含N，O配体的过渡金属配合物的控制合成与性质研究
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摘要
本学位论文主要研究对象为分别由两种配体：Schiff碱和芳香多羧酸构成的配合物的合成与性质研究。特别之处在于，Schiff碱配合物中配体的结构因发生了C-N键的重建而改变，配体与金属离子间的配比变化也使所得的配合物显现了不同的自组装结构。同时，描述了影响配合物结构的反应因素。根据内容，本文共分4章。
第一章主要介绍了本研究的背景，特别讲述了配位化合物的应用及其在合成方面的影响因素。重点强调了Schiff碱配合物在生物应用上的意义和羧酸配合物的发光功能性质。最后，对本论文选题意义做出陈述。
第二章介绍了五个二价金属配合物的合成与性质。配合物1-5的三种不同Schiff碱配体分别用H2_L1，H_2L2和HL3表示。通过两种合成方法：水(溶剂)热法和溶液法，我们得到了这5个配合物的晶体：[Zn(L1)(H_2O)](1)、[Co(L1)](2)、[Cu(L1)](3)、[Ni_2(L2)Cl_2](4)和[NiL3]Cl·H_2O(5)。单晶X-射线衍射表明配合物1-3和配合物5是简单的单核配合物，配合物4是双核配合物。产物中配体的结构都发生了多胺的重构现象：配体H_2L01中发生-C-N-断裂生成配体H_2L1，配体H_2L02中发生-C-N-加合生成配体H_2L2，配体H_3L03中发生重排生成配体HL3。比较配合物1-4与配合物5的合成条件，可以得出出现这一现象的原因是由于合成过程中加热条件的影响所导致的。
第三章介绍了混合配体与二价金属配合物的合成与性质。通过完全相同的合成条件我们得到了分别以间苯二甲酸(H_2BDA)、均苯三酸(H_3BTA)、4，4’-联吡啶(Bpy)和3，5—二甲基吡唑(pz)为配体的6个聚合物：[Cu_6(BDA)_2(2-oxo-BDA)_2(Bpy)_2O_2]_n(6)、[Cu(HBDA)_2(Bpy)]_n(7)、[Zn(BDA)(pz)_2]_n(8)、{[Zn_3(BTA)_2(pz)_6]·2H_2O}_n(9)、[Cd(BDA)(pz)_2]_n(10)、[Co(BDA)(pz)_2]_n(11)和一个单核配合物[Mn(BDA)(pz)_4](12)。其中，6，7是以间苯二甲酸和4，4’-联吡啶为配体，配合物8-12是以间苯二甲酸(均苯三酸)和3，5-二甲基吡唑为配体。单晶X-射线衍射表明除配合物6为二维聚合物配合物12为单核配合物之外，配合物7-11都是一维配位聚合物且都具有[M(pz)_2]这一第二结构单元。在研究合成配合物8-12的过程中，所加入的两种配体间配比以及配体与金属盐之间的配比也影响着是否能够合成目标产物。
第四章对全文的实验结果做以总结，分析了在合成配合物过程中影响金属配合物结构的重要因素：温度，第二配体以及配体与金属之间配比。
This dissertation focuses on the synthesis and solid properties of bivalent metal complexesderived from the ligands of sorts as Schiff bases and aromatic carboxylic acids. Of particular, thestructures of complexes of Schiff base ligands, demonstrating unusual C-N bond reconstructionand those of carboxylic acids, presenting intriguing self-assembly scheme of metal ion andligands are discussed in detail. Meanwhile, the effects of reaction parameters on structure ofcomplexes are described. According to the contents, the thesis is divided into four chapters asfollows.
Chapter 1 was elucidated mainly the background of this research, especially the aspects ofsynthesis and applications of coordination compounds. Stress of the section was placed on theintroduction to biomimic significance of Schiff base complexes and luminous functionality ofcarboxylic acid complexes. Finally, the consideration why we choose the field as topic of mythesis is presented.
Chapter 2 reports the synthesis of five bivalent complexes, 1-5 of three diverse Schiff baseligands that are denoted as H_2L1, H_2L2 and HL3(see abbreviation). The metal complexes wereisolated as crystals by two methods, specifically, hydrothermal and ambient solution reactions.X-Ray single-crystal diffraction revealed that complexes, 1-3 and 5 are mononuclear and 4 ismultinuclear. Structures of these products indicate that the ligands are in-situ generated fromreconstruction of polyamines. In particular, the formation of H_2L1 and HL3 show the C-N bondcleavage and H_2L2 show the C-N bond formation. Comparing the synthesis conditions ofcomplexes 1-4 with that of 5, we believe that the reconstruction of polyamine is caused byheating.
Chapter 3 describes the synthesis and structures of complexes with mixed ligands. Totally sixnovel coordination polymers, [Cu_6(BDA)_2(2-oxo-BDA)_2(Bpy)_2O_2]_n(6), [Cu(HBDA)_2(bpy)]_n(7),[Zn(BDA)(pz)_2]_n(8), {[Zn_3(BTA)_2(pz)_6]·2H_2O}_n (9), [Cd(BDA)(pz)_2]_n(10), [Co(BDA)(pz)_2]_n(11)and a monomer[Mn(BDA)(pz)_4](12), were included in the section, of which 6 and 7 arederived from bpy and H_2BDA and 8-12 from pz and H_2BDA (or H_3BTA). Their crystalstructures were determined by single-crystal X-ray diffraction, revealed that all the complexes,except for 6 in 2-D sheet and 12 in 0-D monomer, are structured in 1D chains and they have the[M(pz)_2] as second building blocks. Generation of 8-12 proves that the proportion of ligands andmetal salt affects the structures of the complexes.
