X-ray pair distribution function (XPDF) measurements can acquire structural information on non-crystalline species and are particularly sensitive to heavier elements such as Zr and Hf due to their high electron density. In our previous work, we have shown that ex situ XPDF measurements are sensitive to the identity of the cluster in UiO family MOFs, and can clearly distinguish between isolated Zr atoms, Zr6 clusters, and Zr12 clusters. Ex situ XPDF measurements can detect and differentiate between tetramer and single cluster species in room temperature solutions related to UiO syntheses, and have successfully been used in situ to track the size of interlinked cluster aggregates forming MOF crystallites in solvothermal UiO-66 syntheses, as well as of metal oxido nanoclusters. However, until now, no study has been able to follow both the cluster formation and the coordination of the MOF framework in the same in situ reaction.