| In this paper, eleven novel coordination complexes containing flexible bis(benzimidazole) ligands which have never been reported previously were synthesized. This article represents a systematical examination of their structures. In order to survey the influence of the neutral ligands, anions, and metal ions on the formation of the final structures, three flexible ligands, 1,1'-(1, 4-butanediyl)bis(2-methylbenzimidazole) (L1), 1,1'-(1, 4-butanediyl)bis(2-ethylbenz -imidazole) (L2) and 1,1'-(1, 4-butanediyl)bis(2-benzylbenzimidazole) (L3) and four kinds of acid, p-Methoxy-benzoic acid (Hpmb), Cinnamic acid (Hcin) 2-(N-Morpholino)ethane- sulfonic acid (HMES) and Adipic acid (H2adi) are selected for study, and eleven novel compounds have been synthesized: [Cu(pmb)2(L1)] (1), [Cu(pmb)2(L2)] (2), [Cd(cin)2(L1)]·H2O (3), [Cd(cin)2(L2)] (4), [Ag(MES)(L1)(0.5] (5), [Ag(MES)(L2)0.5]·H2O (6), [Zn(adi)(L1)]·H2O (7), [Zn(adi)(L2)0.5] (8), [Cd(adi)(L1)]·2H2O (9), [Cd(adi)(L2)] (10) and [Cd(adi)(L3)]·2H2O (11). The crystal structures have been determined by single-crystal X-ray diffraction. Compounds 1–5 display one-dimensional (1D) chain structures. Compounds 6–9 possess 2D polymeric structures. The layers of 7 and 9 interlace with each other by hydrogen bonds to generate a twofold interpenetration three-dimensional supramolecular structure. Compound 8 contains a dimeric unit, which is built from two zinc atoms and four adi ligands. Both compounds 10 and 11 reveal typically diamondoid frameworks, and a fourfold interpenetrated framework has been observed in 10. Thermogravimetric analyses (TGA) for these compounds are discussed. The luminescent properties for 3–11 are also discussed in detail.
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