Abstract Nylon 13,6 was successfully synthesized and its chemical composition, thermal properties, crystal structure, and moisture absorption characterized. Melting temperature and glass transition temperature were determined to be 206 °C and 60 °C, respectively, while the equilibrium melting temperature was determined to be 248 °C. Characterization of the crystallization kinetics showed that nylon 13,6 exhibits very fast crystallization compared to the industrially important nylons, nylon 6 and nylon 6,6. In addition, the moisture absorption of nylon 13,6 was dramatically lower than nylon 6 and nylon 6,6 which is consistent with the much lower amide content of nylon 13,6. The crystal structure was determined to be different from the expected γ-form, which possess a pseudohexagonal unit cell. Instead, the x-ray scattering pattern was more similar to the α-form. A similar result has been obtained for other odd–even nylons including nylon 5,6, nylon 5,10, nylon 9,2, nylon 11,10, and nylon 11,12.