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摘要：本文在水热条件下合成出了两种具有新颖结构的基于金属-氧簇和过渡金属配合物的新型材料：[CuCl(Phen)(H2O)][PW12O40][4,4′-H2bpy]·1.5H2O (1) 和 (4,4′-H2bpy){[Cu(4,4′-bpy)]2[SiW12O40]} (2) (Phen = 1,10-邻菲罗啉，bpy=吡啶)。由单晶结构分析可以看出，化合物1是由游离的双质子化的[4,4′-H2bpy]2+、Keggin型钨-氧簇阴离子[PW12O40]3- (POM)、过渡金属配离子[CuCl(Phen)(H2O)]+ 和水分子组成的。通过金属-氧簇阴离子和过渡金属配离子的相互作用，化合物1组合了一种一维链状结构。化合物2是由两个过渡金属配离子[Cu(4,4-bpy)]+，一个Keggin型钨-氧簇阴离子[SiW12O40]4−和一个双质子化的 4,4′-H2bpy组成的。化合物2在金属-氧簇阴离子以及过渡金属配离子的两者的相互作用下形成了一维链状结构，这些一维链又在氢键的作用下形成了三维超分子网络结构。探究了反应所需要的温度、酸碱度和反应时间对生成物的影响。然后对化合物进行了红外、X-射线单晶衍射、紫外以及元素分析，为更加深入的探索多酸的性能与结构的联系奠定了基础。50539
毕业论文关键词：金属-氧簇；水热合成；晶体结构
Structure Characterization and Syntheses of New Materials Based on POMs and Transition Metal Coordination Complexes
Abstract: Two new new materials based on POMs and transition metal coordination complexes have been successfully hydrothermal synthesized: [CuCl(Phen)(H2O)][PW12O40][4,4′-H2bpy]·1.5H2O (1) and (4,4′-H2bpy) {[Cu(4,4′-bpy)]2[SiW12O40]} (2). Single crystal analysis reveals that compound 1 is consists of Keggin W-O cluster anion [PW12O40]3- (POM), dissociated 4,4’-bpy moiety, water molecules and transition metal complex [CuCl(Phen)(H2O)]+. Compound 1 presents a 1-D chain structure constructed from polyoxometalates (POMs) and transition metal complexes. Compound 2 contains a dissociated 4,4’-bpy moiety, two transition metal complexes [Cu(4,4-bpy)]+ and a Keggin polyoxoanion [SiW12O40]4−. Compound 2 exhibits an infinite 1-D ladder like structure through interactions between POMs and transition metal coordination complexes, which is further interconnected into a new 3-D supramolecular framework through hydrogen bonding interactions. The reaction temperature, pH value and reaction time on the influence of the products were studied. The compounds have been characterized by IR, UV-Vis, X-ray structural analyses,and elemental analysis, which provide basis in the explorations of structures and functions for the compounds.
Key Words: POMs; Hydrothermal synthesis; Crystal Structures
目 录
摘 要 1
引 言 2
1 实验部分 3
1.1 仪器与试剂 3
1.2 实验方法 4
2 结果与讨论 5
2.1 化合物的结构分析 5
2.2 化合物的表征 9
3 结论 11
参考文献 11
致 谢 13
基于金属氧簇和过渡金属配合物的新型材料的水热合成与晶体结构
引 言
金属-氧簇又称多金属氧酸盐，简称POMs，它有六种基本的结构。从POMs应用性的广泛角度来讲多金属氧酸盐中含V、Mo和W的应用是比较广泛的。例如可以被用在分析、催化、光化学、临床医学、生物化学等方面。由于金属-氧簇具有广泛的用途，所以此类化合物逐渐受到的人们的广泛关注，现在它的组成元素已经扩展到元素周期表中的几十种元素了[1-4]。