基于苯多酸配体的金属有机配合物的合成及其性能研究
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摘要
近年来,利用过渡金属或稀土金属离子与具有多官能团的有机配体,通过配位键驱动自组装得到配位化合物一直是超分子化学研究中的活跃领域。由于配位化合物在光电、磁性、氧化还原催化、离子交换、气体吸附、分离纯化、分子识别等方面具有广泛的应用,配位化学家和晶体工程学家致力于配位化合物的设计和合成,筛选出一些良好的特殊功能材料,并且发现了许多新颖的拓扑结构类型,同时掌握了一些自组装过程中影响化合物最终结构的因素,如溶剂、配体构型、温度等,以期达到控制合成的目的。
在过去的几十年中,共平面的羧酸类配体由于强的配位能力以及配位的多样性在晶体构筑过程中被广泛应用。研究表明,配体的构型和金属离子的配位模式对晶体结构有重要影响,对配体结构的简单修饰即可改变自组装产物的结构。本论文选用一系列具有空间位阻效应的非共面羧酸为主配体,掺杂咪唑类、吡啶类、或螯合的邻菲啰啉配体作为辅助配体,通过配位键或超分子弱作用与金属离子组装合成新颖的配位化合物,进一步探讨了各种因素对化合物最终结构的影响,并测定了它们的气体吸附、荧光等性能。主要做了以下工作：综述了羧酸的配位化学,以羧酸配体为主与过渡金属或稀土金属离子在水／溶液热条件下组装合成了14个新颖的配位化合物：Cu4(OH)2(SO4)(HBTC)2(bpy)·bpy(1)、Cu1.5(H2O)(TMBTC)(bpy)·0.5H2O (2)、Cd2(H2O)5(TMBTC)(bpy)2·NO3·3H2O (3)、Ni(BITMB)(TMIPA)·2H2O (4)、Zn(BITMB)(IPA)·H2O (5)、Zn2(BITMB)2(HIPA)2(IPA)·H2O(6)、Zn(TBDC1)0.5(TBDC2)0.5 (7)、Er(BDC)1.5(dmf)(H2O) (8)、Tm(BDC)1.5(dmf)(H2O) (9)、Er2(BDC)3(phen)2·3H2O (10) Tm(TBDC)1.5(dmf)(H2O)·2H2O (11)、Er2(TBDC)3(phen)2·4dm·2H2O (12)、Tm(BDC)1.5(H2O)·0.5dmf-C2H5OH·2H2O (13) Tm4(BDC)6(H2O)2(dmf)2·4dmf·2H2O (14)。
单晶X-射线衍射分析表明：化合物1为三维三重穿插结构；化合物2为三维二重穿插结构、3为三维结构、4为一维链状结构、5为二维层状穿插结构、6为三维孔道结构、7是基于二核SBU构筑的三维(3,5)-连接拓扑网络结构、8和9均属于三维二重穿插结构、10-14属于三维非穿插网状结构。其中,化合物1和2是利用共面的和非共面的羧酸配体而得到不同的结构；化合物4、5、6是利用一种具有顺式-或反式-结构的咪唑类柔性配体,通过溶剂或金属控制得到配体构型和维度均不相同的化合物；化合物7通过粉末衍射证实,可通过二维双层状结构MOF-47直接转换获得；化合物8、9为异质同晶结构；化合物10-12是利用空间位阻效应得到的非穿插的镧系金属有机框架物；化合物13-14则是利用一维棒状单元组装得到的非穿插微孔金属有机框架物。同时,对化合物3、5-7做了固态荧光谱学的测试,化合物12-14做了气体吸附性质的测试,化合物1-8、12、13做了热重测试分析。
以上金属-有机配合物不仅为超分子及金属-有机复合材料化学增添了新的内容,而且为寻找、筛选金属-有机复合材料提供了新的途径。
Investigation on the coordination complexes constructed by transition metals or lanthanide ions and ligands with muti-functional groups through coordinative bonds is an active research field in recent years. Due to the wide applications of coordination complexes in photoelectricity, magnetic material, redox catalysis, ion exchange, adsorption, separation, and molecular recognition etc., much attention has been devoted to the design and synthesis of novel kinds of structural topologies and compounds with special properties. It is important to master the factors influencing the structure of the coordination complex, such as solvent, conformations of ligands and temperature etc., so that we can control the formation of the complexes.
