Three three-dimensional (3D) compounds constructed from octamolybdate clusters and 1D–3D CuI/CuII-bis(triazole) motifs, [CuI4(btx)4][β-Mo8O26] (1), [CuI4(btx)2][β-Mo8O26]·H2O (2), and [CuII2(btx)4][α-Mo8O26] (3) [btx = 1,6-bis(1,2,4-triazol-1-yl)hexane], were hydrothermally synthesized in the presence of different amounts of reducing agent Et3N. The crystal structures have been determined by X-ray diffraction. In 1, the copper(I)-btx motif is a 1D meso-helix chain which is further linked by hexadentate β-[Mo8O26]4−clustersvia coordinating to CuI cations to achieve an intricate 3D structure. In 2, the copper(I)-btx motif exhibits a 2D grid sheet, and the hexadentate β-[Mo8O26]4−clusters interact with neighboring sheets to construct a 3D structure. In 3, the copper(II)-btx motif possesses a 3D (4,4)-connected framework with the (65.8)(64.82) topology, which is further connected by the tetradentate α-[Mo8O26]4−clusters forming a 3D self-penetrating (4,6)-connected hybrid network. The thermal stability and luminescent properties of 1–3 are investigated in the solid state.
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