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In this work, we report an atomically precise material model to address this challenge. The key to our solution is the rational incorporation of Fe species into polyoxotitanium cluster to form a heterometallic <jats:bold>Ti<jats:sub>4<\/jats:sub>Fe<jats:sub>1<\/jats:sub><\/jats:bold> cocrystal. This newly designed cocrystal cluster, which well governs the energy and charge transfer as evidenced by spectroscopic characterizations and theoretical calculations, enables the synergistic process involving C(sp<jats:sup>3<\/jats:sup>)\u2212H bond activation by photogenerated holes and further reactions by singlet oxygen (<jats:sup>1<\/jats:sup>O<jats:sub>2<\/jats:sub>). Remarkably, the cocrystal <jats:bold>Ti<jats:sub>4<\/jats:sub>Fe<jats:sub>1<\/jats:sub><\/jats:bold> cluster achieves efficient and selective oxidation of hydrocarbons (C<jats:sub>5<\/jats:sub> to C<jats:sub>16<\/jats:sub>) into aldehydes and ketones with a conversion rate up to 12\u2009860\u2005\u03bcmol\u2009g<jats:sup>\u22121<\/jats:sup>\u2009h<jats:sup>\u22121<\/jats:sup>, 5 times higher than that of Fe\u2010doped <jats:bold>Ti<jats:sub>3<\/jats:sub>Fe<jats:sub>1<\/jats:sub><\/jats:bold> cluster. This work provides insights into photocatalyst design at atomic level enabling synergistic catalysis.<\/jats:p>","DOI":"10.1002\/anie.202215540","type":"journal-article","created":{"date-parts":[[2022,10,31]],"date-time":"2022-10-31T13:57:31Z","timestamp":1667224651000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":56,"title":["Precisely Tailoring Heterometallic Polyoxotitanium Clusters for the Efficient and Selective Photocatalytic Oxidation of Hydrocarbons"],"prefix":"10.1002","volume":"61","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-6628-5190","authenticated-orcid":false,"given":"Mei\u2010Yan","family":"Gao","sequence":"first","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou 350002 Fujian P. R. 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