In the past several decades, planar carboxylate ligands have been widely studied because of their strong coordination ability and varieties of coordination modes. As known, the ligand conformation and coordination geometries of the metal ion have signifinant influence on the final structures of a MOF, and a little change of the ligand may result in new topological complexes. In this thesis, we try to synthesize novel coordination complexes by the use of carboxylic acids or combination with imidazole/pyridine/phenanthroline ligands assembling with metal ions through coordinative bonds or supramolecular weak interactions and to study the factors influencing the final structures and properties. The coordination chemistry of carboxylate ligands has been reviewed. The assembly reactions of rigid benzene-muti-carboxylate and and N-donor ligands with metal ions have yielded 14 novel coordination complexes: Cu4(OH)2(SO4)(HBTC)2(bpy)·bpy (1), Cu1.5(H2O)(TMBTC)(bpy)·0.5H2O (2), Cd2(H2O)5(TMBTC)(bpy)2·NO3·3H2O (3), Ni(BITMB)(TMIPA)·2H2O (4), Zn(BITMB)(IPA)·H2O (5), Zn2(BITMB)2(HIPA)2(IPA)·H2O(6), Zn(TBDC1)0.5(TBDC2)0.5 (7), Er(BDC),.5(dmf)(H2O) (8), Tm(BDC)1.5(dmf)(H2O) (9), Er2(BDC)3(phen)2-3H2O (10), Tm(TBDC)1.5(dmf)(H2O)·2H2O (11), Er2(TBDC)3(phen)2·4dmf-2H2O (12), Tm(BDC)1.5(H2O)0.5dmf·C2H5OH·2H2O (13), Tm4(BDC)6(H2O)2(dmf)2·4dmf·2H2O (14).All complexes have been determined by single-crystal X-ray diffraction. Complex 1 is three-dimensional three-fold interpenetrated complex; complexes 2 possesses three-dimensional two-fold interpenetrated structure; complexes 3 belongs to three-dimensional architecture; complexes 4 is one-dimensional chain; complex 5 belongs to two-dimensional interpenetrated layers; complexes 6 is three-dimensional porous framework; complexes 7 possesses three-dimensional framework with a rare (3,5)-connected net based on a dinuclear SBU; complex 8 and 9 are both three-dimensional structures with two-fold interpenetrating nets; complexes 10-14 belong to three-dimensional non-interpenetrated lanthanide-organic framework. In complexes 1 and 2, the different geometries of the carboxylate ligands (planarity and nonplanarity) induced two different assembly units. The flexible BITMB adopts syn or anti conformations in the complexes 4,5,6 which can be controlled by the presence or lack of water in the reaction, moreover, the dimensionality of the product can be controlled by the ligand conformation of BITMB. Complex 7 can be transformed from a previously reported 2D double layer (MOF-47) by liberating the coordinated water and dmf molecules, which was confirmed by X-ray powder diffraction. Complexes 8 and 9 are isostructural; complexes 10-12 apply organic ligands containing large hindrance groups to prevent the formation of interpenetration; while complexes 13-14 use in-situ reactions generated rod-shaped SBUs to improve final framework, with non-interpenetrated porous nets. Complexes 3,5-7 have been characterized by fluorescent spectra and gas sorption studies have been done for complexes 12-14; complexes 1-8,12 and 13 have been measured by TGA.
The results reported herein demonstrate that the use of non-plannar polybenzenecarboxylate ligands as precursors to bind transition metal or lanthanide metal ions, is a new approach for the formation of novel supramolecular networks with interesting physical properties.
在过去的几十年中,共平面的羧酸类配体由于强的配位能力以及配位的多样性在晶体构筑过程中被广泛应用。研究表明,配体的构型和金属离子的配位模式对晶体结构有重要影响,对配体结构的简单修饰即可改变自组装产物的结构。本论文选用一系列具有空间位阻效应的非共面羧酸为主配体,掺杂咪唑类、吡啶类、或螯合的邻菲啰啉配体作为辅助配体,通过配位键或超分子弱作用与金属离子组装合成新颖的配位化合物,进一步探讨了各种因素对化合物最终结构的影响,并测定了它们的气体吸附、荧光等性能。主要做了以下工作：综述了羧酸的配位化学,以羧酸配体为主与过渡金属或稀土金属离子在水／溶液热条件下组装合成了14个新颖的配位化合物：Cu4(OH)2(SO4)(HBTC)2(bpy)·bpy(1)、Cu1.5(H2O)(TMBTC)(bpy)·0.5H2O (2)、Cd2(H2O)5(TMBTC)(bpy)2·NO3·3H2O (3)、Ni(BITMB)(TMIPA)·2H2O (4)、Zn(BITMB)(IPA)·H2O (5)、Zn2(BITMB)2(HIPA)2(IPA)·H2O(6)、Zn(TBDC1)0.5(TBDC2)0.5 (7)、Er(BDC)1.5(dmf)(H2O) (8)、Tm(BDC)1.5(dmf)(H2O) (9)、Er2(BDC)3(phen)2·3H2O (10) Tm(TBDC)1.5(dmf)(H2O)·2H2O (11)、Er2(TBDC)3(phen)2·4dm·2H2O (12)、Tm(BDC)1.5(H2O)·0.5dmf-C2H5OH·2H2O (13) Tm4(BDC)6(H2O)2(dmf)2·4dmf·2H2O (14)。
单晶X-射线衍射分析表明：化合物1为三维三重穿插结构；化合物2为三维二重穿插结构、3为三维结构、4为一维链状结构、5为二维层状穿插结构、6为三维孔道结构、7是基于二核SBU构筑的三维(3,5)-连接拓扑网络结构、8和9均属于三维二重穿插结构、10-14属于三维非穿插网状结构。其中,化合物1和2是利用共面的和非共面的羧酸配体而得到不同的结构；化合物4、5、6是利用一种具有顺式-或反式-结构的咪唑类柔性配体,通过溶剂或金属控制得到配体构型和维度均不相同的化合物；化合物7通过粉末衍射证实,可通过二维双层状结构MOF-47直接转换获得；化合物8、9为异质同晶结构；化合物10-12是利用空间位阻效应得到的非穿插的镧系金属有机框架物；化合物13-14则是利用一维棒状单元组装得到的非穿插微孔金属有机框架物。同时,对化合物3、5-7做了固态荧光谱学的测试,化合物12-14做了气体吸附性质的测试,化合物1-8、12、13做了热重测试分析。
以上金属-有机配合物不仅为超分子及金属-有机复合材料化学增添了新的内容,而且为寻找、筛选金属-有机复合材料提供了新的途径。
Investigation on the coordination complexes constructed by transition metals or lanthanide ions and ligands with muti-functional groups through coordinative bonds is an active research field in recent years. Due to the wide applications of coordination complexes in photoelectricity, magnetic material, redox catalysis, ion exchange, adsorption, separation, and molecular recognition etc., much attention has been devoted to the design and synthesis of novel kinds of structural topologies and compounds with special properties. It is important to master the factors influencing the structure of the coordination complex, such as solvent, conformations of ligands and temperature etc., so that we can control the formation of the complexes.
