Traditional design strategies for porous coordination polymers and Metal-Organic Frameworks (MOFs) frequently rely on de novo solvothermal crystallization to dictate framework topology and pore function. While post-synthetic modification (PSM) offers a powerful alternative for introducing functional groups inaccessible via direct synthesis, its utility is heavily limited by size-exclusion barriers that restrict reactant guests from traversing the internal channel networks. Applying applied hydrostatic pressure offers a clean, solid-state vector to mechanically overcome these steric limitations, driving unique guest encapsulation and framework reactivity [1].
Here, we present the high-pressure post-synthetic ligand exchange of a flexible, scandium-based wine-rack framework, MIL-53(Sc)-edb (GUF-1), tracked in situ using synchrotron single-crystal X-ray diffraction inside a diamond anvil cell [2]. When compressed in a methanol (MeOH) pressure-transmitting medium, the framework undergoes a crystalline single-crystal-to-single-crystal transformation. At a critical pressure of 0.71 GPa, pressure-induced entry of MeOH into the channel voids triggers a partial ligand exchange. This process replaces the bridging hydroxide groups residing at the axial coordination sites of the tetranuclear Sc(IV) paddlewheel units with bridging methoxide groups.
Intriguingly, this post-synthetic ligand exchange prompts a sudden, disproportionate closing hinge motion of the wine-rack matrix. This mechanical distortion is stabilized by the introduction of four symmetrical, intra-framework CH-pi interactions between the newly grafted methyl groups and the ethynylenedibenzoate linkers, effectively "pulling" the pore walls together. The result is a transformation from the native, solvent-accessible hydrophilic channels to volume-restricted rectangular channels featuring a highly hydrophobic surface. This work provides a rare demonstration of pressure-dependent, reversible solid-state reactivity within a flexible matrix, highlighting the vast potential of using mechanical stress to tune non-covalent interactions and local coordination spheres in advanced stimuli-responsive materials.