摘要
由于在光学、电学、磁学、分子识别和催化等领域里具有巨大的应用潜力,设计合成新型功能超分子化合物是当今配位化学、超分子化学、晶体工程学等领域的研究热点之一。本论文选择含碘刚性羧酸配体及自行设计合成了一系列柔性二羧酸配体,通过与d10过渡金属离子和稀土离子自组装,合成了三个系列共17个不同维度的超分子化合物,并通过X-射线单晶衍射、元素分析、X-射线粉末衍射、热重分析、荧光分析等技术对它们进行了表征。全文共分为五章,各章内容如下：
第一章前言,简单介绍了配位化学、晶体工程学、超分子化学、配位聚合物等基本概念和原理,主要合成方法等。有选择性的重点描述了配位聚合物发展的新方向及新思路。
第二章中,首先设计合成了六个具有合适角度的柔性二羧酸配体(H2L1～H2L4, H2L9, H2L10),通过它们与过渡金属离子、稀土金属离子的自组装,得到九个金属—有机超分子配合物Cd2(L1)2(DMF)4(H2O)2-H2O(1), Tm2(L1)2(DMF)4(NO3)2(2), Cu4(L3)4(H2O)4·3DMF (3), Cu4(L4)4(DMF)2-(EtOH)2-8DMF-6H2O(4), Mn4(L4)4(DMF)4(H2O)4·6DMF·H2O(5), Mn3(L4)3-(DMF)4-2DMF-3H2O(6), [Zn(L9)(phen)]-4H2O(7), (H2O)2]-2H2O-2EtOH(8)和Mn3(1L2)2(2L2)(DMF)2(H2O)2·5DMF (9)。通过X-射线单晶衍射结构分析得到单晶结构分别为零维金属—有机大环,零维金属—有机配位笼和一维/二维配位聚合物。在零维环状或笼状结构中,柔性配体采取顺式构象,而在一维或者二维结构中,柔性配体采取反式构象或者同时采取顺式与反式两种构象。
第三章的目标是通过设计改变柔性羧酸配体中羧酸官能团的位置,研究柔性配体中配位基团的取代位置对超分子化合物结构的影响。继续合成了H2L6-H2L8配体,通过它们与金属Cu2+离子自组装,得到了四个基于轮状铜次级构筑单元的金属—有机超分子化合物10-13：配合物Cu2(L6)2(DMF)2·2DMF·H2O(10)和Cu2(L7)2(DMF)2·2DMF(11)是零维分子椅；配合物Cu2(L7)2(bpy)·2DMF·H2O(12)是分子椅构筑的一维链状结构(通过加入4,4'-bipy配体,把零维分子椅连接形成一维结构)；配合物Cu2(L8)2(DMF)2·DMF·H2O(13)是含有68元金属有机大环的二维波浪状层状物。在分子椅结构中,配体采取顺式构象,在二维结构中,配体采取反式构象。
第四章中,使用刚性含碘羧酸配体H2atiip与锌离子或者镉离子自组装得到了四个一维超分子配合物(14～17):[Zn(atiip)(bpy)·3H2O] (14,15), [Cd(atiip)(Im)2] (16, Im=imidazole,咪唑)和[Cd(atiip)(DMF)](17)。配合物14和15是一维金属—有机纳米管,且两者互为超分子异构体；配合物16是一维之字链；配合物17是一维手性螺旋链,通过加入手性诱导剂,实现了手性突破。
第五章中,我们做出了总结与展望。
The design and synthesis of new functional metal-organic supramolecular complexes in coordination chemistry, supramolecular chemistry, crystal engineering is one of the active research fields in recent years, due to their special properties in new topology, photoelectricity, magnetism, molecular recognition and catalysis etc. In this thesis, we try to synthesize novel coordination complexes by use of flexible and rigid dicarboxylate ligands to assemble with transitional metal ions or rare-earth metal ions. The assembly of dicarboxylate with metal ions yielded 17 novel metal-organic complexes. All complexes have been determined by single-crystal X-ray diffraction、elemental analyses、XRPD analysis、thermal analysis and fluorescence spectroscopy. There are following five chapters:
In chapter i:A brief introduction of the coordination chemistry, crystal engineering, supramolecular chemistry, coordination polymers and other basic concepts and principles. Selective focus on the development of coordination polymers described in a new direction and new ideas.
The chapter ii:First designed and synthesized the flexible dicarboxylate ligand (H2L1～H2L4, H2L9, H2L10) with the right angle, by their self-assembly with transition metal ions, we have got nine metal organic complexes: Cd2(L1)2(DMF)4(H2O)2-H2O(2), Tm2(L1)2(DMF)4(NO3)2(2), Cu4(L3)4(H2O)4-3DMF(3), Cu4(L4)4(DMF)2(EtOH)2·8DMF·6H2O(4), Mn4(L4)4(DMF)4(H2O)4·6DMF·H2O(5), Mn3(L4)3(DMF)4·2DMF·3H2O(6), [Zn(L9)(phen)]·4H2O(7), [Zn4(L10)3(μ3-OH)2(H2O)2]·2H2O·2EtOH(8)和Mn3(1L2)2(2L2)(DMF)2(H2O)2·5DMF(9). X-ray diffraction structure analysis showed they were zero-dimensional crystal structure of metal organic macrocycle, zero-dimensional metal-organic coordination cage and one- / two-dimensional coordination polymer. In the zero-dimensional ring or cage-like structure, flexible ligand adopted cis-configuration, but in the one-dimensional or two-dimensional structure, the flexible ligand adopted the trans configuration or both cis- and trans configurations.
In chapter iii:By changing the positions of the functional groups, there continually synthesized H2L6～H2L8 ligand, the positions of the functional SBUstituents in the central benzene ring change gradually from 1,2-,1,3- to 1,4-position. By applying these flexible ligands to assemble with copper ions, four metal-organic supramolecules (10-13) based on paddlewheel SBU have been isolated. Complexes 10 and 11 are discrete molecular chairs. Complex 12 is a 1D molecular-chair-based coordination polymer. The molecular chairs, similar to that found in 10 and 11, are infinitely connected by the bridging 4,4' -bipy ligands to result in the formation of the 1D chain structure. Complex 13 is a two-dimensional wavelike layer structure containing 68-membered ring. Both L6 and L7 in 10 and 11 adopt cis, cis conformation, while L8 adopts cis, trans conformation, which results in the formation of the 2D layer structure of complex 13.
In chapter iv, The assembly of iodine-based rigid dicarboxylate ligands H2atiip with zinc or cadmium ion, there are isolated four one-dimensional coordination complexes (14-17):[Zn(atiip)(bpy)·3H2O] (14,15), [Cd(atiip)(Im)2] (16), [Cd(atiip)(DMF)] (17) (Im=imidazole). Complexes 14 and 15 are one-dimensional metal-organic nanotubes, which are supramolecular isomers, complex 16 is a non-chiral zigzag chain, complexes 17 are one-dimensional chiral helical chains(by adding chiral inducer).
In chapter v, The conclusions and prospects.
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