The structural transformations and guest dynamics of methanol-loaded beta-form hydroquinone (HQ) clathrate were investigated using temperature-dependent Raman spectroscopy. Methanol-loaded beta-form HQ clathrate was obtained by recrystallization and characterized by elemental analysis, synchrotron X-ray diffraction, solid-state C-13 NMR spectroscopy, and Raman spectroscopy. Temperature-dependent Raman spectra of methanol-loaded beta-form. HQ clathrate were measured in the temperature range 300-412 K at increments of 4 K. Although no significant changes were evident in the temperature range 300-376 K, abrupt changes in the relative intensity and shape of the Raman bands were observed between 380 and 412 K indicating the structural transition from methanol-loaded beta-form HQ clathrate to pure alpha-form HQ Methanol molecules were gradually released from the beta-form HQ clathrate in the range 364-380 K. Upon returning to ambient conditions, the crystal structure of the HQ sample remained identical to that of pure alpha-form HQ Therefore, the temperature-induced structural transition of methanol-loaded HQ clathrate is completely irreversible and alpha-form HQ is more stable at ambient conditions.