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The selective detection and separation of target ions or molecules is an intriguing issue. Herein, a novel supramolecular organic framework (SOF-THBP) was constructed by bis-thioacetylhydrazine functionalized pillar[5]arenes. The SOF-THBP shows a fluorescent response for Fe3+ , Cr3+ , Hg2+ and Cu2+ ions. The xerogel of SOF-THBP shows excellent recyclable separation properties for these metal ions and the absorption rates were up to 99.29 %. More interestingly, by rationally introducing these metal ions into the SOF-THBP, a series of metal-ion-coordinated SOFs (MSOFs) such as MSOF-Fe, MSOF-Hg and MSOF-Cu were constructed. These metal ions coordinated MSOFs could selectively sense F- , Br- , and l-Cys, respectively. The detection limits of these MSOFs for F- , Br- and l-Cys were about 10-8 m.