Two novel hybrid materials based on two kinds of octamolybdate anions and metal–organic frameworks (MOFs), namely, [Ag8(L1)4(α-Mo8O26)(β-Mo8O26)(H2O)3]·H2O (1) and [CuI3.1CuII0.5(β-Mo8O26)0.5(ζ-Mo7VIMoVO26)0.5(L2)2(H0.8L2)0.5] (2), where L1 = 1,1′-(1,3-propanediyl)bis[2-(4-pyridyl)benzimidazole] and L2 = 1,1′-(1,4-butanediyl)bis[2-(3-pyridyl)benzimidazole], have been successfully synthesized. Crystal structure analysis revealed that 1 is a three-dimensional (3D) framework constructed of silver(I)–organic sheets and two types of (Mo8O26)4− isomers. Compound 2 is a rare 3D framework containing copper(I,II)–organic cages and 1D channels occupied by the (ζ-Mo7VIMoVO26)5− and (β-Mo8O26)4− anions. The two compounds were characterized by elemental analysis, IR spectroscopy, diffuse reflectivity spectroscopy, and photoluminescent spectroscopy. In addition, the photocatalytic behavior of 1 was investigated.
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