Growing practical interest to the bibenzyl compounds stimulates an intensive study of their fundamental physical-chemical properties by various experimental techniques and quantum-chemical calculations at different levels of theory. These ligands attract considerable attention due to conformational flexibility and an unusual shortening of central C(sp3)-C(sp3) bond [1]. Herein, we report the preparation, IR characterization, X-ray study and thermal analysis of new 2D coordination polymer {[Co(4,4'-bpy)2(H2O)2](BF4)2(dadpe)(C2H5OH)2}n (1) using rigid rod-like N,N-bipyridyl-based ligand such as bpy (4,4′ -bipyridyl) as the bidentate linker and linear dadpe (4,4′-diaminodiphenylethane) as a guest molecule. 1 was obtained as a result of the reaction between Co(BF4)2·6H2O, bpy and dadpe in C2H5OH solvent. The IR spectra of 1 and the pure dadpe and bpy were measured and confirm the presence of organic ligands in the coordination polymer. The absorption bands at 3480-3359 cm-1 were assigned to asymmetric and symmetric stretching vibrations ʋ(NH2), while deformation vibration δ(NH) were registered at 1605 cm-1. The bands at 1221-1173 cm-1 were assigned to the ʋs(C-N) and ʋas(C-N) stretching vibrations. 1 is monoclinic, space group C2/c: a=19.0858, b=11.4429, c=22.5537 Å; β=121.947o, V = 4179.6(6) Å3. The Co(II) cation adopts a slightly distorted octahedral geometry with the N4O2-set of donor atoms. The Co-N bond distances range from 2.170(3) to 2.223(2) Å and Co-O distance is 2.057(2) Å. Fig. 1. TG/DTG/DTA plots of 1 In the crystal the coordination layers are united by O-H...N and N-H...O hydrogen bonds through uncoordinated dadpe and C2H5OH guest molecules. Thermal analysis curves of the title compound are shown in figure 1. The DTG curve has four intense maxima. The first stage covers the range of 96-223oC and indicates the elimination of two C2H5OH molecules with a mass loss of 9.98% (10.39% calc.), followed by the loss of two water molecules, with the mass loss of 4.66% (4. 05% calc.). Immediately after this, the ligands start to decompose. The bpy decomposition, proceeds simultaneously with the loss of water molecules and up to 301oC, and the dadpe ligand completely decomposes at 660oC. The subsequent increase in temperature leads to oxidative degradation of the organic residue and the formation of cobalt oxide, the mass fraction of the resulting residue is 7.09% (8.47% calc.).