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Such designs address critical limitations inherent in traditional 2D covalent organic frameworks (2D COFs), including obscure active sites, constrained interlayer charge transport, and suboptimal exciton utilization. This work reports the synthesis of a 3D COF (PhFOONi\u2010COF) featuring a helical\u2010staggered interlayer\u2010connected topology, achieved through sequential covalent assembly and precise nickel anchoring. The resulting hybrid bonding setup naturally creates continuous pathways for charge transfer and spatially open catalytic sites, thus efficiently balancing the activity\u2010selectivity dilemma in photocatalytic H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production. The integrated framework, featuring nitrogen\u2010engineered fluorenone units coordinated with Ni centers, exhibits exceptional photocatalytic performance with a H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production rate of 9.73\u00a0mmol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00a0h\n                    <jats:sup>\u22121<\/jats:sup>\n                    under visible light, which is 15 times that of its purely covalent counterpart. Advanced in situ investigations and density functional theory calculations systematically reveal that the integrated covalent\u2010coordination structure facilitates dual functionality: the Ni\u2010N4 sites geometrically confine O\n                    <jats:sub>2<\/jats:sub>\n                    molecules in optimal adsorption configurations, and the conjugated fluorenone skeleton enables directional electron funneling to catalytic centers through orbital hybridization. This work pioneers a paradigm\u2010shifting strategy for designing multifunctional photocatalytic platforms through atomic\u2010level integration of covalent and coordination networks.\n                  <\/jats:p>","DOI":"10.1002\/anie.202515814","type":"journal-article","created":{"date-parts":[[2026,3,28]],"date-time":"2026-03-28T09:17:32Z","timestamp":1774689452000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Nickel Single Atoms Reconfigured 3D COFs Boost H\n                    <sub>2<\/sub>\n                    O\n                    <sub>2<\/sub>\n                    Photosynthesis"],"prefix":"10.1002","volume":"65","author":[{"given":"Lei","family":"Hao","sequence":"first","affiliation":[{"name":"Key Laboratory for Biobased Materials and Energy of Ministry of Education, College of Materials and Chemical Engineering South China Agricultural University Guangzhou P.R. 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