Metal-organic frameworks (MOFs) are representative robust and porous crystalline materials consisting of metal and organic linkers. With their interesting properties, MOFs are explored for gas separation, adsorption and catalysis. Various post-synthetic modification (PSM) strategies have been reported to modify the intrinsic properties of MOFs and to enhance the performance in applications. Typically, modification of the organic ligands is the first option for PSM, followed by the exchange of the metal ions. Herein, a new type of click reaction, sulfur(VI) fluoride exchange (SuFEx),¹ has been utilized to prepare two post-synthetic modified (PSM) UiO-67 series, whose single-crystal-to-crystal transformations of the click reaction were confirmed by X-ray single crystal analysis. This SuFEx method will provide versatile tools for introducing new functionality inside MOFs