Poly(hexamethylene furanoate)-co-(dilinoleic furanoate) (PHF-DLF). The collected 1 H and C NMR spectra verified the chemical structure of copolyesters. Minor signals ascribed to the end-groups of α,ω-ALD appeared at the 3.68 -3.64 ppm region clearly indicating that enzymatic synthesis was successfully performed and products with relatively high molecular weight were formed. On the basis of the proton signal integration ratio of signals characteristic for hard and soft segments, it was possible to calculate the real segmental composition (see Supporting Information). Calculated values are close to those established theoretically which indicates good control over the process. However, as can be noticed from Table , the content of hard segments increases with an increasing number of carbon atoms within α,ω-ALD. Most probably this phenomenon is related to the fact that under applied vacuum and high reaction temperatures, some quantities of diols possessing lower boiling points were removed from the reaction mixture. Since the boiling point values increase with the increasing length of the diol chain, PDDF-DLF material possesses greater hard segment content in comparison to PHF-DLF copolyester (70.7 vs 67.5 wt%, respectively).