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Herein, we demonstrate that tailoring the polymer skeleton from poly(diethynylthieno[3,2\u2010b]thiophene) (<jats:bold>pDET<\/jats:bold>) to poly(2,6\u2010diethynylbenzo[1,2\u2010b:4,5\u2010b\u2032]dithiophene (<jats:bold>pBDT<\/jats:bold>) and poly(diethynyldithieno[3,2\u2010b:2\u2032,3\u2032\u2010d]thiophene) (<jats:bold>pDTT<\/jats:bold>) in conjugated acetylenic polymers (CAPs) introduces highly efficient active sites for water dissociation. As a result, <jats:bold>pDTT<\/jats:bold> and <jats:bold>pBDT<\/jats:bold>, grown on Cu substrate, demonstrate benchmark photocurrent densities of 170\u2005\u03bcA\u2009cm<jats:sup>\u22122<\/jats:sup> and 120\u2005\u03bcA\u2009cm<jats:sup>\u22122<\/jats:sup> (at 0.3\u2005V vs. RHE; pH\u200513), which are 4.2 and 3\u2005times higher than that of <jats:bold>pDET<\/jats:bold>, respectively. Moreover, by combining DFT calculations and electrochemical operando resonance Raman spectroscopy, we propose that the electron\u2010enriched C<jats:sub>\u03b2<\/jats:sub> of the outer thiophene rings of <jats:bold>pDTT<\/jats:bold> are the water dissociation active sites, while the \u2212C\u2261C\u2212 bonds function as the active sites for hydrogen evolution.<\/jats:p>","DOI":"10.1002\/anie.202104469","type":"journal-article","created":{"date-parts":[[2021,6,25]],"date-time":"2021-06-25T09:46:01Z","timestamp":1624614361000},"page":"18876-18881","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":38,"title":["Thiophene\u2010Based Conjugated Acetylenic Polymers with Dual Active Sites for Efficient Co\u2010Catalyst\u2010Free Photoelectrochemical Water Reduction in Alkaline Medium"],"prefix":"10.1002","volume":"60","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-0899-9288","authenticated-orcid":false,"given":"Mino","family":"Borrelli","sequence":"first","affiliation":[{"name":"Center for Advancing Electronics Dresden (cfaed) and Department of Chemistry and Food Chemistry Dresden University of Technology  Mommsenstrasse 4 01062 Dresden Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Christine Joy","family":"Querebillo","sequence":"additional","affiliation":[{"name":"Chair of Electrochemistry Department of Chemistry and Food Chemistry Dresden University of Technology  Zellescher 19 01062 Dresden Germany"},{"name":"Institute for Complex Materials Leibniz-Institute for Solid State and Materials Research (IFW)  Helmholtzstrasse, 20 01069 Dresden Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Dominik L.","family":"Pastoetter","sequence":"additional","affiliation":[{"name":"Center for Advancing Electronics 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