磁性功能配合物的设计，合成，表征与性质研究

【作者】 刘波；

【导师】 鲁晓明；

【作者基本信息】 首都师范大学 ， 物理化学， 2006， 硕士

【摘要】 本论文的研究内容主要以草酸根为桥联配体，邻菲罗林为终端配体，选择合适的中心金属离子进行反应，合成了Cu（H₂O）（phen）（ox）.H₂O,Fe（H₂O）₃（phen）SO₄,{[Mo（phen）₃][MoNa（ox）₃]}_n（phen=1,10-phenanthroline,ox=oxalate）,{[Fe（phen）₃][FeNa（ox）₃]}_n四种配合物，并且通过红外，元素分析，顺磁，扫描电镜，透射电镜以及X单晶衍射实验的表征。在这篇论文中，两种类型的材料被研究，第一类是通过π-π相互作用和氢键作用堆积而成的，另一类是完全由共价键构建的主-客体结构。 对于第一类型配合物，通过水热反应合成了Cu（H₂O）（phen）（ox）.H₂O和，Fe（H₂O）₃（phen）SO₄两种配合物，并对这两种配合物进行了一系列的红外，元素分析，顺磁，扫描电镜以及X单晶衍射实验的表征。第一类型的配合物通过π-π相互作用和氢键作用堆积而成，这导致有机-无机层的交替排列。分子内氢键在同一无机层中连接毗邻的配合物分子，而在有机层中由相邻层中的芳香体系产生的π-π相互作用把无机层联系在一起。 对于第二类型配合物，通过水热反应制备了[Mo（phen）₃][MoNa（ox）₃]}_n（phen=1,10-phenanthroline,ox=oxalate）,{[Fe（phen）₃][FeNa（ox）₃]}_n两种配合物。在第二类型配合物中，主-客体超分子配合物显示具有纳米尺寸的孔洞。主体分子完全由共价键构建，具有传统渗水材料所不具有的稳定性。同时，填充在主体分子孔洞中的客体分子的直径也在纳米级，这对配合物起到进一步的稳定作用。 通过，单晶衍射，SEM，TEM的表征，两种类型的配合物的微观结构与宏观结构在几何上也具有一致性。更多还原

【Abstract】 In this paper, we choice oxalate as bridged ligands, 1,10-phenanthr as terminal ligands, transition metal ion as reaction center to synthesis new complexes. Cu（H₂O）（phen）（ox）.H₂O, {[Mo（phen）₃][MoNa（ox）₃]}_n （phen=1,10-phenanthroline, ox=oxalate）, Fe（H₂O）₃（phen）SO₄, {[Fe（phen）₃][FeNa（ox）₃]}_n, were synthesized and characterized by IR, EA, EPR, SEM, TEM and X-ray diffraction analysis. In my work, two kinds of nanoporous materials are studied, one is honst-guest structure architected fully by covalent bonds, and the other is constructed by inter-molecular interactions, including inter-molecular H-bonds and π-π interaction.For the first model complexes, Cu（H₂O）（phen）（ox）.H₂O, Fe（H₂O）₃（phen）SO₄ were obtained by hydro-thermal reaction. A series of characterizations of IR, XPS, SEM and X-ray diffraction determine the molecular structure. The complexes pile together by inter-molecular H-bonds and π-π interaction, which results in organic-inorganic layers arranging alternately. Inter-molecular H-bonds link the adjacent molecular within inorganic layers, while in organic layers, π-π interaction from aromatic rings connect adjacent inorganic layers.For the other model complexes, {[Mo（phen）₃][MoNa（ox）₃]}_n （phen=1,10-phenanthroline, ox=oxalate）, Fe（H₂O）₃（phen）SO₄, {[Fe（phen）₃][FeNa（ox）₃]}_n,were synthesized and characterized by IR, EA, EPR, SEM, TEM and X-ray diffraction analysis. In first type, host-guest supra-molecular complex shows cavities with nano size. The framework was constructed fully by covalent bonds, which possesses certain stability. Meanwhile, guest molecule with diameter close to 1nm occupied the cavities, which further improve the stability.By the means of SEM, TEM, the relationship between micro- and macro structure was studied. We found that geometry of micro- and macrostructure were coherent.更多还原