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Crystal defects are pivotal to boosting catalytic performance and an in‐depth understanding of the working mechanism of transition‐metal chalcogenides (TMDs), but their facile and controllable engineering are yet challenging. Herein, a new route is introduced to engineer defects on MoS2 via in situ intercalation during its hydrothermal preparation, accomplishing the efficient catalytic transfer hydrogenation (CTH) of nitroarenes. The combination of multiple structural characterizations demonstrates that the density of S defects can be tuned by the intercalation of ammonium and dimethylamine cations due to lattice strain/distortion and ligand substitution. As a proof of concept, the defect‐dependent catalytic performance is evidenced in the CTH of nitrobenzene with isopropanol, highlighting the significance of coordinatively unsaturated Mo sites in generating reactive chemisorbed H for subsequent hydrogenation. The good efficiency of defective MoS2 within a broad substrate scope further verifies the promise of the intercalation‐driven defect‐engineering strategy for designing TMDs‐based catalysts.
In situ intercalation of ammonium and dimethylamine cations is for the first time introduced to controllably engineer defects on MoS2 toward the efficient catalytic‐transfer‐hydrogenation of various nitroarenes. The enriched sulfur vacancies account for the promoted chemisorption of hydrogen donors that produces reactive *H for the facilitated hydrogenation kinetics.