Abstract: This work presents six CuII, CoII, and NiII supramolecular complexes assembled from a bent dipyridyl ligand 2,5-bis(3-pyridyl)-1,3,4-oxadiazole (3-bpo) and R-isophthalic acids (R =–CH3 for 5-methylisophthalic acid or R =–OCH3 for 5-methoxyisophthalic acid), which have been prepared using the layer-separation diffusion method and fully characterized by IR, elemental analysis, and powder X-ray diffraction (PXRD) techniques. Single-crystal X-ray diffraction indicates that these complexes show 1-D tube-like (for CuII complexes 1 and 2) or discrete cage-like dinuclear (for CoII and NiII complexes 3–6) coordination patterns. Furthermore, extended 3-D supramolecular architectures are constructed via secondary interactions between the coordination arrays, and three types of packing fashions are observed for the dinuclear species 3–6. Structural diversification for these complexes can be properly attributed to the inherent discrepancy of metal ions and the substituent effect of R-isophthalate tectons. [Copyright &y& Elsevier]