Thermal analysis (TGA) was carried out in Argon using a NETZSCH STA 409 thermal analyzer at a heating rate of 5 K•min -1 . The air sensitive MOF sample was prepared in an Ar-filled glovebox and inserted in the instrument with little exposure to ambient conditions. Total X-ray scattering data were collected at the Powder Diffraction and Total Scattering Beamline, P02.1, PETRA III, Deutsches Elektronen-Synchrotron (DESY). The X-ray wavelength was λ = 0.0207361 nm and the data were collected on a Varex XRD 4343CT (150×150 µm2 pixel size, 2880 x 2880 pixel area, CsI scintillator directly deposited on amorphous Si photodiodes). For calibration of the experimental geometry, LaB6 SRM 660c NIST powder was prepared in a soda lime glass capillary with an internal diameter of 0.8 mm. The pyFAI software was used for both calibration of the experimental geometry and for azimuthal integration. The sample-to-detector distance (SDD) was calibrated to be 300.613 mm. The area detector was placed such that the beam center was at the lower right corner of the area detector, when looking downstream from the sample position, resulting in quarter Debye-Scherrer rings collected on the detector. For the LaB6 SRM 660c NIST powder, total scattering data were collected for 300 s. The DUT-76(Cu) powder was prepared in a borosilicate capillary with an internal diameter of 0.5 mm and total scattering data were collected for 1500 s. The background contribution to the total scattering data were collected for 1500 s for an empty borosilicate capillary with an internal diameter of 0.5 mm. To take X-ray intensity fluctuations during data acquisition into account, the background data were scaled prior to subtraction from the DUT-76(Cu) data. To obtain the reduced atomic pair distribution function (PDF), the PDFgetX3 algorithm was used through the xPDFsuite software. The maximum value of momentum transfer for complete quarter rings on the area detector was Qmax,inst = 27.7 Å -1 . However, to improve the signal-to-noise ratio of the resulting PDF, the Fourier transformation was terminated at a value of Qmax = 17.9 Å -1 , reflecting the poor counting statistics at higher Q-values due to limited signal of interest from the sample.