本論文主要合成鑭系金屬的普魯士藍錯合物,得到9個以CN為架橋基4f-3d雙金屬錯合物及其單晶結構,[Tb(DMF)4(H2O)4Fe(CN)6]•H2O (1)、[Dy(DMF)3(o-phen)(H2O)3Fe(CN)6]•H2O (2)、[Er(DMF)3(o-phen)(H2O)3Fe(CN)6]•H2O (3)、[Nd(DMF)4(H2O)4Co(CN)6]•H2O (4)、[Sm(DMF)3(o-phen)(H2O)Fe(CN)6]2•4H2O•MeOH (5)、[Nd(DMF)2(MeOH)2(H2O)2Fe(CN)6]2 (6)、[Sm(bpy)(H2O)4Fe(CN)6]n•4nH2O•1.5n(bpy) (7)、[Pr(H2O)3Fe(CN)6]•2H2O (8)、 [Dy(H2O)2Fe(CN)6]•2H2O (9),其中發現第一個像鑽石網狀構造的三維結構錯合物8、9。在溫度範圍( 2 - 300 K )測得這些透過CN架橋連接鑭系與過渡金屬錯合物的變溫磁化率,其分子內的磁作用表現,則伴隨著鑭系金屬離子4f軌域上電子數不同與結構改變而表現反鐵磁性或鐵磁性偶合作用。 Nine novel cyano-bridged 4f-3d-metal complexes, [Tb(DMF)4(H2O)4Fe(CN)6]•H2O (1), [Dy(DMF)3(o-phen)(H2O)3Fe(CN)6]•H2O (2), [Er(DMF)3(o-phen)(H2O)3Fe(CN)6]•H2O (3), [Nd(DMF)4(H2O)4Co(CN)6]•H2O (4), [Sm(DMF)3(o-phen)(H2O)Fe(CN)6]2•4H2O•MeOH (5), [Nd(DMF)2(MeOH)2(H2O)2Fe(CN)6]2 (6), [Sm(bpy)(H2O)4Fe(CN)6]n•4nH2O•1.5n(bpy) (7), [Pr(H2O)3Fe(CN)6]•2H2O (8), [Dy(H2O)2Fe(CN)6]•2H2O (9), have been prepared and X-ray structural characterization. We found that complexes 8 and 9 are the first examples of 3-D structure with diamond-like network. The temperature ( 2 - 300 K ) dependence of magnetic susceptibility measurements of these Ln3+-NC-Fe3+ complexes shown that the antiferro- or ferromagnetic interactions between 3d and 4f are corresponding to their electron configuration of 4fn and structural features of Complexes (1) ~ (9).