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Herein, we report a pyrene\u2010based hydrogen\u2010bonded organic framework (Py\u2010HOF) that enables highly sensitive and selective dual\u2010mode (colorimetric and fluorometric) visual detection of Ce\n                    <jats:sup>4+<\/jats:sup>\n                    . The sensing mechanism exploits Ce\n                    <jats:sup>4+<\/jats:sup>\n                    as a potent one\u2010electron oxidant to trigger the formation of stable pyrene cation radicals (Py\u2022\n                    <jats:sup>+<\/jats:sup>\n                    ) within the structurally ordered HOF. Crucially, the rigid, columnar \u03c0\u2010stacked architecture of Py\u2010HOF effectively stabilizes the Py\u2022\n                    <jats:sup>+<\/jats:sup>\n                    species. The synergistic interplay between naked\u2010eye\u2010visible color change and fluorescence quenching enables a gradual transition from yellow to cyan under irradiation as the concentration of Ce\n                    <jats:sup>4+<\/jats:sup>\n                    increases (response time &lt; 8 s), significantly enhancing visual resolution. The process is chemically reversible with reductants like ascorbic acid (AA). Leveraging this mechanism, we fabricate a 3D\u2010printed portable sensor for smartphone\u2010assisted rapid quantification of Ce\n                    <jats:sup>4+<\/jats:sup>\n                    in real water samples with a linear range of 1\u201335 \u00b5M and a limit of detection (LOD) of 0.3 \u00b5M, and AA in commercial juices with a linear range of 2\u201322 \u00b5M and LOD of 0.6 \u00b5M. This work demonstrates the feasibility of radical\u2010based optoelectronic HOF materials as a dual\u2010mode platform for metal ion sensing.\n                  <\/jats:p>","DOI":"10.1002\/smll.74087","type":"journal-article","created":{"date-parts":[[2026,6,4]],"date-time":"2026-06-04T10:33:33Z","timestamp":1780569213000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Ce\n                    <sup>4+<\/sup>\n                    \u2010Triggered Stable Pyrene Radical Cation Formation in a Hydrogen\u2010Bonded Organic Framework Enabling on\u2010Site Dual\u2010Mode Sensing"],"prefix":"10.1002","author":[{"given":"Haibo","family":"Liang","sequence":"first","affiliation":[{"name":"School of Chemistry Sun Yat\u2010sen University  Guangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gan","family":"Luo","sequence":"additional","affiliation":[{"name":"School of Chemistry Sun Yat\u2010sen 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