Integrating Fenton chemistry and nanomedicine into cancer therapy has significantly promoted the development of chemodynamic therapy (CDT). Nanoscale polyoxometalates (POMs), with their reversible redox properties, exhibit promising potential in developing outstanding CDT drugs by exploring their Fenton-like 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