Metal-organic frameworks have attracted much attention to the design and construction of transition metal complexes because of their intriguing network topologies and potential applications, and due to their capacity for gas storage, and luminescent and magnetic properties. The assembly of three-dimensional (3D) heterometallic complexes, however, is a formidable task due to the variable and versatile coordination numbers of the mixed metal ions, their low stereochemical preference and also because of competitive reactions between metals coordinated with the same organic ligands. Being in line with these investigations we report herein the products of interaction of Co(II)/Zn(II), Zn(II)/Cd(II) salts with 1,2-bis(4- pyridyl)ethane (bpe) in the presence of 2,2'-dithiodibenzoic acid (H2dtdb). On the basis of above mentioned considerations, we obtained two new 3D coordination polymers [CoZn(bpe)2(dtdb)2]n (1) and [ZnCd(bpe)2(dtdb)2]n (2) under hydrothermal conditions, and crystals were further characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction. Compounds 1 and 2 are isostructural and crystallize in the noncentrosymmetric trigonal P3121 space group: a=11.4871(7), b=11.4871(7), c=16.7589(16) Å, γ=120º, V=1915.12 Å3 for 1 and a=11.5786(12), b=11.5786(12), c=16.4899(19) Å, γ=120º, V=1914.52 Å3 for 2. Both compounds are isostructural with homonuclear compound [Zn(bpp)2(dtdb)2]n [1]. The octahedral N2O4 metal coordination cores in 1 and 2 are originated from two N atoms of bidentate bridging bpe molecules, four O atoms of two tetradentate dtdb2- coordinated in chelate‒bridging mode. Figure. Packing view which indicates different metallocycles in 1 (Co/Zn) (2 – isostructural (Zn/Cd)). In the IR spectra of the complexes, the presence of phenyl rings is indicated by the bands at 1613 cm-1 in 1 and 1612 cm-1 in 2. The asymmetric stretching vibrations νas(COO) are observed at 1647 cm-1 in 1, 1644 cm-1 in 2, and the νs(COO) bands are at 1368 cm-1 in 1 and 1398 cm-1 in 2. Characteristic vibration bands at 1155 cm-1 and 1280 cm-1 belong to νs(C–N). The thermogravimetric analyses are in progress.