Abstract Two unique bimetalic Pt(II) coordination polymers of composition [Ni( hydeten) 2Pt(CN) 4] ( Ni– Pt) and [Cu( hydeten) 2Pt(CN) 4] ( Cu– Pt) [ hydeten = N-(2-hydroxyethyl-ethylenediamine) or 2-(2-aminoethylamino)ethanol] have been synthesized and structurally characterized by various methods in this study. The crystal structure of Cu– Pt was determined by single-crystal X-ray diffraction analysis. The structure of Cu– Pt forms of infinite 2,2-TT type [–Cu( hydeten) 2–NC–Pt(CN) 2–CN–] chains containing paramagnetic copper atoms bridged by tetracyanoplatinate species. In this complex, Cu(II) centers display an axially elongated octahedron with two chelating hydeten molecules in the equatorial positions and N-bonded bridging cyano groups in the axial positions, whereas Pt(II) centers are four coordinate with four cyanide-carbon atoms in a square-planar arrangement. The decrease of the moments of these complexes in temperature range of 50 305 K can assigned to the antiferromagnetic interactions in the structures. The thermal decomposition of Cu– Pt comprise of five distinguished stages, while the thermal decomposition of Ni– Pt take place four different stages.