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Crystal structure and thermal behavior of isostructural binary complexes [Rh(en)3][Fe(CN)6] and [Rh(en)3][Cо(CN)6]

Abstract Binary complex compounds (BCC) [Rh(en)3][Fe(CN)6]·2H2O (I) and [Rh(en)3][Co(CN)6]·2H2O (II) have been prepared and characterized by the X-ray diffraction, crystal optic, elemental and thermal analyses. The crystal structures I and II (space group P21/n) are described within the monoclinic crystal system, are insular and isostructural. The thermal behavior of BCC I and II is identical, with an exception of a higher temperature (~by 50°C) of II decomposition. In air atmosphere, the ligand removal is followed by the formation of, respectively, Rh+1/2Fe2O3 and Rh+Co that on further heating up to 1000°C convert into RhFeO3 and RhCoO1.5. The residues of annealing at 1000°C in argon atmosphere are Rh+1/2Fe2O3 and Rh+CoO, respectively.