2p-4f及2p-3d-4f体系配合物的合成，结构及磁性研究
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摘要
以氮氧自由基为配体,设计合成2p-4吸2p-3d-4盼子纳米磁体。成功得到了25个未见文献报道的氮氧自由基-稀土及氮氧自由基-稀土-过渡金属配合物。解析了这些配合物的晶体结构。同时运用红外光谱,元素分析等研究手段对得到的配合物进行了表征,并对它们进行了磁学性质的研究。本论文的主要工作如下：
1.分别以甲基,环丙烷基,3-溴-4-甲氧基苯基取代氮氧自由基为配体,与稀土的六氟乙酰丙酮盐反应,得到了9个氮氧自由基桥联稀土离子形成的一维链状配合物[Ln(hfac)3(NIT-Me)]n (LnⅢ=Y, Tb, Dy),[Ln(hfac)3(NIT-C3H5)]n (LnⅢ=Gd, Tb)及[Ln(hfac)3(NIT-3BrPhOMe)]n (LnⅢ=Gd, Tb, Dy)。磁性研究表明：配合物[Dy(hfac)3(NIT-Me)]n与[Tb(hfac)3(NIT-C3H5)]n均显示了相外频率依赖性,可能为单链磁体。配合物[Ln(hfac)3(NIT-3BrPhOMe)]n(LnⅢ=Tb, Dy)展示缓慢磁化强度弛豫和三维反铁磁有序共存的现象。
2.以苯并咪唑基,2-甲基苯并咪唑基及4-甲氧基-3-吡啶基取代的功能化氮氧自由基为配体,与稀土三氟取代或六氟取代的乙酰丙酮盐反应,得到9个氮氧自由基-稀土单核配合物[Ln(tfa)3(NIT-BzImH)](LnⅢ=Gd, Tb, Dy),[Ln(hfac)3(NIT-BzImCH3)](LnⅢ=Gd, Tb, Y)与[Ln(hfac)3(NIT-3BDOCH3)](LnⅢ=Gd, Tb, Dy)。磁学性质研究表明,配合物[Ln(tfa)3(NIT-BzImH)](LnⅢ=Tb, Dy),[Tb(hfac)3(NIT-BzlmCH3)]与[Tb(hfac)3(NIT-3BDOCH3)2]相外磁化率显示频率依赖性,表明这几个化合物可能为单分子磁体。
3.分别以4-丙氧基苯和4-苄氧基苯取代的氮氧自由基为桥联配体,同时与Ln(hfac)3·2H2O和Cu(hfac)2反应,合成得到六例2p-3d-4f一维链状配合物[Ln3Cu(hfac)11(NIT-PhOPr)4]n (LnⅢ=Gd, Tb, Dy),和[Ln3Cu(hfac)11(NIT-PhOCH2Ph)4]n (LnⅢ=Gd, Tb, Dy)。AC测量研究表明配合物[Ln3Cu(hfac)11(NIT-PhOPr)4]n (LnⅢ=Tb, Dy)均显示相外磁化率频率依赖性,表明这两个化合物可能具有单链磁体行为。
The synthesis and study of metal complexes with nitronyl nitroxide radical have been one of the most attractive fields in the molecular-based magnetic materials. Focused on this topic, twenty-five new2p-4f and2p-3d-4f complexes have been synthesized by reacting nitronyl nitroxide radicals with metal ions in this work. Their structures have been determined by X-ray crystallographic methods, and they have been characterized by elemental analyses, IR and DC/AC magnetic measurements. Main contents are as follows:
1. By using2-methyl, cyclopropanyl and3-Bromo-4-methoxyphenyl substituted nitronyl nitroxide as ligand. Reaction of the ligands with Ln(hfac)3-2H2O, nine1D chain complexes have been obtained, namely,[Ln(hfac)3(NIT-Me)]n (LnⅢ=Y, Tb, Dy),[Ln(hfac)3(NIT-C3H5)]n (LnⅢ=Gd, Tb) and [Ln(hfac)3(NIT-3BrPhOMe)]n (LnⅢ=Gd, Tb, Dy). The AC magnetic measurements show that complexes [Dy(hfac)3(NIT-Me)]n and [Tb(hfac)3(NIT-C3H5)]n exhibit slow magnetic relaxation in low temperature, suggesting SCM behavior. Complexes [Ln(hfac)3(NIT-3BrPhO Me)]n (LnⅢ=Tb, Dy) exhibit the coexistence of slow magnetic relaxation and antiferromagnetic three-dimensional magnetic ordering.
