Ex situ PXRD data were collected on Panalytical Aeris tabletop X-ray diffractometer, with CuK α radiation (40 kV, 7.5 mA) in Bragg-Brentano geometry, with the sample mounted on a zero background silicon plate. TGA and DSC experiments were performed by Simultaneous thermal analyzer (STA) 6000 (PerkinElmer, Inc.) in platinum crucibles at 5 • C min -1 heating rate under nitrogen gas purging at a flow of 20 mL min -1 . Rietveld refinement was performed in TOPAS. In situ synchrotron PXRD monitoring of grinding and wet/dry cycling. In Germany). A capillary of 0.5 mm width was filled with ca. 5 mg of D-U hyd sample and was heated using Oxford Cryostream system (operating in 100-500 K temperature range).