The crystal structure of a double complex salt of the composition [Au(en)2]2[Cu(C2O4) 2]3·8H2O (en = ethylenediamine) at 150 K is determined by single crystal X-ray diffraction. The crystal data for C 20H48Au2Cu3N8O32 are: a = 9.1761(3) Å, b = 16.9749(6) Å, c = 13.4475(5) Å, β = 104.333(1)°, V = 2029.43(12) Å3, P21/c space group, Z = 2, dx = 2.450 g/cm3. It is demonstrated that the thermal decomposition of the double complex salt in a helium or hydrogen atmosphere affords the solid solution Au0.4Cu0.6. Original Russian Text Copyright © 2011 by E. V. Makotchenko, E. A. Bykova, E. Yu. Semitut, Yu. V. Shubin, P. V. Snytnikov, and P. E. Plyusnin.