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However, the detailed mechanism insights into zeolite\u2010catalyzed reactions under microscale aqueous environment remain elusive. Here, using multiple dimensional solid\u2010state NMR experiments coupled with ultrahigh magic angle spinning technique and theoretical simulations, we establish a fundamental understanding of the role of water in benzene methylation over ZSM\u20105 zeolite under water vapor conditions. We show that water competes with benzene for the active sites of zeolite and facilitates the bimolecular reaction mechanism. The growth of water clusters induces a micro\u2010hydrophobic effect in zeolite pores, which reorients benzene molecules and drives their interactions with surface methoxy species (SMS) on zeolite. We identify the formation and evolution of active SMS\u2010Benzene complexes in a microscale aqueous environment and demonstrate that their accumulation in zeolite pores boosts benzene conversion and methylation.<\/jats:p>","DOI":"10.1002\/anie.202313974","type":"journal-article","created":{"date-parts":[[2023,11,7]],"date-time":"2023-11-07T14:06:51Z","timestamp":1699366011000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":19,"title":["Water\u2010Induced Micro\u2010Hydrophobic Effect Regulates Benzene Methylation in Zeolite"],"prefix":"10.1002","volume":"63","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-6079-2391","authenticated-orcid":false,"given":"Chao","family":"Wang","sequence":"first","affiliation":[{"name":"National Center for Magnetic Resonance in Wuhan State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics Wuhan Institute of Physics and Mathematics Innovation Academy for Precision Measurement Science and Technology Chinese Academy of Sciences  430071 Wuhan China"},{"name":"University of Chinese Academy of Sciences  100049 Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yueying","family":"Chu","sequence":"additional","affiliation":[{"name":"National Center for Magnetic Resonance in Wuhan State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics Wuhan Institute of Physics and Mathematics Innovation Academy for Precision Measurement Science and Technology Chinese Academy of Sciences  430071 Wuhan China"},{"name":"University of Chinese Academy of Sciences  100049 Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Danfeng","family":"Xiong","sequence":"additional","affiliation":[{"name":"Key Laboratory for Advanced Materials and Joint International Research Laboratory of Precision Chemistry and Molecular Engineering Feringa Nobel Prize Scientist Joint Research Center Research Institute of Industrial Catalysis and Centre for Computational Chemistry School of Chemistry and Molecular Engineering East China University of Science and Technology  200237 Shanghai China) + These authors contributed equally to this work."}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Haifeng","family":"Wang","sequence":"additional","affiliation":[{"name":"Key Laboratory for Advanced Materials and Joint International Research Laboratory of Precision Chemistry and Molecular Engineering Feringa Nobel Prize Scientist Joint Research Center Research Institute of Industrial Catalysis and Centre for Computational Chemistry School of Chemistry and Molecular Engineering East China University of Science and Technology  200237 Shanghai China) + These authors contributed equally to this work."}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Min","family":"Hu","sequence":"additional","affiliation":[{"name":"National Center for Magnetic Resonance in Wuhan State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics Wuhan Institute of Physics and Mathematics Innovation Academy for Precision Measurement Science and Technology Chinese Academy of Sciences  430071 Wuhan China"},{"name":"University of Chinese Academy of Sciences  100049 Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qiang","family":"Wang","sequence":"additional","affiliation":[{"name":"National Center for Magnetic Resonance in Wuhan State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics Wuhan Institute of Physics and Mathematics Innovation Academy for Precision Measurement Science and Technology Chinese Academy of Sciences  430071 Wuhan China"},{"name":"University of Chinese Academy of Sciences  100049 Beijing 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