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A novel vanadium polyoxometalate (POM)\u2010based material, Na\n                    <jats:sub>4<\/jats:sub>\n                    (H\n                    <jats:sub>2<\/jats:sub>\n                    O)\n                    <jats:sub>12<\/jats:sub>\n                    [(CH\n                    <jats:sub>2<\/jats:sub>\n                    OH)\n                    <jats:sub>3<\/jats:sub>\n                    CNH\n                    <jats:sub>3<\/jats:sub>\n                    ]\n                    <jats:sub>2<\/jats:sub>\n                    [V\n                    <jats:sub>10<\/jats:sub>\n                    O\n                    <jats:sub>28<\/jats:sub>\n                    ]\u00b74H\n                    <jats:sub>2<\/jats:sub>\n                    O (1) is presented, incorporating non\u2010innocent cations and whose electrocatalytic activity can be switched from the production of oxygen to hydrogen through its assembly on carbon nanotubes (CNT). A physical mixture (1\/CNT) shows remarkable oxygen evolution reaction (OER) activity, with an overpotential of 0.34\u00a0V at 10\u00a0mA\u00a0cm\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>2<\/jats:sup>\n                    , outperforming commercial IrO\n                    <jats:sub>2<\/jats:sub>\n                    (0.45\u00a0V) and approaching Ir\/C (0.31\u00a0V), with 80% Faradaic efficiency. In contrast, directed assembly (1@CNT) unlocks TRIS \u207a= [(CH\n                    <jats:sub>2<\/jats:sub>\n                    OH)\n                    <jats:sub>3<\/jats:sub>\n                    CNH\n                    <jats:sub>3<\/jats:sub>\n                    ]\u207a groups functionality, enabling high hydrogen evolution reaction (HER) efficiency, with an onset potential of \u22120.07\u00a0V, close to Pt\/C, and 94% Faradaic efficiency. Mechanistic studies, strongly supported by in\u2010operando confocal microscopy and theoretical calculations, reveal that the modulation of crystal interactions and the local microenvironment is key to orchestrating the OER\/HER tuning. OER is proposed to proceed via an alcohol oxidation reaction (AOR), while HER benefits from TRIS\u207a moieties acting as a \u201cproton sponge\u201d. This work provides a compelling approach for rational design of bifunctional molecular electrocatalysts based on earth\u2010abundant elements and controlled nanoassembly, with clear relevance for advancing green hydrogen production technologies.\n                  <\/jats:p>","DOI":"10.1002\/adma.202512902","type":"journal-article","created":{"date-parts":[[2025,11,26]],"date-time":"2025-11-26T12:40:29Z","timestamp":1764160829000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["POM\u2010Based Water Splitting Catalyst Under Acid Conditions Driven by Its Assembly on Carbon Nanotubes"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3386-8685","authenticated-orcid":false,"given":"Eugenia P.","family":"Quir\u00f3s\u2010D\u00edez","sequence":"first","affiliation":[{"name":"Centro Singular de Investigaci\u00f3n en Qu\u00edmica Biol\u00f3xica e Materiais Moleculares (CiQUS) Universidade de Santiago de Compostela  Santiago de Compostela 15782 Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0636-0448","authenticated-orcid":false,"given":"Melanie","family":"Guill\u00e9n\u2010Soler","sequence":"additional","affiliation":[{"name":"Centro Singular de Investigaci\u00f3n en Qu\u00edmica Biol\u00f3xica e Materiais Moleculares (CiQUS) Universidade de Santiago de Compostela  Santiago de Compostela 15782 Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0619-3822","authenticated-orcid":false,"given":"Carlos","family":"Herreros\u2010Lucas","sequence":"additional","affiliation":[{"name":"Centro Singular de Investigaci\u00f3n en Qu\u00edmica Biol\u00f3xica e Materiais Moleculares (CiQUS) Universidade de Santiago de Compostela  Santiago de Compostela 15782 Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5620-6129","authenticated-orcid":false,"given":"Alejandro","family":"L\u00f3pez\u2010Moreno","sequence":"additional","affiliation":[{"name":"Centro Singular de Investigaci\u00f3n en Qu\u00edmica Biol\u00f3xica e Materiais Moleculares (CiQUS) Universidade de Santiago de Compostela  Santiago de Compostela 15782 Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1839-0495","authenticated-orcid":false,"given":"Jos\u00e9 Manuel","family":"Vila\u2010Fungueiri\u00f1o","sequence":"additional","affiliation":[{"name":"Centro Singular de Investigaci\u00f3n en Qu\u00edmica Biol\u00f3xica e Materiais Moleculares (CiQUS) Universidade de Santiago de Compostela  Santiago de Compostela 15782 Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8203-3791","authenticated-orcid":false,"given":"Antonio Luis","family":"Llamas\u2010Saiz","sequence":"additional","affiliation":[{"name":"X\u2010Ray Unit \u00c1rea Infraestruturas Investigaci\u00f3n Universidade de Santiago de Compostela  Santiago de Compostela 15782 Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8733-9012","authenticated-orcid":false,"given":"Karol","family":"Struty\u0144ski","sequence":"additional","affiliation":[{"name":"CICECO\u2014Aveiro Institute of Materials Department of Chemistry University of Aveiro  Aveiro 3810\u2010193 Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1929-0477","authenticated-orcid":false,"given":"Manuel","family":"Melle\u2010Franco","sequence":"additional","affiliation":[{"name":"CICECO\u2014Aveiro Institute of Materials Department of Chemistry University of Aveiro  Aveiro 3810\u2010193 Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4644-2528","authenticated-orcid":false,"given":"Mar\u00eda del Carmen","family":"Gim\u00e9nez\u2010L\u00f3pez","sequence":"additional","affiliation":[{"name":"Centro Singular de Investigaci\u00f3n en Qu\u00edmica Biol\u00f3xica e Materiais Moleculares (CiQUS) Universidade de Santiago de Compostela  Santiago de Compostela 15782 Spain"}]}],"member":"311","published-online":{"date-parts":[[2025,11,26]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"crossref","first-page":"2785","DOI":"10.1002\/anie.201813895","volume":"58","author":"Ghosh T.","year":"2019","journal-title":"Angew. 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