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Compound [Ni(AEAPTS)2]3[Fe(CN)6]2 (AEAPTS=N‐(2‐aminoethyl)‐3‐aminopropyltrimethoxysilane), in which Ni2+ and Fe3+ ions are ferromagnetically coupled through cyano bridges, was prepared. Sol–gel processing of the AEAPTS derivative resulted in incorporation of the cyanometallate in silica. The obtained material is magnetically ordered below 22 K with an effective magnetic moment μeff of 4.46 μB at room...