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© 2021 American Chemical Society.Developing new catalysts for highly efficient and selective oxidation of saturated C–H bonds is significant due to their thermodynamic strength. Via incorporation of PW12O403–, pyridine–2,5–dicarboxylic acids (pydc), and Fe(III) ions into one framework, a new polyoxometalate–based metal–organic framework, [HFe4O2(H2O)4(pydc)3PW12O40]·10.5H2O (FeW–PYDC), was successfully prepared by a hydrothermal method. Interestingly, FeW–PYDC features a three–dimensional porous structure with {Fe4O2} interconnecting with PW12O403– units. FeW–PYDC displayed excellent performance in the selective oxidation of C–H bonds of alkylbenzenes with high conversion (95.7%) and selectivity (96.6%). As an effective heterogeneous catalyst, FeW–PYDC demonstrates good reusability and structural stability.
