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By drawing inspiration from inorganic metastable systems, we propose a strategy to fabricate organic metastable materials to address this critical challenge. By integrating supersaturated ionic liquids into a polymeric architecture, RTP hydrogels are obtained under transient stimulus, without requiring persistent stimulation. The soft hydrogels switch to a tough crystallized state via in situ stacking of ionic\u2010liquid crystals. A 10 fold enhancement in toughness and a 34 fold increase in phosphorescence lifetime are achieved, compared to their metastable counterparts. The mechanical reinforcement stems from confined segments and entangled chains caused by in situ stacked ionic\u2010liquid crystals, while the intertwinement of polymer chains further promotes the denser stacking of ionic\u2010liquid crystals to produce long\u2010lived RTP. Leveraging the advantage of 2D correlation spectroscopy in elucidating dynamic mechanisms, we map the microscopic response order of different groups in the crystallization process of ionic liquids and reveal the aforementioned mechanism at the atomic level. This work not only provides a design paradigm for addressing the challenge of transient response in existing stimuli\u2010responsive RTP materials but also charts a route for developing organic metastable materials to unlock unprecedented functionality.<\/jats:p>","DOI":"10.1002\/adma.72626","type":"journal-article","created":{"date-parts":[[2026,2,20]],"date-time":"2026-02-20T14:24:38Z","timestamp":1771597478000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["Organic Metastable Hydrogels via In Situ Ionic\u2010Liquid Crystal Stacking for Latching Room\u2010Temperature Phosphorescence"],"prefix":"10.1002","volume":"38","author":[{"given":"Xipeng","family":"Yang","sequence":"first","affiliation":[{"name":"State Key Laboratory of Natural Product Chemistry Key Laboratory of Nonferrous Metal Chemistry and Resources Utilization of Gansu Province Lanzhou Magnetic Resonance Center College of Chemistry and Chemical 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