridyl)-3,5-hexadiyn-1-ol, is synthesized and crystallized. The crystals evaporated slowly from n-hexane/Et(2)O and n-hexane/CH2Cl2 formed a stiff frame. X-ray, UV-Vis, Raman and IR spectroscopic studies were utilized to determine the structure of the monomer crystals and the polymers formed on irradiation in aqueous solution.