X-ray powder diffraction data for Mo2.85Al1.91Si4.81 are presented here. The new Mo2.85Al1.91Si4.81 compound was successfully prepared, using the self-propagating high-temperature synthesis (SHS) technique. The starting atomic mixture of reactant powders was Mo + 2(1 - x)Si + 2xAl with 0.2 ≤ x ≤ 0.5. The final powder compound obtained by the SHS technique was determined to be in x = 0.2; Mo(Si, Al)2 and in 0.3 ≤ x ≤ 0.5; Mo2.85Al1.91Si4.81. respectively X-ray powder diffraction pattern of Mo2.85Al1.91Si4.81 was recorded using an X-ray powder diffractometer and CuKa radiation that have been analyzed by automatic indexing programs. Mo2.85Al1.91Si4.81 was found to be hexagonal.
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