The synthesis and detailed characterization of a few samples of the compound RbxMn[Fe(CN)6]y·zH2O are described. The composition of the materials significantly depends on the applied preparativeconditions. Analysis of spectroscopic results (FTIR, Raman, 57Fe Mössbauer, XPS) and X-ray powder-diffraction data yielded a further assessment of the difference in structural features in terms of the amountof Fe(CN)6 vacancies and the associated number of water molecules. The characteristic individual magneticbehavior, as well as the metal-to-metal charge-transfer capabilities of the various samples, could be relatedto significant changes within the structures that appear to be associated with the synthetic method used.
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