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The active sites and the mechanism of this reaction remain controversial. This work is focused on the operando X\u2010ray absorption near edge structure spectroscopy analysis of conventional Mo\/ZSM\u20105 catalysts during their whole lifetime. Complemented by other characterization techniques, we derived spectroscopic descriptors of molybdenum precursor decomposition and its exchange with zeolite Br\u00f8nsted acid sites. We found that the reduction of Mo\u2010species proceeds in two steps and the active sites are of similar nature, regardless of the Mo content. Furthermore, the ZSM\u20105 unit cell contracts at the beginning of the reaction, which coincides with benzene formation and it is likely related to the formation of hydrocarbon pool intermediates. Finally, although reductive regeneration of used catalysts via methanation is less effective as compared to combustion of coke, it does not affect the structure of the catalysts.<\/jats:p>","DOI":"10.1002\/chem.202103894","type":"journal-article","created":{"date-parts":[[2021,11,25]],"date-time":"2021-11-25T11:45:35Z","timestamp":1637840735000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":23,"title":["Understanding the Preparation and Reactivity of Mo\/ZSM\u20105 Methane Dehydroaromatization Catalysts"],"prefix":"10.1002","volume":"28","author":[{"given":"Yujie","family":"Liu","sequence":"first","affiliation":[{"name":"Laboratory of Inorganic Materials &amp; Catalysis Department of Chemical Engineering and Chemistry Eindhoven University of Technology  P.O. 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