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Alpha alumina (α‐Al2O3) are inert materials with outstanding thermal, chemical and mechanical stability. Herein, we fabricate porous single‐crystalline (PSC) α‐Al2O3 monoliths at centimeter scale to endow them with high catalytic activity while maintaining their stability. We reduce PSC α‐Al2O3 monoliths to create oxygen vacancies in lattice and stabilize them by the ordered lattice to construct unsaturated Al−O coordination structures for enhancing the catalytic activity. The generation of oxygen vacancy at 18e wyckoff position contributes to the unsaturated Al−O coordination. As a case study, we demonstrate the outstanding performance with conversion (≈34 %) and selectivity (≈95 %) toward non‐oxidative dehydrogenation of ethane to ethylene at 700 °C. We achieve the outstanding performance without obvious degradation even after a continuous operation over 1000 hours at 700 °C. [ABSTRACT FROM AUTHOR]

Hydrogen‐bonded organic frameworks (HOFs) are porous materials with great potential for biological applications. The self‐assembly of HOFs and biomacromolecules, however, is challenging. We report herein the self‐assembly of nanoscale HOFs (nHOFs) to encapsulate protein for intracellular biocatalysis. The self‐assembly of tetrakis(4‐amidiniumphenyl)methane and azobenzenedicarboxylate can encapsulate protein in situ to form protein@nHOFs under mild conditions. This strategy is applicable to proteins with different surface charge and molecular weight, showing a high protein encapsulation efficiency and minimal effect on protein activity. A cellular delivery study shows that the protein@TA‐HOFs can efficiently enter cells and retain enzyme activity for biochemical catalysis in living cells for neuroprotection. Our strategy paves new avenues for interfacing nHOFs with biological settings and sheds light on expanding nHOFs as a platform for biomacromolecule delivery and disease treatment. [ABSTRACT FROM AUTHOR]