Аннотация:Dichalcogenides of transition metals are especially interesting. Majority of chalcoginides are semiconductors and some of them show interesting properties in certain regions of optical spectrum. Such properties allow application of these compounds in optico-electronics, radio-photonics, laser physics etc. Direct synthesis one of simple chalcogenides - rhenium disulphide - has been carried out from source components: metallic rhenium and elemental sulfur. In this research we used high temperature annealing at 1000 0C and the pressure of 10-5 atm in 24 hours. The synthesis was carried out in a sealed quartz ampoule. Photoelectron spectra and IR absorption spectra of molybdenum disulfide (IV) and rhenium disulfide (IV) were measured during the research. We shows that rhenium disulfide (IV) crystallize in CdI2 structural type. S2p sulfur bond energy for molybdenum disulfide (IV) and rhenium disulfide (IV) are at almost identical values. IR spectrum analysis shows that rhenium disulfide (IV) structure compared with molybdenum disulfide (IV).