新型金属—羧基配位扩展结构化合物的合成
摘要
晶体工程学是分子工程学的一个重要组成部分,它涉及分子或化学基团在晶体中的行为、晶体的设计、结构与性能的控制以及晶体结构的预测等,它研究的主要目的在于寻找分子识别和分子组装的规律,从而通过控制构筑单元间相互作用的类型、强度及几何性质来获得具有所希望结构和性能的晶体材料,是实现从分子到材料的一条重要途径。我们从金属-有机配合物晶体材料的新颖结构和自组装规律的角度出发,通过选择合适的金属中心、羧基配体及第二配体,并有目的的调节反应条件,构筑具有新颖拓扑结构和潜在应用价值的新晶体材料,并为这类材料的定向合成提供有价值的实践支持。
本论文致力于通过桥连配体、端基配体与金属离子的协同作用和结构调控,组装一维、二维和三维的新型金属-羧基配位扩展结构晶体材料。
1.在水热体系下,我们合成了两个具有金属-草酸扩展框架结构化合物。我们成功地将有机羧酸配体草酸引入到亚硒酸铟的无机骨架中,得到一个无机-有机杂化的开放结构,这对于进一步扩展无机开放骨架方面的研究,具有一定的指导意义;我们在有机模板剂存在的条件下合成了具有三维扩展骨架结构的草酸铟,并研究了金属铟(III)中心离子的配位方式在不同骨架结构中的变化。
2.我们合成了一系列金属-偶氮羧酸配位化合物,对影响化合物结构的因素进行了比较和探讨,并讨论了化合物中的弱相互作用和缠结网络结构。此外,我们对化合物的磁性质进行了初步研究。我们在水热条件下,合成了8个具有金属-羧基配位扩展结构的化合物。
Crystal engineering is an important part of molecular engineering and is involved with the behavior of molecules or chemical groups within the crystal lattice, the control of crystal design and properties, and the prediction of crystal structure. Recently, the new research fields in the crystal engineering contain inorganic-organic hybrid material, microporous material, molecular magnet and coordination polymers, et al. The research in these areas not only enrich the study of physical laws underlying the assembling processes and experiment of the synthesis chemistry, but also extend the application prospect in the area of electronic, optics, magnetism, catalysis and biology simulation. According to the principle of crystal engineering, it is possible to design and synthesis crystalline material by selecting certain geometric metal ions and special organic ligands. Meanwhile, by selecting functional metal ions and organic ligands with functional groups, crystalline materials with optics, electric, magnetism, resolution of racemates and catalysis can be synthesized. The carboxylate ligand has been widely used in the research of synthesizing new materials for its vast diversity and unusual features in the structure and various coordination modes.
The aim of our work is to design and synthesize a series of metal-carboxyl coordination extended frameworks by selecting suitable ligands and metal ions. This thesis is completed by four chapters.
In the first chapter, the concept and development of crystal engineering is briefly reviewed, with major emphases on the metal-carboxyl coordination extended frameworks, including the histories, new developments and potential applications. Also the goals and achievements of this thesis are summarized.
Among the hybrid compounds there are metal oxalates which exhibit vast diversity and unusual features in structure. A variety of metal oxalates with 1D, 2D and 3D structures have been reported during the past years. The incorporation of the oxalate group in metal-oxo open-frameworks is also of interest because additional structure features may appear after the oxalate incorporation. In Chapter 2, two new indium(III) compounds with extended structures are introduced: [In2(SeO3)2(C2O4)(H2O)2]·2H2O (1) and [NH3(CH2)2NH3][In(C2O4)2]2·5H2O (2). In compound 1, indium-selenite chains are bridged by oxalate units to form two-dimensional (2D) In2(SeO3)2C2O4 layers, separated by non-coordinating water molecules. In compound 2, the indium atoms are connected through the oxalate units to generate a 3D open framework containing cross-linked 12-membered and 8-membered channels.
Azobenzene derivative is a good candidate ligand for its excellent property in many areas such as nonlinear optics, photochromism, photoinduced birefringence, optical switching and image storage. However, reports on azobenzene, especially metal-azobenzene carboxylates are rarely been prepared.
In Chapter 3, a series of 5 trans-ADBbenzene-4,4-dicarboxylic acid (ADB) assembly compounds are introduced: [Zn(ADB)] (3), [Zn(ADB)(phen)] (4), [Co(ADB)(phen)] (5), [In2(ADB)3(phen)2] (6), [Cd(ADB)(phen)]·H2O (7). The strategy is to design low-dimensional structures by appling the“ligand regulation”method and using the bridging ligands and terminal ligands. Compound 3-7 are 1D polymers with differentπ-πstacking interactions, H-bond interactions and different characterized supramolecular frameworks. Compound 3-5 and 7 exhibits zig-zag chains, whereas compound 6 consists of ladder-like chains with left and right-hand helixes combined by ADB ligands. The synthesis and structures are described and the role of factors in packing of molecules are probed.
In Chapter 4, a compound exhibiting fantastic five equivalent interwoven three-dimensional nets is introduced: [Co2(ADB)2(H2O)(phen)2] 8. Two ADB carboxylates and one bridging water molecule bridge the adjacent Co(II) atoms, forming a paddle-wheel Co2(CO2)4(phen)2O motif as secondary building units (SBU). The SBU is further bridged by ADB ligands forming an abnormal 5-fold interpenetration of diamondoid networks. Left- and right-handed helixes, sharing the ADB ligands, have been found in the open frameworks. Characteristic weak overall antiferromagnetic interactions between the metal centers have been observed.