Chapter 4 as summarization of the results of experiments describes the important factorsinfluencing the construction of metal complexes, such as temperature, second ligand andproportion of ligands and metal salt.
第一章主要介绍了本研究的背景，特别讲述了配位化合物的应用及其在合成方面的影响因素。重点强调了Schiff碱配合物在生物应用上的意义和羧酸配合物的发光功能性质。最后，对本论文选题意义做出陈述。
第二章介绍了五个二价金属配合物的合成与性质。配合物1-5的三种不同Schiff碱配体分别用H2_L1，H_2L2和HL3表示。通过两种合成方法：水(溶剂)热法和溶液法，我们得到了这5个配合物的晶体：[Zn(L1)(H_2O)](1)、[Co(L1)](2)、[Cu(L1)](3)、[Ni_2(L2)Cl_2](4)和[NiL3]Cl·H_2O(5)。单晶X-射线衍射表明配合物1-3和配合物5是简单的单核配合物，配合物4是双核配合物。产物中配体的结构都发生了多胺的重构现象：配体H_2L01中发生-C-N-断裂生成配体H_2L1，配体H_2L02中发生-C-N-加合生成配体H_2L2，配体H_3L03中发生重排生成配体HL3。比较配合物1-4与配合物5的合成条件，可以得出出现这一现象的原因是由于合成过程中加热条件的影响所导致的。
第三章介绍了混合配体与二价金属配合物的合成与性质。通过完全相同的合成条件我们得到了分别以间苯二甲酸(H_2BDA)、均苯三酸(H_3BTA)、4，4’-联吡啶(Bpy)和3，5—二甲基吡唑(pz)为配体的6个聚合物：[Cu_6(BDA)_2(2-oxo-BDA)_2(Bpy)_2O_2]_n(6)、[Cu(HBDA)_2(Bpy)]_n(7)、[Zn(BDA)(pz)_2]_n(8)、{[Zn_3(BTA)_2(pz)_6]·2H_2O}_n(9)、[Cd(BDA)(pz)_2]_n(10)、[Co(BDA)(pz)_2]_n(11)和一个单核配合物[Mn(BDA)(pz)_4](12)。其中，6，7是以间苯二甲酸和4，4’-联吡啶为配体，配合物8-12是以间苯二甲酸(均苯三酸)和3，5-二甲基吡唑为配体。单晶X-射线衍射表明除配合物6为二维聚合物配合物12为单核配合物之外，配合物7-11都是一维配位聚合物且都具有[M(pz)_2]这一第二结构单元。在研究合成配合物8-12的过程中，所加入的两种配体间配比以及配体与金属盐之间的配比也影响着是否能够合成目标产物。
第四章对全文的实验结果做以总结，分析了在合成配合物过程中影响金属配合物结构的重要因素：温度，第二配体以及配体与金属之间配比。
This dissertation focuses on the synthesis and solid properties of bivalent metal complexesderived from the ligands of sorts as Schiff bases and aromatic carboxylic acids. Of particular, thestructures of complexes of Schiff base ligands, demonstrating unusual C-N bond reconstructionand those of carboxylic acids, presenting intriguing self-assembly scheme of metal ion andligands are discussed in detail. Meanwhile, the effects of reaction parameters on structure ofcomplexes are described. According to the contents, the thesis is divided into four chapters asfollows.
Chapter 1 was elucidated mainly the background of this research, especially the aspects ofsynthesis and applications of coordination compounds. Stress of the section was placed on theintroduction to biomimic significance of Schiff base complexes and luminous functionality ofcarboxylic acid complexes. Finally, the consideration why we choose the field as topic of mythesis is presented.
Chapter 2 reports the synthesis of five bivalent complexes, 1-5 of three diverse Schiff baseligands that are denoted as H_2L1, H_2L2 and HL3(see abbreviation). The metal complexes wereisolated as crystals by two methods, specifically, hydrothermal and ambient solution reactions.X-Ray single-crystal diffraction revealed that complexes, 1-3 and 5 are mononuclear and 4 ismultinuclear. Structures of these products indicate that the ligands are in-situ generated fromreconstruction of polyamines. In particular, the formation of H_2L1 and HL3 show the C-N bondcleavage and H_2L2 show the C-N bond formation. Comparing the synthesis conditions ofcomplexes 1-4 with that of 5, we believe that the reconstruction of polyamine is caused byheating.
Chapter 3 describes the synthesis and structures of complexes with mixed ligands. Totally sixnovel coordination polymers, [Cu_6(BDA)_2(2-oxo-BDA)_2(Bpy)_2O_2]_n(6), [Cu(HBDA)_2(bpy)]_n(7),[Zn(BDA)(pz)_2]_n(8), {[Zn_3(BTA)_2(pz)_6]·2H_2O}_n (9), [Cd(BDA)(pz)_2]_n(10), [Co(BDA)(pz)_2]_n(11)and a monomer[Mn(BDA)(pz)_4](12), were included in the section, of which 6 and 7 arederived from bpy and H_2BDA and 8-12 from pz and H_2BDA (or H_3BTA). Their crystalstructures were determined by single-crystal X-ray diffraction, revealed that all the complexes,except for 6 in 2-D sheet and 12 in 0-D monomer, are structured in 1D chains and they have the[M(pz)_2] as second building blocks. Generation of 8-12 proves that the proportion of ligands andmetal salt affects the structures of the complexes.
Chapter 4 as summarization of the results of experiments describes the important factorsinfluencing the construction of metal complexes, such as temperature, second ligand andproportion of ligands and metal salt.
引文
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