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Four octamolybdate hybrid materials based on a new flexible multidentate ligand, namely, H4L(γ-Mo8O26)·2H2O (1), [Cu(H2L)(β-Mo8O26)(H2O)2]·3H2O (2), [Cu(H2L)(γ-Mo8O26)]·3H2O (3), and Cu(HL)2(β-Mo8O26) (4), where Lis 1,1′-(1,4-butanediyl)bis[2-(4-pyridyl)benzimidazole], have been synthesized at different pH values under hydrothermal conditions. Compound 1, which is hydrothermally prepared at pH ≈ 1, exhibits a rare one-dimensional (1D) molybdenum oxide chain. Compounds 2and 3are hydrothermally obtained at pH ≈ 2.5. In 2, CuIIcations are bridged by H2L2阨᪝ and (β-Mo8O26)4–anions to form an interesting two-dimensional (2D) layer. In 3, the H2L2阨᪝ and (γ-Mo8O26)4–clusters bridge adjacent CuIIcations to form a 3D framwork. When the pH value is adjusted to 3.5, compound 4is obtained. Because the HL熫抢 acts as a monodentate ligand, compound 4only exhibits a 1D chain structure. The structural diversities of 1–4reveal that the pH value of the reaction system plays a crucial role in the assembly of POM-based metal–organic frameworks (MOFs). In addition, the electrochemical property of compound 4has also been investigated in 1 M H2SO4aqueous solution. [ABSTRACT FROM AUTHOR]