本论文致力于通过桥连配体、端基配体与金属离子的协同作用和结构调控,组装一维、二维和三维的新型金属-羧基配位扩展结构晶体材料。
1.在水热体系下,我们合成了两个具有金属-草酸扩展框架结构化合物。我们成功地将有机羧酸配体草酸引入到亚硒酸铟的无机骨架中,得到一个无机-有机杂化的开放结构,这对于进一步扩展无机开放骨架方面的研究,具有一定的指导意义;我们在有机模板剂存在的条件下合成了具有三维扩展骨架结构的草酸铟,并研究了金属铟(III)中心离子的配位方式在不同骨架结构中的变化。
2.我们合成了一系列金属-偶氮羧酸配位化合物,对影响化合物结构的因素进行了比较和探讨,并讨论了化合物中的弱相互作用和缠结网络结构。此外,我们对化合物的磁性质进行了初步研究。我们在水热条件下,合成了8个具有金属-羧基配位扩展结构的化合物。
Crystal engineering is an important part of molecular engineering and is involved with the behavior of molecules or chemical groups within the crystal lattice, the control of crystal design and properties, and the prediction of crystal structure. Recently, the new research fields in the crystal engineering contain inorganic-organic hybrid material, microporous material, molecular magnet and coordination polymers, et al. The research in these areas not only enrich the study of physical laws underlying the assembling processes and experiment of the synthesis chemistry, but also extend the application prospect in the area of electronic, optics, magnetism, catalysis and biology simulation. According to the principle of crystal engineering, it is possible to design and synthesis crystalline material by selecting certain geometric metal ions and special organic ligands. Meanwhile, by selecting functional metal ions and organic ligands with functional groups, crystalline materials with optics, electric, magnetism, resolution of racemates and catalysis can be synthesized. The carboxylate ligand has been widely used in the research of synthesizing new materials for its vast diversity and unusual features in the structure and various coordination modes.
The aim of our work is to design and synthesize a series of metal-carboxyl coordination extended frameworks by selecting suitable ligands and metal ions. This thesis is completed by four chapters.
In the first chapter, the concept and development of crystal engineering is briefly reviewed, with major emphases on the metal-carboxyl coordination extended frameworks, including the histories, new developments and potential applications. Also the goals and achievements of this thesis are summarized.
Among the hybrid compounds there are metal oxalates which exhibit vast diversity and unusual features in structure. A variety of metal oxalates with 1D, 2D and 3D structures have been reported during the past years. The incorporation of the oxalate group in metal-oxo open-frameworks is also of interest because additional structure features may appear after the oxalate incorporation. In Chapter 2, two new indium(III) compounds with extended structures are introduced: [In2(SeO3)2(C2O4)(H2O)2]·2H2O (1) and [NH3(CH2)2NH3][In(C2O4)2]2·5H2O (2). In compound 1, indium-selenite chains are bridged by oxalate units to form two-dimensional (2D) In2(SeO3)2C2O4 layers, separated by non-coordinating water molecules. In compound 2, the indium atoms are connected through the oxalate units to generate a 3D open framework containing cross-linked 12-membered and 8-membered channels.
Azobenzene derivative is a good candidate ligand for its excellent property in many areas such as nonlinear optics, photochromism, photoinduced birefringence, optical switching and image storage. However, reports on azobenzene, especially metal-azobenzene carboxylates are rarely been prepared.
In Chapter 3, a series of 5 trans-ADBbenzene-4,4-dicarboxylic acid (ADB) assembly compounds are introduced: [Zn(ADB)] (3), [Zn(ADB)(phen)] (4), [Co(ADB)(phen)] (5), [In2(ADB)3(phen)2] (6), [Cd(ADB)(phen)]·H2O (7). The strategy is to design low-dimensional structures by appling the“ligand regulation”method and using the bridging ligands and terminal ligands. Compound 3-7 are 1D polymers with differentπ-πstacking interactions, H-bond interactions and different characterized supramolecular frameworks. Compound 3-5 and 7 exhibits zig-zag chains, whereas compound 6 consists of ladder-like chains with left and right-hand helixes combined by ADB ligands. The synthesis and structures are described and the role of factors in packing of molecules are probed.
In Chapter 4, a compound exhibiting fantastic five equivalent interwoven three-dimensional nets is introduced: [Co2(ADB)2(H2O)(phen)2] 8. Two ADB carboxylates and one bridging water molecule bridge the adjacent Co(II) atoms, forming a paddle-wheel Co2(CO2)4(phen)2O motif as secondary building units (SBU). The SBU is further bridged by ADB ligands forming an abnormal 5-fold interpenetration of diamondoid networks. Left- and right-handed helixes, sharing the ADB ligands, have been found in the open frameworks. Characteristic weak overall antiferromagnetic interactions between the metal centers have been observed.
引文
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[1] Volkringer, C., Loiseau, T., Marrot, J., etc., A MOF-type magnesium benzene-1,3,5-tribenzoate with two-fold interpenetrated ReO3 nets[J]. CrystEngComm, 2009, 11 (1): 58-60.
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