In situ PXRD experiments on DUT-76(Cu) in parallel to adsorption and desorption of hydrocarbons at their boiling points were conducted according to previously published setup and procedure. A customized setup based on laboratory powder X-ray diffractometer Empyrean-2 (PANALYTICAL GmbH), equipped with a closed-cycle helium cryostat (ARS DE-102) and home-built X-ray transparent adsorption cell, connected to volumetric adsorption instrument BELSORP-max (Microtrac MRB) was used. The TTL trigger was used to establish the communication between BELSORP-max and Empyrean and ensure the measurement of the adsorption isotherm and PXRD pattern data collection in a fully automated mode in the predefined points of the isotherm. The parallel linear Cu Kα1 beam, obtained by using a hybrid 2xGe(220) monochromator, 4 mm mask, and primary divergence and secondary antiscatter slits with 1/4° opening, were used for data collection. A Pixcel-3D detector in 1D scanning mode (255 active channels) was used. The diffraction experiments were performed using ω-2θ scans in transmission geometry in the range of 2θ = 3-70°. SEM images of DUT-76(Cu) were taken with secondary electrons in a HITACHI SU8020 microscope using 1.0 kV acceleration voltage and 15.2-16.4 mm working distance. Sample preparation was performed in an argon atmosphere on an inert sample holder. As the sample showed degradation when being prepared directly on a sticky carbon pad powdered samples were prepared on a dry silicon wafer attached to a sample holder with a sticky carbon pad as a conductor.