The present research is based on a low temperature operated feasible method for the synthesis of immiscible iron and molybdenum metals' nanoalloy for technological applications. The nanoalloy has been synthesized by pyrolysis of homogeneous powder precipitated, from a common solvent, of the two complexes, trisbipyridineiron(II)chloride, [Fe(bipy)(3)]Cl-2, and bipyridinemolybedenum(IV) chloride, [Mo(bipy)Cl-4], followed by heating at 500 degrees C in an inert atmosphere of flowing argon gas. The resulting nanoalloy has been characterized by using EDXRF, AFM, XRD, magnetometery, Fe-57 Mossbauer and impedance spectroscopies. These results showed that under provided experimental conditions iron and molybdenum metals, with known miscibility barrier, alloy together to give (1:1) single phase material having particle size in the range of 48-66 nm. The magnetism of iron is considerably reduced after alloy formation and shows its trend toward superparamagnetism. The designed chemical synthetic procedure is equally feasible for the fabrication of other immiscible metals. (C) 2013 Elsevier Ltd. All rights reserved.