[Et_4NB_(12)H_(11)NHCOCH_2CONH_2]^-及bipyO_2的稀土混配配合物研究

Studies on Rare Earth Complexes of Mixed-Ligands Containing [Et_4NB_12H_11NHCOCH_2CONH_2]- and bipyO_2

将[Et_4]_2B_(12)H_(12)与丙二腈反应,生成化合物Et_4NB_(12)H_(11)NCCH_2CN,水解后得[Et_4NB_(12)H_(11)NHCOCH_2CONH_2]^-·[Et_4NBN]^-,该衍生物与稀土氯化物(LnCl_3)及2,2＇-联吡啶-N,N＇-二氧化物(bipyO_2)反应,合成了几种新型的混配稀土配合物Ln(bipyO_2)_4(Et_4NBN)_3(Ln=La,Nd,Sm,Gd,Dy,Ho,Er).元素分析确定了它们的组成,通过IR、UV、~1H NMR、ESR、摩尔电导测定及TG-DTA等对其性质进行了研究。

Mono-substituted amide derivative of [Et4N]2B12H12, [Et4N]2B12H11NHCOCH2CONH2 ·([Et4N]2BN), was obtained from acid-catalyzed reaction between [Et4N]2B12H12 and malononjtrile, followed by hydrolysis. The derivative reacts with lanthanide chlorides and 2, 2'-bipyridine-N,N' -dioxide (bipyO2) to produce 7 novel mixed- ligand rare earth (Ⅲ) complexes with the formula Ln(bipyO2)4(Et4NBN)3, where Ln = La, Nd, Sm, Gd, Dy, Ho and Er. These complexes were characterized by elemental analysis, IR, UV, 1H NMR, ESR and molar conductivities. The thermal properties of the ligands and the complexes were investigated by TG-DTA.