Rhenium alkoxocomplexes (Re4O6(OMe)12) and Re4O6(OPri)10) were obtained by the anodic dissolution of rhenium. The complexes were studied using the IR spectrometry and Energy Dispersive Analysis. Bimetallic rhenium–nickel alkoxocomplexes (Re4 – xNixO6(OMe)12, Re4 – xNixO6(OPri)10) and rhenium–cobalt alkoxocomplexes (Re4 – xCoxO6(OMe)12, Re4 – xCoxO6(OPri)10) were synthesized of monometallic alkoxocomplexes and characterized using the IR spectrometry. It is shown that homogeneous bimetallic powder of Re0.79Ni0.21 alloy can be produced of rhenium–nickel methylate and isopropylate and the powder of Re0.67Co0.33 alloy, of rhenium–cobalt methylate using the reduction in the hydrogen atmosphere at a temperature of 650°C and a pressure of 5 atm.