磺基苯甲酸银配位聚合物的合成、结构和性质研究
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摘要
近年来,配位聚合物由于其新颖的综合性能以及多样性的拓扑网络结构而受到广泛关注,本论文选用Ag(Ⅰ)磺基苯甲酸(sb)类配合物为建筑模块,辅以含氮和／或含磷等中性配体,探索合成具有特殊拓扑结构和导电性能的多功能磺基苯甲酸银配合物,共得到22个未见文献报道的含银配位聚合物和5个非银磺基苯甲酸化合物,解析了全部27个晶体结构,并对它们进行了元素分析、红外光谱、热重分析、荧光以及导电性等性质表征,结合性质和结构的相关性对不同配体对结构和性质的影响进行了研究和讨论。包括：
1.选用邻、间、对磺基苯甲酸为酸性配体结合吡啶类中性配体以及三苯基膦(PPh3),分别得到邻、间、对磺基苯甲酸Ag(Ⅰ)配合物各5个、5个和6个,其中两个对磺基苯甲酸配合物为非常少见的常温原位反应产物,实验证明AgNO3和4,4’—联吡啶(4,4'-bipy)在此原位反应过程中起了不可替代的作用。对此16个配合物进行结构和性能分析表明Ag-Ag,π-π和Ag...π作用在其室温导电性能中作用显著。
2.选用非吡啶类六次甲基四胺(hmt)为中性配体,得到邻、间、对磺基苯甲酸Ag(Ⅰ)配合物各一个,对3个结构进行表征发现,其中两个配合物的基础结构在结合sb配体时发生了构型反转,导致其合成困难；三个结构中Ag-Ag作用的不同存在状态导致其不同的荧光和导电性能。
3.选用三苯基膦和氨基吡啶(apy)/吡啶胺(Hdpa)为中性配体,得到3个双中性配体银配合物,结构分析表明含有PPh3的金属配合物中由于多苯环间作用(PEs)的存在倾向于形成低维结构,各种PEs成为其网络向高维扩展的主要作用,PEs在结构中的不同排列模式导致其不同的性能。
4.研究以上22个磺基苯甲酸银配合物中邻、间、对酸性配体的多样化配位模式及其在整体结构中的不同作用,分析酸性配体和中性配体对结构的共同调控作用,以及不同结构和弱相互作用对结构和性能的影响；结合本论文成果及相关文献探讨银原子三种不同价态下的优势构型。
5.分析5个非银磺基苯甲酸化合物的多样性结构,研究氢键在其结构中的决定性作用以及结构与性能的关系。
Nowadays, coordination polymers have become hot topic of research because of their novel multifunctions and the diverse topological network structures. In this thesis,22 sulfobenzoate-based Ag(I) complexes with N or/and P-donor neutral ligands and 5 non-silver sulfobenzoate (sb) compounds have been prepared to study the special topological networks and the conductivity. All of them were characterized by X-ray single crystal structure analysis, IR, and element analysis. And also the thermal stability behavior, fluorescent emission and conducting behaviors of them have been analyzed. Among them:
1. Five 2-sb, five 3-sb and six 4-sb silver complexes incorporating pyridine or PPh3 netural ligands have been obtained, in which two complexes are rare in situ products. It is confirmed that both AgNO3 and 4,4'-bipy are indispensable in the in situ reaction. The study of the 16 structures and the performances shows that the weak interactions such as Ag-Ag,π-πand Ag…πare important for the conductivity.
2. Three Ag-hmt complexes with sb ligands were synthesized. The structural characterizations find that the configurations in two basic structures have changed, which leads to the difficulties in the process of preparation. The different existing environment of Ag-Ag interactions in the three structures explains their different fluorescent emissions and conducting behaviors.
3. Three silver-sb complexes with two different netural ligands, PPh3 and apy/Hdpa, have been obtained. In the metal-PPh3 complexes, the phenyl embrace interactions (PEs) favor low dimensional structure, which are the main interactions for the strucutral extension, and the different PE arrays bring about different functions.
