The complex salts ((DienH3)[IrCl6](NO3) (I), (DienH3)[PtCl6](NO3) (II), and (DienH3)[IrCl6]0.5[PtCl6]0.5(NO3) (III) (where Dien is NH2(CH2)2NH(CH2)2NH2) were synthesized and characterized by elemental, X-ray diffraction, and thermal analyses and by electronic and IR spectroscopies. Solid solution of the composition Ir0.35Pt0.65 was obtained by decomposition of compound III in the atmosphere of hydrogen.