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Nanoscale polyoxometalates (POMs), with their reversible redox properties, exhibit promising potential in developing outstanding CDT drugs by exploring their Fenton\u2010like catalytic reactivity in tumor environments. However, such research is still in its infancy due to the challenges of acquiring POMs that are both easily prepared and possess ideal therapeutic effects, physiological solubility, biocompatibility and safety. In this work, we report the synthesis of a new crystalline antimonotungstate {Dy<jats:sub>2<\/jats:sub>Sb<jats:sub>2<\/jats:sub>W<jats:sub>7<\/jats:sub>O<jats:sub>23<\/jats:sub>(OH)(DMF)<jats:sub>2<\/jats:sub>(SbW<jats:sub>9<\/jats:sub>O<jats:sub>33<\/jats:sub>)<jats:sub>2<\/jats:sub>} (<jats:bold>1<\/jats:bold>, DMF=N, N\u2010dimethylformamide) with gram\u2010scale high yield via a facile \u201cone\u2010pot\u201d solvothermal reaction. <jats:bold>1<\/jats:bold> exhibits not only a soluble and water\u2010stable POM nanocluster, but also excellent catalytic activity for hydroxyl radical\u2010generating Fenton\u2010like reactions. Further biomedical studies reveal that <jats:bold>1<\/jats:bold> can trigger cell apoptosis and promote lipid peroxidation, exhibiting high cytotoxicity and selectivity towards B16\u2010F10 mouse melanoma cancer cells with an IC<jats:sub>50<\/jats:sub> value of 4.75\u2005\u03bcM. Especially, <jats:bold>1<\/jats:bold> can inhibit melanoma growth <jats:italic>in vivo<\/jats:italic> with favorable biosafety, achieving a 5.2\u2010fold reduction in tumor volume and a weight loss of 76.0\u2009% at the dose of 70\u2005\u03bcg\/kg. This research not only demonstrates the immense potential of antimonotungstates in CDT drug development for the first time but also provides new insights and directions for the development of novel anticancer drugs.<\/jats:p>","DOI":"10.1002\/anie.202422949","type":"journal-article","created":{"date-parts":[[2024,12,16]],"date-time":"2024-12-16T10:05:31Z","timestamp":1734343531000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":25,"title":["A Highly Biocompatible Polyoxotungstate with Fenton\u2010like Reaction Activity for Potent Chemodynamic Therapy of Tumors"],"prefix":"10.1002","volume":"64","author":[{"given":"Hui\u2010Ping","family":"Xiao","sequence":"first","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Inorganic Oxygenated Materials Fuzhou University  Fuzhou Fujian 350108 China"},{"name":"College of Chemistry and Materials Jiangxi Normal University  Nanchang Jiangxi 330022 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