Abstract: | This work reports the preparation and characterization of the crystalline inclusion complex between polymeric guest, poly(neopentyl glycol) (PNPG), and small‐molecular host, β‐cyclodextrin (β‐CD). The crystalline inclusion complex was characterized with FTIR, TGA, X‐ray diffraction, 1H NMR and 13C CP/MAS NMR spectroscopes. It was found that the crystalline inclusion complex has higher temperature stability than the pure β‐CD. The X‐ray powder diffraction patterns of the crystalline inclusion complex proved that it has a columnar structure. 13C CP/MAS NMR spectra of the crystalline inclusion complex indicate that CDs adopt a more symmetrical conformation in the complex, while pure CD assume a less symmetrical conformation in the crystal without a guest inside its cavity. |