Coordination polymers recently known as metal-organic frameworks (MOFs) have become a forefront in scientific research and public interest, due to the potential for neutral guest bonding, including gas storage studies such as hydrogen storage and gas separations. The aim of this work was the synthesis, determination of the composition, structure, and sorption properties of Zn(II) MOFs using rigid ligands. Here we report a method of solvothermal synthesis of Zn(II) complex using 2,3,5,6tetramethyl-1,4-carboxyphenyl benzene (4-CH3-TF) and bis-imidazolyl-bis-phenylene (BIBPh) as starting ligands. The synthesized product represents a tridimensional polymeric compound [Zn2(4-CH3-TF)2(BIBPh)(DEF)]n. The composition and structure of the complex was demonstrated by physical methods of analyses (X-ray, thermogravimetry, IR). Single crystal Xray structure investigation of this coordination compound has demonstrated, that in the crystalline phase a polymeric structure was obtained, where binuclear Zn(II) groups are interconnected by two bridging tetradentate molecules of 4-CH3-TF ligand and one bidentate BIBPh. Two types of large cavities were identified in the polymer, where solvent molecules of DEF are adsorbed (Figure). Thermogravimetric study has demonstrated that heating of polymeric sample up to 250°C leads solely to elimination of solvent molecules from micropores.The degassed compound is stable up to 400°C, then an irreversible collapse of molecular framework occures. Sorption properties have been tested through N2 adsorption at 77 K and shown a maximum sorption value of ~110 cm3/g.