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Two new compounds with microporous Co 3 [MnMo 9 O 32 ]·15H 2 O (1) and Cu 3 [MnMo 9 O 32 ]·15H 2 O (2) have been synthesized, and characterized by IR, element analysis, TG and single-crystal X-ray analysis. The structure analyses reveal that compounds 1 and 2 are isostructural. In crystal, the Waugh-type polyoxoanions [MnMo 9 O 32 ] 6-are connected by Co 2+ or Cu 2+ cations to a 3D open-framework, which possesses channels along the [1 2 2] direction of approximately 8.27 × 11.97 Å. The photocatalytic performances of compounds 1 and 2 for photodegradation of RhB with UV irradiation have been studied, which show a good photocatalytic activity for photodegradation of RhB. porous materials, Waugh-type polyoxoanion, single-crystal structure, photocatalysis

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