The double complex salts [Au(En)2][Ir(NO2)6] • 2H2O (I) and [Au(En)2][Ir(NO2)6] (II) and solid solutions [Au(En)2][Ir(NO2)6]x[Rh(NO2)6]1–x • nH2O, where x = 0.25, 0.5, 0.75, were prepared and characterized by powder X-ray diffraction, IR spectroscopy, elemental analysis, and DTA. The crystal structures were determined by X-ray diffraction. The thermal behavior of compounds under reducing atmosphere was studied. The final products of thermolysis were found to be two-phase mixtures consisting of nano-sized pure gold particles (~55 nm) and particles of Au–Ir–Rh solid solutions (~3 nm).
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