A simple, novel method for improving the electrochemical response of Sn in lithium cells is proposed that involves preparing Sn by a reduction procedure in the presence of Mo powders. Four different Mo x Sn1− x mixtures (0< x <0.26) were electrochemically tested and their structural and textural properties determined by using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The electrochemical properties of the resulting composites in lithium cells were studied by galvanostatic, step potential electrochemical spectroscopy (SPES) and electrochemical impedance spectroscopy (EIS) measurements. The mixtures were found to consist of crystalline Sn and Mo; however, the presence of the latter element modified the Sn habit in two ways, namely, by significantly decreasing particle size and increasing the reactivity towards oxygen. Although Mo is inert towards lithium, it increased both the discharge capacity and the capacity retention of the electrode in relation to pure Sn. The improved interparticle connectivity, reduced electrolyte decomposition and decreased charge-transfer resistance observed in the Mo-containing samples appear to be beneficial effects of the addition of Mo.