New double complex salt [PdEn2]3[Rh(NO2)6]2 · 2.67H2O: Synthesis, crystal structure, and thermal properties

Abstract

The crystal structure of the double complex salt (DCS) [PdEn₂]₃[Rh(NO₂)₆]₂ • 2.67H₂O (I) has been determined by X-ray diffraction. Crystals are triclinic, space group \(P\bar 1\), Z = 4, a = 9.2331(3) Å, b = 9.9136(4) Å, c = 13.7824(5) Å, α = 84.3230(14)°, β = 89.9655(14)°, γ = 66.7272(13)°, V = 1152.19(7) ų, ρ_calcd = 2.141 g/cm³, R = 0.0279. The thermal behavior of complex salt I has been studied in various gas atmospheres. The end product of thermolysis in reductive atmosphere is a mixture of Pd_0.45Rh_0.55 and Pd_0.95Rh_0.05 solid solutions. The end product of thermolysis in an inert atmosphere is a homogeneous Pd_0.6Rh_0.4 solid solution.