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However, only 2, 3, and 6 connectivity of MCCOFs have been achieved in reported structures. Developing a higher connectivity remains a great challenge in the MCCOFs due to the difficulties in introducing multiple connecting nodes to the metal cluster. In this work, two 3D [8\u00a0+\u00a02]\u2010connected MCCOFs were synthesized by condensing an 8\u2010connectivity aluminum cluster\u2010based building block (termed Al\n                    <jats:sub>8<\/jats:sub>\n                    \u20108c) with linear dialdehyde linkers. Furthermore, these AlCCOFs showed efficient photocatalytic O\n                    <jats:sub>2<\/jats:sub>\n                    \u2010to\u2010H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    conversion due to the suitable energy band structure, efficient photoelectron conversion capability and the AlCCOF\u20101 showed H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    photosynthetic efficiency of 16794.69\u00a0\u00b5mol\u00a0g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    using water and benzyl alcohol reaction system. The in situ EPR, in situ FTIR, and DFT calculations were then performed to study the structure\u2010function relationships on the two AlCCOFs for H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    photosynthesis. This work is the first report of high\u2010connectivity MCCOFs bearing 8\u2010connected cluster units, showing the great potential of using metal clusters to construct complicate reticular frameworks by covalent linkage.\n                  <\/jats:p>","DOI":"10.1002\/anie.202507624","type":"journal-article","created":{"date-parts":[[2025,6,3]],"date-time":"2025-06-03T22:59:59Z","timestamp":1748991599000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":34,"title":["Reticular Synthesis of 3D Metal Cluster\u2010Based COFs With Record High\u2010Connectivity for Efficient Photocatalytic H\n                    <sub>2<\/sub>\n                    O\n                    <sub>2<\/sub>\n                    Synthesis"],"prefix":"10.1002","volume":"64","author":[{"given":"Mi","family":"Zhang","sequence":"first","affiliation":[{"name":"Guangdong Provincial Key Laboratory of Carbon Dioxide Resource Utilization School of Chemistry South China 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