Partial irreversible contraction of the framework during adsorption/desorption cycling can also be observed in ex situ PXRD experiments, conducted on the samples before and after the cycling experiments (see Figure ). The reflection intensities gradually decrease with increasing the chain length of the hydrocarbons, used in adsorption/desorption cycling experiments, although part of the sample still retain the crystallinity. This observation is well agreed with physisorption experiments indicating the reduced gas uptake and pristine shape of the isotherm.