Double Complex Salt [Pd(NH3)4][VO(H2O)(C2O4)2]·2H2O: Structure and Thermal Properties

A synthesis of the [Pd(NH3)4][VO(H2O)(C2O4)2]·2H2O double complex salt (DCS) is developed and optimized. The compound is characterized by single-crystal and powder XRD, IR spectroscopy, and diffuse reflectance spectroscopy (DRS). Crystal data: $$P\bar{1}$$ space group, a = 7.3160(10) Å, b = 8.2700(2) Å, c = 12.9205(2) Å, α = 71.576(10)°, β = 78.477(10)°, γ = 83.844(10)°, Z = 2. An exchange interaction between complex anions is revealed by EPR. The process of DCS thermal decomposition in inert and reducing atmospheres is studied. It is established that the final thermolysis product in the reducing atmosphere is a mixture of the Pd0.90V0.10 solid solution and vanadium(III) oxide. The DRS spectra for the obtained DCS are theoretically calculated.