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The development of novel high-efficiency photocatalysts to solve the bottleneck problems of low efficiency and harsh conditions of organic oxidation reactions is of vital significance. In this paper, a novel hybrid polyoxometalate (POM) crystal, (C 2 H 8 N) 6 [SiW 11 CdO 39 ][Ru(bpy) 2 (dcbpy)]• DMF•5.5H 2 O (RuCd−SiW), was synthesized by combining the metalloligand [Ru(bpy) 2 (dcbpy)] with the oxidation catalyst POM. The introduction of the metalloligand extended the light absorption range of RuCd−SiW to the visible region, while electrochemical measurements demonstrated its potential as an excellent photocatalyst. Under visible light (λ > 400 nm) irradiation with O 2 as the sole oxidant, RuCd−SiW showed highly efficient photocatalytic activity for the selective oxidation of thioanisole to (methylsulfoxide)benzene with a yield of 99.5%, a turnover number of 497.5, and a turnover frequency of 103 h −1 . Particularly, the yield of (methylsulfoxide)benzene was still higher than 99% after five rounds of recycling, demonstrating its high stability and recyclability.

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