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Herein, we construct a compositionally tunable Ni\u2500Al catalyst system whose architecture evolves from conventional Ni\/Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    to inverse Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    \/Ni. This structural evolution gives rise to an unusual double\u2010volcano catalytic behavior in furfural reductive amination. Two activity maxima are identified over 30Ni\/Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    and inverse Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    \/90Ni, respectively, with the optimal Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    \/90Ni catalyst delivering 98.5% furfurylamine yield and a space\u2010time yield of 65\u00a0mmol g\n                    <jats:sub>cat<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00a0h\n                    <jats:sup>\u22121<\/jats:sup>\n                    under mild conditions. Adsorption studies, initial\u2010rate kinetic isotope effect and reaction\u2010order measurements, apparent activation\u2010energy analysis, and in situ infrared spectroscopy indicate that the double\u2010volcano behavior reflects the coupled evolution of catalyst composition and architecture and a composition\u2010dependent balance between Lewis\u2010acid\u2010assisted intermediate formation and hydrogen\u2010dependent intermediate conversion. Hydrogen\u2010dependent steps exert a stronger kinetic influence over 30Ni\/Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    than over Al\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    \/90Ni, while the inverse catalyst exhibits enhanced H\n                    <jats:sub>2<\/jats:sub>\n                    adsorption and activation and more rapid Schiff base conversion. These results indicate a shift in the dominant kinetic limitation between the two catalysts and provide a framework for designing efficient non\u2010noble\u2010metal catalysts for multifunctional cascade reactions involving coupled substrate and hydrogen activation.\n                  <\/jats:p>","DOI":"10.1002\/anie.2347270","type":"journal-article","created":{"date-parts":[[2026,10,13]],"date-time":"2026-10-13T05:47:27Z","timestamp":1791870447000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Double\u2010Volcano Catalytic Response in Furfural Reductive Amination Over Inverse Ni\u2500Al Catalysts"],"prefix":"10.1002","author":[{"given":"Jida","family":"Wang","sequence":"first","affiliation":[{"name":"School of Power and Mechanical Engineering Wuhan University  Wuhan China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuan","family":"Li","sequence":"additional","affiliation":[{"name":"School of Power and Mechanical Engineering Wuhan University  Wuhan China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ruoting","family":"Shan","sequence":"additional","affiliation":[{"name":"School of Power and Mechanical Engineering Wuhan University  Wuhan China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yupeng","family":"Lei","sequence":"additional","affiliation":[{"name":"School of Power and Mechanical Engineering Wuhan University  Wuhan China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junchen","family":"Xu","sequence":"additional","affiliation":[{"name":"School of Integrated Circuits Wuhan University  Wuhan China"},{"name":"The Institute of Technological Sciences Wuhan University  Wuhan China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7060-7532","authenticated-orcid":false,"given":"Yanfei","family":"Xu","sequence":"additional","affiliation":[{"name":"School of Power and 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