2. By using benzimidazolyl,2-methyl-benzimidazolyl and4-methoxy-3-pyridine substituted nitronyl nitroxide as ligands. Reaction of the ligands with Ln(tfa)3-2H2O and Ln(hfac)3-2H2O. Nine mononuclear2p-4f compounds have been synthesized. They are Ln(tfa)3(NIT-BzImH)](LnⅢ=Gd, Tb,Dy),[Ln(hfac)3(NIT-BzImCH3)](LnⅢ=Gd, Tb, Y) and [Ln(hfac)3(NIT-3BDOCH3)](LnⅢ=Gd, Tb, Dy). The AC magnetic measurements show that complexes [Ln(tfa)3(NIT-BzImH)](LnⅢ=Tb, Dy),[Tb(hfac)3(NIT-BzImCH3)] and [Tb(hfac)3(NIT-3BDOCH3)] exhibit slow magnetic relaxation in low temperature, suggesting SMM behavior.
3. Using4-propoxyphenyl and4-benzyphenyl substituted nitronyl nitroxide as ligands. Reaction of the ligands with Ln(hfac)3-2H2O and Cu(hfac)2-2H2O at the same time. Six1D2p-3d-4f chains have been synthesized. They are [Ln3Cu(hfac)11(NIT-PhOPr)4]n (LnⅢ=Gd, Tb, Dy), and [Ln3Cu(hfac)11 (NIT-PhOCH2Ph)4]n (LnⅢ=Gd, Tb, Dy)。The AC magnetic measurements show that complexes [Ln3Cu(hfac)11(NIT-PhOPr)4]n(LnⅢ=Tb, Dy) exhibit slow magnetic relaxation in low temperature, suggesting SCM behavior.
1.分别以甲基,环丙烷基,3-溴-4-甲氧基苯基取代氮氧自由基为配体,与稀土的六氟乙酰丙酮盐反应,得到了9个氮氧自由基桥联稀土离子形成的一维链状配合物[Ln(hfac)3(NIT-Me)]n (LnⅢ=Y, Tb, Dy),[Ln(hfac)3(NIT-C3H5)]n (LnⅢ=Gd, Tb)及[Ln(hfac)3(NIT-3BrPhOMe)]n (LnⅢ=Gd, Tb, Dy)。磁性研究表明：配合物[Dy(hfac)3(NIT-Me)]n与[Tb(hfac)3(NIT-C3H5)]n均显示了相外频率依赖性,可能为单链磁体。配合物[Ln(hfac)3(NIT-3BrPhOMe)]n(LnⅢ=Tb, Dy)展示缓慢磁化强度弛豫和三维反铁磁有序共存的现象。
2.以苯并咪唑基,2-甲基苯并咪唑基及4-甲氧基-3-吡啶基取代的功能化氮氧自由基为配体,与稀土三氟取代或六氟取代的乙酰丙酮盐反应,得到9个氮氧自由基-稀土单核配合物[Ln(tfa)3(NIT-BzImH)](LnⅢ=Gd, Tb, Dy),[Ln(hfac)3(NIT-BzImCH3)](LnⅢ=Gd, Tb, Y)与[Ln(hfac)3(NIT-3BDOCH3)](LnⅢ=Gd, Tb, Dy)。磁学性质研究表明,配合物[Ln(tfa)3(NIT-BzImH)](LnⅢ=Tb, Dy),[Tb(hfac)3(NIT-BzlmCH3)]与[Tb(hfac)3(NIT-3BDOCH3)2]相外磁化率显示频率依赖性,表明这几个化合物可能为单分子磁体。
3.分别以4-丙氧基苯和4-苄氧基苯取代的氮氧自由基为桥联配体,同时与Ln(hfac)3·2H2O和Cu(hfac)2反应,合成得到六例2p-3d-4f一维链状配合物[Ln3Cu(hfac)11(NIT-PhOPr)4]n (LnⅢ=Gd, Tb, Dy),和[Ln3Cu(hfac)11(NIT-PhOCH2Ph)4]n (LnⅢ=Gd, Tb, Dy)。AC测量研究表明配合物[Ln3Cu(hfac)11(NIT-PhOPr)4]n (LnⅢ=Tb, Dy)均显示相外磁化率频率依赖性,表明这两个化合物可能具有单链磁体行为。
