The pore channels through the material are visible, with no-removable H 2 O molecules blocking the entrance of the pore (c.f. Figure ). Even after in vacuo activation at elevated temperatures, the H 2 O cannot be removed from the crystal structure, rendering the pore channels non-accessible for large molecules like N 2 , CO 2 and CH 4 which was confirmed through sorption experiments (see Figure and Thermogravimetric and differential scanning analysis (TGA and DSC) shows a small weight loss at around 100 °C, attributed to surface bond molecules, while the crystal water leaves the MOF from around 300 °C, followed by decomposition from 400 °C onward (see Figure ). This means that activation of the crystal happens already at 100 °C, but crystal water remains until decomposition. From TGA and DSC we find that the sample is free of the modulator, and also the XRD shows no additional reflections, giving a phase-pure MIL-116(Ga) pattern. Furthermore, via IR spectroscopy in Figure , guest free spectra are obtained, comparable to the reproduced, unmodulated MIL-116(Ga).