Abstract: New double perovskites LaPbMSbO₆, where M²⁺ = Mn²⁺, Co²⁺, and Ni²⁺, were synthesized as polycrystals by an aqueous synthetic route at temperatures below 1000 ^°C. All samples are monoclinic, space group P2₁/n, as it is observed from Rietveld analysis of X-ray powder diffraction patterns. The distribution of M²⁺ and Sb⁵⁺ among the two octahedral sites have 3% of disorder for M²⁺ = Ni²⁺, whereas for M²⁺ = Mn²⁺ and Co²⁺ less disorder is found. The three samples have an antiferromagnetic transition, due to the antiferromagnetic coupling between M^{2 +} through super-superexchange paths M²⁺-O^2--Sb⁵⁺-O^2--M²⁺. Transition temperatures are low: 8, 10 and 17 K for Mn²⁺, Co²⁺, and Ni^{2 +} respectively, as a consequence of the relatively long distances between the magnetic ions M²⁺. Besides, for LaPbMnSbO₆ a small transition at 45 K was found, with ferrimagnetic characteristics, possibly as a consequence of a small disorder between Mn²⁺ and Sb⁵⁺. This disorder would give additional and shorter interaction paths: superexchange Mn²⁺-O^2--Mn²⁺.

Abstract: Y[Fe(CN)6]·4H2O has been synthesized and characterized. The crystal structure was refined by Rietveld analysis using X-ray powder diffraction data. Y[Fe(CN)6]·4H2O crystallizes in the orthorhombic crystal system, space group Cmcm. Y3+ ion is eight-coordinated forming a bicapped distorted trigonal prism YN6O2. Fe3+ ion is six-coordinated in the form of an irregular octahedra FeC6 group and cyanide linkages between YN6O2 and FeC6 groups build an infinite polymeric array. The vibrational spectrum shows two bands corresponding to antisymmetric and symmetric stretching 12C14N in the CN stretching region. These bands are accompanied by four weak isotopic bands at lower frequency due to the presence of 13C and 15N in relative natural abundance. The HOH bending band split into three bands around 1600 cm−1 due to the presence of two kinds of water molecules in the structure. The thermal decomposition has been followed by thermogravimetric and differential thermal analysis, IR spectroscopy and powder XRD. The size and morphology of the complex and its thermal decomposition products were evaluated by scanning electron microscopy. The magnetic measurements confirm that Y[Fe(CN)6]·4H2O shows an antiferromagnetic order at low temperatures.