The synthesis and study of metal complexes with nitronyl nitroxide radical have been one of the most attractive fields in the molecular-based magnetic materials. Focused on this topic, twenty-five new2p-4f and2p-3d-4f complexes have been synthesized by reacting nitronyl nitroxide radicals with metal ions in this work. Their structures have been determined by X-ray crystallographic methods, and they have been characterized by elemental analyses, IR and DC/AC magnetic measurements. Main contents are as follows:
1. By using2-methyl, cyclopropanyl and3-Bromo-4-methoxyphenyl substituted nitronyl nitroxide as ligand. Reaction of the ligands with Ln(hfac)3-2H2O, nine1D chain complexes have been obtained, namely,[Ln(hfac)3(NIT-Me)]n (LnⅢ=Y, Tb, Dy),[Ln(hfac)3(NIT-C3H5)]n (LnⅢ=Gd, Tb) and [Ln(hfac)3(NIT-3BrPhOMe)]n (LnⅢ=Gd, Tb, Dy). The AC magnetic measurements show that complexes [Dy(hfac)3(NIT-Me)]n and [Tb(hfac)3(NIT-C3H5)]n exhibit slow magnetic relaxation in low temperature, suggesting SCM behavior. Complexes [Ln(hfac)3(NIT-3BrPhO Me)]n (LnⅢ=Tb, Dy) exhibit the coexistence of slow magnetic relaxation and antiferromagnetic three-dimensional magnetic ordering.
2. By using benzimidazolyl,2-methyl-benzimidazolyl and4-methoxy-3-pyridine substituted nitronyl nitroxide as ligands. Reaction of the ligands with Ln(tfa)3-2H2O and Ln(hfac)3-2H2O. Nine mononuclear2p-4f compounds have been synthesized. They are Ln(tfa)3(NIT-BzImH)](LnⅢ=Gd, Tb,Dy),[Ln(hfac)3(NIT-BzImCH3)](LnⅢ=Gd, Tb, Y) and [Ln(hfac)3(NIT-3BDOCH3)](LnⅢ=Gd, Tb, Dy). The AC magnetic measurements show that complexes [Ln(tfa)3(NIT-BzImH)](LnⅢ=Tb, Dy),[Tb(hfac)3(NIT-BzImCH3)] and [Tb(hfac)3(NIT-3BDOCH3)] exhibit slow magnetic relaxation in low temperature, suggesting SMM behavior.
3. Using4-propoxyphenyl and4-benzyphenyl substituted nitronyl nitroxide as ligands. Reaction of the ligands with Ln(hfac)3-2H2O and Cu(hfac)2-2H2O at the same time. Six1D2p-3d-4f chains have been synthesized. They are [Ln3Cu(hfac)11(NIT-PhOPr)4]n (LnⅢ=Gd, Tb, Dy), and [Ln3Cu(hfac)11 (NIT-PhOCH2Ph)4]n (LnⅢ=Gd, Tb, Dy)。The AC magnetic measurements show that complexes [Ln3Cu(hfac)11(NIT-PhOPr)4]n(LnⅢ=Tb, Dy) exhibit slow magnetic relaxation in low temperature, suggesting SCM behavior.
引文
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