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In this work, we rationalize an amine\u2010mediated approach that combines a mild chemical pretreatment with pyrolysis to direct the transformation of a\n                    <jats:bold>PdIn\u2010MOF<\/jats:bold>\n                    precursor into dispersed PdIn intermetallic nanoparticles supported on N\u2010doped carbon. Advanced characterization techniques, including synchrotron ex situ and in situ X\u2010ray absorption spectroscopy (XAS) and X\u2010ray diffraction (XRD), demonstrate that the chemical pretreatment, involving in situ amine generation under reductive conditions, facilitates the early formation of Pd nanoparticles. This pre\u2010nucleation influences the kinetics of intermetallic phase formation during the subsequent pyrolysis, promoting a more regulated alloying process. Systematically varying nitro precursors and solvents shows that amine sterics and basicity govern nanoparticle size, phase development, PdIn ratio, nitrogen doping, and surface area. Finally, catalytic evaluation in alkyne semihydrogenation shows that the family of PdIn catalysts thus prepared achieves outstanding selectivity and high productivity, outperforming benchmarking Pd\/C and Lindlar catalysts across diverse substrates. Specifically, materials synthesized using ethanol and amines with low pKb values offer superior control over particle formation and catalytic behavior. Overall, these findings establish and explain a modular strategy for designing next\u2010generation bimetallic catalysts for selective hydrogenation applications via MOF\u2010derived syntheses.\n                  <\/jats:p>","DOI":"10.1002\/adma.202515111","type":"journal-article","created":{"date-parts":[[2025,11,21]],"date-time":"2025-11-21T07:07:16Z","timestamp":1763708836000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["In Situ Amine Formation to Modulate MOF\u2010Derived PdIn N\u2010Doped Carbon Catalysts"],"prefix":"10.1002","volume":"38","author":[{"given":"Gonzalo","family":"Egea","sequence":"first","affiliation":[{"name":"Instituto de Tecnolog\u00eda Qu\u00edmica Universitat Polit\u00e8cnica de Val\u00e8ncia\u2010Consejo Superior de Investigaciones Cient\u00edficas (UPV\u2010CSIC)  Avda. de los Naranjos s\/n Valencia 46022 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jordan","family":"Santiago Martinez","sequence":"additional","affiliation":[{"name":"Instituto de Tecnolog\u00eda Qu\u00edmica Universitat Polit\u00e8cnica de Val\u00e8ncia\u2010Consejo Superior de Investigaciones Cient\u00edficas (UPV\u2010CSIC)  Avda. de los Naranjos s\/n Valencia 46022 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"M. Asunci\u00f3n","family":"Molina","sequence":"additional","affiliation":[{"name":"Department of Chemistry University College London  20 Gordon Street London WC1H 0AJ UK"},{"name":"Research Complex at Harwell Rutherford Appleton Laboratories Harwell Science and Innovation Campus  Harwell Didcot OX11 0FA UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jaime","family":"Mazar\u00edo","sequence":"additional","affiliation":[{"name":"Instituto de Tecnolog\u00eda Qu\u00edmica Universitat Polit\u00e8cnica de Val\u00e8ncia\u2010Consejo Superior de Investigaciones Cient\u00edficas (UPV\u2010CSIC)  Avda. de los Naranjos s\/n Valencia 46022 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lucy","family":"Costley\u2010Wood","sequence":"additional","affiliation":[{"name":"ALBA Synchrotron Light Facility  Carrer de la Llum 2\u201026, Cerdanyola del Vall\u00e9s Barcelona 08290 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Christian","family":"Cerezo\u2010Navarrete","sequence":"additional","affiliation":[{"name":"Instituto de Tecnolog\u00eda Qu\u00edmica Universitat Polit\u00e8cnica de Val\u00e8ncia\u2010Consejo Superior de Investigaciones Cient\u00edficas (UPV\u2010CSIC)  Avda. de los Naranjos s\/n Valencia 46022 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Carlo","family":"Marini","sequence":"additional","affiliation":[{"name":"ALBA Synchrotron Light Facility  Carrer de la Llum 2\u201026, Cerdanyola del Vall\u00e9s Barcelona 08290 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Eduardo","family":"Villalobos\u2010Portillo","sequence":"additional","affiliation":[{"name":"ALBA Synchrotron Light Facility  Carrer de la Llum 2\u201026, Cerdanyola del Vall\u00e9s Barcelona 08290 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Andrew","family":"M. Beale","sequence":"additional","affiliation":[{"name":"Department of Chemistry University College London  20 Gordon Street London WC1H 0AJ UK"},{"name":"Research Complex at Harwell Rutherford Appleton Laboratories Harwell Science and Innovation Campus  Harwell Didcot OX11 0FA UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2341-7867","authenticated-orcid":false,"given":"Pascual","family":"O\u00f1a\u2010Burgos","sequence":"additional","affiliation":[{"name":"Instituto de Tecnolog\u00eda Qu\u00edmica Universitat Polit\u00e8cnica de Val\u00e8ncia\u2010Consejo Superior de Investigaciones Cient\u00edficas (UPV\u2010CSIC)  Avda. de los Naranjos s\/n Valencia 46022 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