EN
A series of compounds Li_xMn_{3-x-y}Fe_yO_4 (x=1.0125;0≤y≤0.05) were synthesized by solid state reaction of Li_2CO_3 with the manganese oxide or iron-manganese oxide precursors. Investigations of the structure transformation effect of double substitution with Li^+ and Fe^{3+} ions in LiMn_2O_4, in the temperature range of 10-300 K, were undertaken using high-resolution X-ray powder diffraction at the HASYLAB (DESY) synchrotron. The Li_{1.0125}Mn_{1.9625}Fe_{0.025}O_4 transforms from cubic (Fd3̅ m) to orthorhombic (Fddd) below 250 K, and is stable to 10 K. Whereas in the Li_{1.0125}Mn_{1.9375}Fe_{0.05}O_4 oxide no phase transition was observed, this spinel remains in cubic structure down to the temperature of 10 K.