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To reveal structure\u2013property relationships at the moiety level, we developed a combinatorial precursor design strategy to precisely synthesize eight precursor\u2010derived CDs with tailored organophosphorus moieties, including triphenylphosphonium and phenylphosphonic acid moieties, or their combination, within a shared polyacrylamide (PAM) backbone. The local organophosphorus microenvironment governs the FL properties of CDs. The sterically bulky triphenylphosphonium moieties rigidify the carbon framework to restrict intramolecular motions, thereby activating crosslink\u2010enhanced emission (CEE) and enhancing absolute quantum yield (QY) by 1.57\u2010fold. Conversely, electron\u2010withdrawing phenylphosphonic acid moieties introduce nonradiative electron trap states that attenuate emission intensity by 16.71%. Notably, phenylphosphonic acid and triphenylphosphonium moieties synergistically enhance the coordination affinity for copper(II) ions (\n                    <jats:italic>K<\/jats:italic>\n                    = 2.92 \u00d7 10\n                    <jats:sup>7<\/jats:sup>\n                    M\n                    <jats:sup>\u22121<\/jats:sup>\n                    ), arising from oxygen\u2010donor chelation and steric stabilization. This moiety\u2010level combinatorial precursor strategy enables the rational design of carbon nanostructures with precisely tailored FL and metal\u2010ion affinity capabilities.\n                  <\/jats:p>","DOI":"10.1002\/anie.1790590","type":"journal-article","created":{"date-parts":[[2026,8,25]],"date-time":"2026-08-25T11:24:11Z","timestamp":1787657051000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Organophosphorus Moieties Govern Opposite Fluorescence Modulation and Synergistically Enhance Copper(II) Affinity of Precursor\u2010Derived Carbon Dots"],"prefix":"10.1002","volume":"65","author":[{"given":"Xiangli","family":"Li","sequence":"first","affiliation":[{"name":"Institute for Advanced Ceramics State Key Laboratory of Urban\u2010rural Water Resource and Environment Harbin Institute of Technology  Harbin P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Galina S.","family":"Tsebrikova","sequence":"additional","affiliation":[{"name":"Frumkin Institute of Physical Chemistry and Electrochemistry Russian Academy of Sciences  Moscow Russia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Natalya S.","family":"Nikolaeva","sequence":"additional","affiliation":[{"name":"Federal Research Center for Problems of Chemical Physics and Medicinal Chemistry, Russian Academy of Sciences Institute of Physiologically Active Compounds  Chernogolovka Russia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mariya A.","family":"Lapshina","sequence":"additional","affiliation":[{"name":"Federal Research Center for Problems of Chemical Physics and Medicinal Chemistry, Russian Academy of Sciences Institute of Physiologically Active Compounds  Chernogolovka Russia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5956-2601","authenticated-orcid":false,"given":"Vladimir E.","family":"Baulin","sequence":"additional","affiliation":[{"name":"Frumkin Institute of Physical Chemistry and Electrochemistry Russian Academy of Sciences  Moscow Russia"},{"name":"Federal Research Center for Problems of Chemical Physics and Medicinal Chemistry, Russian Academy of Sciences Institute of Physiologically Active Compounds  Chernogolovka Russia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Aslan","family":"Yu Tsivadze","sequence":"additional","affiliation":[{"name":"Frumkin Institute of Physical Chemistry and Electrochemistry Russian Academy of Sciences  Moscow Russia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7714-4684","authenticated-orcid":false,"given":"Dechang","family":"Jia","sequence":"additional","affiliation":[{"name":"Institute for Advanced Ceramics State Key Laboratory of Urban\u2010rural Water Resource and Environment Harbin Institute of Technology  Harbin P. 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