The new ternary compound of Al2Cu3Gd was prepared by melting with stoichiometric composition in an electric arc furnace. The X-ray powder diffraction data of Al2Cu3Gd have been collected by the Rigaku Smart Lab X-ray powder diffractometer. The Rietveld refinement method had been used to study the crystal structure of Al2Cu3Gd. The results showed that the Al2Cu3Gd, new compound have the hexagonal structure, space group P6/mmm (No. 191) with a = 5.1822 (1) Å, c = 4.1566 (1) Å, V = 96.67 Å3, Z = 1, and the density is 6.62 g cm−3, and the intensity ratio reference intensity ratio is 1.29.