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Metal–organic frameworks (MOFs) are periodic organic–inorganic materials that have garnered considerable attention for electrocatalytic applications due to their wide tunability. Metal-hydroxide organic frameworks (MHOFs), a subset of MOFs that combine layered metal hydroxides with organic ligands of various π–π stacking energy, have shown promising catalytic functions, such as for the oxygen evolution reaction (OER). The long-term electrochemical stability of these materials for the OER is unfortunately not well understood, which is critical to design practical devices. In this study, we investigated how Ni-based MHOFs composed of two linkers with different π–π interaction strength (terephthalate; L1 and azobenzene-4,4′-dicarboxylate; L4) change as a function of cycle number and potential for the OER. All MHOFs tested showed significant increases in the number of electrochemically active Ni sites and …