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However, the active species in this reaction are highly complex, involving diverse Mo species, acidic sites of zeolite, and organic molecules. Herein, we apply 1D <jats:sup>95<\/jats:sup>Mo NMR and 2D <jats:sup>1<\/jats:sup>H\u2010<jats:sup>95<\/jats:sup>Mo heteronuclear correlation solid\u2010state NMR spectroscopy to directly observe the active ensembles in the confined channels of Mo\/ZSM\u20105 zeolite during the MDA reaction. We monitor the evolution of the spatial correlations of Mo species with the Br\u00f8nsted acid sites and organic products (olefins and aromatics) in the zeolite channels. We identified two kinds of MoO<jats:sub><jats:italic>x<\/jats:italic><\/jats:sub>C<jats:sub><jats:italic>y<\/jats:italic><\/jats:sub> species, with the more carbidic one (MoO<jats:sub><jats:italic>x<\/jats:italic><\/jats:sub>C<jats:sub><jats:italic>y<\/jats:italic><\/jats:sub>\u2010II) exhibiting higher activity for methane activation and benzene formation. The strong spatial interactions between the active Mo species and the organic species in the Mo\/ZSM\u20105 pores are related to the MDA activity.<\/jats:p>","DOI":"10.1002\/anie.202306133","type":"journal-article","created":{"date-parts":[[2023,6,1]],"date-time":"2023-06-01T16:29:43Z","timestamp":1685636983000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":18,"title":["Active Ensembles in Methane Dehydroaromatization over Molybdenum\/ZSM\u20105 Zeolite Identified by 2D <sup>1<\/sup>H\u2212<sup>95<\/sup>Mo Magic Angle Spinning Nuclear Magnetic Resonance Correlation Spectroscopy"],"prefix":"10.1002","volume":"62","author":[{"given":"Wei","family":"Gao","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  Wuhan 430071 P. R. China"},{"name":"University of Chinese Academy of Sciences  Beijing 100049 P. R. 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  Wuhan 430071 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guodong","family":"Qi","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  Wuhan 430071 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiawei","family":"Liang","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  Wuhan 430071 P. R. China"},{"name":"University of Chinese Academy of Sciences  Beijing 100049 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chao","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  Wuhan 430071 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2741-381X","authenticated-orcid":false,"given":"Jun","family":"Xu","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  Wuhan 430071 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Feng","family":"Deng","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  Wuhan 430071 P. R. 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