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Hydrogen cyanide, acetylene and ethylene, as well as the products of their reactions, were found in comets, interstellar space and atmospheres of some planets, for example, in the atmosphere of Titan, the largest satellite of Saturn. These small molecules can be participants in the process of multi-stage formation of complex organic compounds under the influence of radiation of various energies in outer space. The method of matrix isolation makes it possible to investigate the mechanisms of such reactions. To date, there are only a few studies devoted to the study of the photochemistry of HCN / hydrocarbon systems in matrix of argon [2]. In this paper, radiation chemistry and spectroscopy of HCN/C2H2 and HCN/C2H4 systems in low-temperature matrices of noble gases was first studied. Radiolysis was performed using an X-ray tube with an average radiation energy of 20 keV at a temperature of 6 K. The cryostat used in this work allows controlled heating in the temperature range of 6-50 K. The HCN...C2H2 and HCN...C2H4 complexes were identified by the IR-spectroscopy, the assignment is consistent with the calculation data. Shown, that the radiolysis efficiency of the complexes is higher than that of isolated molecules. In addition to the main products of the radiolysis of HCN and C2H2 in systems HCN/C2H2/noble gas the formation of cyanoacetylene was observed.