In the past several decades, planar carboxylate ligands have been widely studied because of their strong coordination ability and varieties of coordination modes. As known, the ligand conformation and coordination geometries of the metal ion have signifinant influence on the final structures of a MOF, and a little change of the ligand may result in new topological complexes. In this thesis, we try to synthesize novel coordination complexes by the use of carboxylic acids or combination with imidazole/pyridine/phenanthroline ligands assembling with metal ions through coordinative bonds or supramolecular weak interactions and to study the factors influencing the final structures and properties. The coordination chemistry of carboxylate ligands has been reviewed. The assembly reactions of rigid benzene-muti-carboxylate and and N-donor ligands with metal ions have yielded 14 novel coordination complexes: Cu4(OH)2(SO4)(HBTC)2(bpy)·bpy (1), Cu1.5(H2O)(TMBTC)(bpy)·0.5H2O (2), Cd2(H2O)5(TMBTC)(bpy)2·NO3·3H2O (3), Ni(BITMB)(TMIPA)·2H2O (4), Zn(BITMB)(IPA)·H2O (5), Zn2(BITMB)2(HIPA)2(IPA)·H2O(6), Zn(TBDC1)0.5(TBDC2)0.5 (7), Er(BDC),.5(dmf)(H2O) (8), Tm(BDC)1.5(dmf)(H2O) (9), Er2(BDC)3(phen)2-3H2O (10), Tm(TBDC)1.5(dmf)(H2O)·2H2O (11), Er2(TBDC)3(phen)2·4dmf-2H2O (12), Tm(BDC)1.5(H2O)0.5dmf·C2H5OH·2H2O (13), Tm4(BDC)6(H2O)2(dmf)2·4dmf·2H2O (14).All complexes have been determined by single-crystal X-ray diffraction. Complex 1 is three-dimensional three-fold interpenetrated complex; complexes 2 possesses three-dimensional two-fold interpenetrated structure; complexes 3 belongs to three-dimensional architecture; complexes 4 is one-dimensional chain; complex 5 belongs to two-dimensional interpenetrated layers; complexes 6 is three-dimensional porous framework; complexes 7 possesses three-dimensional framework with a rare (3,5)-connected net based on a dinuclear SBU; complex 8 and 9 are both three-dimensional structures with two-fold interpenetrating nets; complexes 10-14 belong to three-dimensional non-interpenetrated lanthanide-organic framework. In complexes 1 and 2, the different geometries of the carboxylate ligands (planarity and nonplanarity) induced two different assembly units. The flexible BITMB adopts syn or anti conformations in the complexes 4,5,6 which can be controlled by the presence or lack of water in the reaction, moreover, the dimensionality of the product can be controlled by the ligand conformation of BITMB. Complex 7 can be transformed from a previously reported 2D double layer (MOF-47) by liberating the coordinated water and dmf molecules, which was confirmed by X-ray powder diffraction. Complexes 8 and 9 are isostructural; complexes 10-12 apply organic ligands containing large hindrance groups to prevent the formation of interpenetration; while complexes 13-14 use in-situ reactions generated rod-shaped SBUs to improve final framework, with non-interpenetrated porous nets. Complexes 3,5-7 have been characterized by fluorescent spectra and gas sorption studies have been done for complexes 12-14; complexes 1-8,12 and 13 have been measured by TGA.
The results reported herein demonstrate that the use of non-plannar polybenzenecarboxylate ligands as precursors to bind transition metal or lanthanide metal ions, is a new approach for the formation of novel supramolecular networks with interesting physical properties.
引文
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