The present invention relates to a novel crystalline form of ingenol mebutate methods of preparation thereof and to its use. More specifically the invention relates to the conversion of amorphous ingenol mebutate (ingenol-3-angelate PEP005) to a crystalline form which was characterized by single crystal X-Ray crystallography (XRC) attenuated total reflectance Fourier transform infrared (FTIR-ATR) spectroscopy and Differential Scanning Calorimetry (DSC).
