The complex with the formula ［CeFe(CN)6(H2O)3］.2H2O was synthesized and structurally characterized. It crystallizes in hexagonal, space group P3, a＝0.75320(10) nm, b＝0.75320(10) nm, c＝1.4374(3) nm, γ＝120°, V＝0.7062(2) nm3, Z＝3, Dc＝3.048 Mg.m-3, F(000) ＝606, μ＝6.346 mm-1, T＝293(2) K, R1＝0.0169, Wr2＝0.0459. The structure is a three-dimensional network containing open channels formed by the nine-coordinated CeN6(H2O)3 groups and octahedral FeC6 groups through the cyanide linkages. Magnetic susceptibility measurements in the temperature range of 5.1～300 K show an antiferromagnetic interaction between the Ce3+ and Fe3+ ions.
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