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The \u201cshape complementary assembly\u201d (SCA) strategy allows for exclusive formation of the\n                    <jats:italic>cis<\/jats:italic>\n                    \u2010[Pd\n                    <jats:sub>2<\/jats:sub>\n                    <jats:bold>D<\/jats:bold>\n                    <jats:sub>2<\/jats:sub>\n                    <jats:bold>A<\/jats:bold>\n                    <jats:sub>2<\/jats:sub>\n                    ]\n                    <jats:sup>4+<\/jats:sup>\n                    cage isomer. Compared to previously reported statistical\n                    <jats:bold>DA<\/jats:bold>\n                    assemblies, lacking stoichiometry and stereo control, the number of possible electron transfer routes was reduced. This enables a better understanding and tunability of the excited state dynamics. Cage assembly was investigated by NMR, MS, and single crystal X\u2010ray diffraction analysis. Steady\u2010state absorption and electrochemical properties indicate that donor and acceptor moieties remain largely independent in the electronic ground state. Femtosecond pump\u2010probe spectroscopy in the visible and infrared was applied to compare the fate of photoexcited states for pure ligands, donor\u2010 and acceptor\u2010only assemblies, and the donor\u2013acceptor heteroleptic cages. For the latter, ultrafast intracage ligand\u2010to\u2010ligand charge separation is followed by two back electron transfer pathways, occurring on timescales of hundreds of picoseconds and around one nanosecond, assignable to\n                    <jats:bold>D<\/jats:bold>\n                    \/\n                    <jats:bold>A<\/jats:bold>\n                    ligands facing each other in\n                    <jats:italic>cis<\/jats:italic>\n                    \u2010 or\n                    <jats:italic>trans<\/jats:italic>\n                    \u2010position. Our work shows that non\u2010statistical modular self\u2010assembly can be used for the precise positioning of photoredox\u2010active components in defined distances on the nanoscale.\n                  <\/jats:p>","DOI":"10.1002\/anie.202522944","type":"journal-article","created":{"date-parts":[[2026,1,9]],"date-time":"2026-01-09T09:43:00Z","timestamp":1767951780000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Non\u2010Statistical Assembly of Donor\u2013Acceptor Cages for Light\u2010Induced Charge Separation"],"prefix":"10.1002","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1540-4900","authenticated-orcid":false,"given":"Jacopo","family":"Tessarolo","sequence":"first","affiliation":[{"name":"Department of Chemistry and Chemical Biology TU Dortmund University  Otto\u2010Hahn Stra\u00dfe 6 44227 Dortmund Germany"},{"name":"Department of Chemistry Chonnam National University  77 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