4. The diversity of the coordination modes and the functions in the whole structures of sb ligands in the 22 silver-sb complexes mentioned above have been studied. The roles of coregulation of sb and neutral ligands in the networks and the influences of different structures and weak interactions on the properties have been analyzed. And also the preferential coordination modes of the three different silver valence state have been investigated.
5. Diversity frameworks of five non-silver sulfobenzoate compounds were analysized and the foundational roles of hydrogen bonds in the networks and property were investigated.
1.选用邻、间、对磺基苯甲酸为酸性配体结合吡啶类中性配体以及三苯基膦(PPh3),分别得到邻、间、对磺基苯甲酸Ag(Ⅰ)配合物各5个、5个和6个,其中两个对磺基苯甲酸配合物为非常少见的常温原位反应产物,实验证明AgNO3和4,4’—联吡啶(4,4'-bipy)在此原位反应过程中起了不可替代的作用。对此16个配合物进行结构和性能分析表明Ag-Ag,π-π和Ag...π作用在其室温导电性能中作用显著。
2.选用非吡啶类六次甲基四胺(hmt)为中性配体,得到邻、间、对磺基苯甲酸Ag(Ⅰ)配合物各一个,对3个结构进行表征发现,其中两个配合物的基础结构在结合sb配体时发生了构型反转,导致其合成困难；三个结构中Ag-Ag作用的不同存在状态导致其不同的荧光和导电性能。
3.选用三苯基膦和氨基吡啶(apy)/吡啶胺(Hdpa)为中性配体,得到3个双中性配体银配合物,结构分析表明含有PPh3的金属配合物中由于多苯环间作用(PEs)的存在倾向于形成低维结构,各种PEs成为其网络向高维扩展的主要作用,PEs在结构中的不同排列模式导致其不同的性能。
4.研究以上22个磺基苯甲酸银配合物中邻、间、对酸性配体的多样化配位模式及其在整体结构中的不同作用,分析酸性配体和中性配体对结构的共同调控作用,以及不同结构和弱相互作用对结构和性能的影响；结合本论文成果及相关文献探讨银原子三种不同价态下的优势构型。
5.分析5个非银磺基苯甲酸化合物的多样性结构,研究氢键在其结构中的决定性作用以及结构与性能的关系。
Nowadays, coordination polymers have become hot topic of research because of their novel multifunctions and the diverse topological network structures. In this thesis,22 sulfobenzoate-based Ag(I) complexes with N or/and P-donor neutral ligands and 5 non-silver sulfobenzoate (sb) compounds have been prepared to study the special topological networks and the conductivity. All of them were characterized by X-ray single crystal structure analysis, IR, and element analysis. And also the thermal stability behavior, fluorescent emission and conducting behaviors of them have been analyzed. Among them:
1. Five 2-sb, five 3-sb and six 4-sb silver complexes incorporating pyridine or PPh3 netural ligands have been obtained, in which two complexes are rare in situ products. It is confirmed that both AgNO3 and 4,4'-bipy are indispensable in the in situ reaction. The study of the 16 structures and the performances shows that the weak interactions such as Ag-Ag,π-πand Ag…πare important for the conductivity.
2. Three Ag-hmt complexes with sb ligands were synthesized. The structural characterizations find that the configurations in two basic structures have changed, which leads to the difficulties in the process of preparation. The different existing environment of Ag-Ag interactions in the three structures explains their different fluorescent emissions and conducting behaviors.
3. Three silver-sb complexes with two different netural ligands, PPh3 and apy/Hdpa, have been obtained. In the metal-PPh3 complexes, the phenyl embrace interactions (PEs) favor low dimensional structure, which are the main interactions for the strucutral extension, and the different PE arrays bring about different functions.
4. The diversity of the coordination modes and the functions in the whole structures of sb ligands in the 22 silver-sb complexes mentioned above have been studied. The roles of coregulation of sb and neutral ligands in the networks and the influences of different structures and weak interactions on the properties have been analyzed. And also the preferential coordination modes of the three different silver valence state have been investigated.
5. Diversity frameworks of five non-silver sulfobenzoate compounds were analysized and the foundational roles of hydrogen bonds in the networks and property were investigated.
引文
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