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Two-dimensional nanomaterials have become a hot research topic, and progress in research on them in the past decade has been substantial. Here we demonstrate a molecule-based bottom-up method to synthesize freestanding polyoxometalatebased nanosheets in two different ways. The trans substitution of ligands with carboxylate functionality promoted the coordination of organically derivatized hexavanadate with zinc ions with preferential directionality, which led to the formation of coordination polymer nanosheets. Characterization with transmission electron microscopy, powder X-ray diffraction, and infrared spectroscopy confirmed the morphology, structural composition, and preferential direction of the nanosheets. The microwave-assisted heating method and solvent addition method were proved to be effective for the preparation of POM-based nanosheet structures. The nanosheets were found to catalyze the aerobic oxidation of propanethiol (n-PrSH) to its corresponding disulfide (PrSSPr) under mild conditions.
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