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In situ X-ray absorption near edge structure (XANES) investigations were carried out at chlorine K edge and palladium L3 edge to study the mechanism of the thermal decomposition of ammonium hexachloropalladate. The spectra show a characteristic feature for the initial step that might be explained as the formation of the precursor via ligand exchange (Cl ⇒ NH3). Multiple scattering calculations (Feff 8) for the Cl K, Pd and Rh L3 edges were successful in simulating the XANES spectra of the precursor as well as the reference compounds (NH4)2[PdCl4] and (NH4)3[RhCl6].

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