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A novel polyoxometalate(POM)-based metal-organic frameworks(MOFs),[TBA]3[ε‐PMo8ⅤMo4ⅥO36(OH)4Zn4][BTB]4/3·18H2O(NENU-500,H3BTB = benzene tribenzoate,TBA+= tetrabutylammonium ion)),was isolated.