由咪唑二羧酸衍生物配体构筑的配位聚合物的合成、结构和性质研究
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摘要
本论文利用了六种咪唑二羧酸衍生作为有机桥连配体，包括三种刚性配体(2–(4–吡啶基)–4,5–咪唑二羧酸，2–(4–羧苯基)–4,5–咪唑二羧酸和2,4'–双咪唑–4,5–二羧酸)和三种柔性配体(1,2–双(4,5–咪唑二羧酸)乙烷，1,3–双(4,5–咪唑二羧酸)丙烷和1,4–双(4,5–咪唑二羧酸)丁烷)与d~(10)过渡金属离子和镧系金属离子合成新型的配位聚合物，研究这类化合物的合成条件及规律，分析网络所属的拓扑类型，考察分子间作用力，配体的几何构型，辅助配体对于整个结构的影响等规律，探究分子自组装原理，探索新类型的拓扑结构，寻找拓扑类型和结构的内部联系，预言新型拓扑和新结构的形成、以及新物质结构和性能间的关系。
利用水热合成和溶剂热合成技术，合成了31种新型的金属–有机配位聚合物，通过元素分析，IR，PXRD，TG和单晶X–射线衍射对晶体结构进行了表征，对化合物的热稳定性、光致发光性质进行了初步研究。
1.利用2–(4–吡啶基)–4,5–咪唑二羧酸(H_3PIDC)和不同构型的含N和羧酸共配体与d~(10)过渡金属，以及镧系金属离子在水热条件下反应，成功得到7个不同维数的配位化合物，其中包括5个由过渡金属构筑的二维和三维化合物[Cd_2(HPIDC)_2(bipy)]_n(1)，{[Cd_3(HPIDC)_2(btc)(H_2O)]·2H_2O}_n(2),{[Cd_2(HPIDC)_2(bdc)_(1/2)(H_2O)Cl]·H_2O}_n(3),{[Cd_2(PIDC)(Ac)(H_2O)]·H_2O}_n(4)，[Zn2(HPIDC)(ox)(H_2O)_2]n(5)，2个由镧系金属构筑的三维骨架结构{[Eu(HPIDC)(ox)1/2H_2O]·2H_2O}_n(6)，{[Tb(HPIDC)(ox)1/2H_2O]·2H_2O}_n(7)，并且考察了辅助配体的引入对最终化合物网络结构的影响。螯合配体bipy的引入钝化了金属中心，化合物1只形成了由左右手螺旋链连接所构成二维层状结构。化合物2是一个(4,4)格子状的二维层状结构，尽管多齿的btc配体被使用，但仍然没能使骨架向高维扩展。化合物3和4都是由配体连接柱状的次级构筑单元所构成，分别拥有(3,4)-连接和(3,4,5)-连接的三维骨架结构。化合物5则是一个由H_3PIDC，草酸和d~(10)金属共同构筑的三维CdSO4网络。同构的化合物6和7均是由H_3PIDC和草酸共同连接镧系金属离子所构成，在骨架中两种配体均以线性方式连接金属离子，整个骨架展示了三维α-Po网络。对7个化合物的固态荧光性质进行了研究。
2.合成了两种新的咪唑二羧酸衍生配体，2–(4–羧苯基)–4,5–咪唑二羧酸(H_4CpIDC)和2,4'–双咪唑–4,5–二羧酸(H_4BIDC)配体，利用它们与不同的含N共配体和d~(10)过渡金属离子在水热条件和低温混合溶剂热条件作用，成功得到了9个化合物，其中包括5个由H_4CpIDC配体构筑的化合物[Cd_3(HCpIDC)_2(H_2O)6]n(8)，[Cd(H_2CpIDC)(H_2O)]n(9),{[Cd_2(CpIDC)(2,2'–bpy)_2]·2H_2O}_n(10)，{[Zn3(HCpIDC)_2(4,4'–bipy)(H_2O)]·4H_2O}_n(11)，{[Zn2(CpIDC)(BIMB)]·H_2O}_n(12)，4个由H_4BIDC配体构筑的化合物，{[Cd_2(H_2BIDC)_2(H_2O)_2]·5H_2O}_n(13)，[Cd(H_2BIDC)]n(14)，[Zn3(BIMB)_2(HBIDC)_2]n(15)，{[Cd4(BIMB)_4(H_2BIDC)_4]·6H_2O]}_n(16)。化合物8是由H_4CpIDC连接金属CdII离子形成的一维Z字型链状结构。化合物9是由双核过渡金属和H_4CpIDC构筑的(3,3)连接的二维层状结构。化合物10是H_4CpIDC和辅助的2,2'-bipy共同连接CdII离子形成的具有(4,4)格子拓扑的二维层状结构。化合物11和12由H_4CpIDC和不同长度的线性桥连共配体连接金属ZnII离子所形成的(4,4)-连接和(3,4,6)-连接的三维网络。化合物13和14都是由H_4BIDC配体和金属CdII离子所构筑，但是不同反应溶剂导致了不同骨架结构。化合物13是的二维(4,4)格子结构，而化合物14是一个三维(3,3)-混连接骨架结构。化合物15和16是由H_4BIDC配体，BIMB共配体和d~(10)金属离子共同构筑的化合物。但是不同金属中心导致了两种截然不同三维骨架。化合物15展示了(3,4)-混连接的三维柱撑型骨架。化合物16则是一个三维(6,6)-连接骨架结构。同时对这些化合物的热稳定性和荧光性质进行了研究。
3.通过在两个咪唑二羧酸基团之间引入烷基链，成合了一个柔性配体1,2–双(4,5–咪唑二羧酸)乙烷(H_4EBIDC)。利用其和不同的含N有机共配体与ZnII离子在水热条件下反应得到5个从一维到三维的配位化合物，{[Zn_4(EBIDC)_2(bbi)_3/2(H_2O)]·7H_2O}_n(17)，{[Zn_4(EBIDC)_2(bix)_2]·7H_2O}_n(18)，{[Zn_8(EBIDC)_4(bpb)_3(H_2O)_2]·7H_2O}_n(19)，{[Zn2(EBIDC)(BIMB)]·H_2O}_n(20)，{[Zn_8(EBIDC)_4(bbi)_3]·7H_2O}_n(21)。在化合物17~21中，H_4EBIDC配体连接ZnII离子都形成笼状的[Zn_4(EBIDC)_2]次级构筑单元，次级构筑单元被不同的中性辅助配体连接形成不同的骨架结构。化合物17展示了一维梯状结构，而化合物18同样是一维链状结构，但是链与链之间进一步互锁成了三维骨架结构。化合物19是一个三重互穿的二维层状结构。化合物20展示了一个具有八重互穿的金刚石网络结构。化合物21与化合物17采用了相似的合成方法，但是不同金属锌盐，导致了不同的骨架。化合物21是一个三维(4,6)-连接的网络结构。对化合物和配体的荧光性质进行了研究。
4.通过延长烷基链的长度，合成了两个新的带有双咪唑二羧酸基团的柔性配体，1,3–双(4,5–咪唑二羧酸)丙烷(H_4PBIDC)和1,4–双(4,5–咪唑二羧酸)丁烷(H_4BBIDC)。利用H_4PBIDC配体与过渡金属离子和镧系金属离子成功构筑了4个二维和三维化合物，[Zn(H_2PBIDC)(H_2O)]n(22)，{[Zn2(H_2PBIDC)_2(H_2O)_2]·H_2O}_n(23)，[Cd(H_2PBIDC)(BIMB)]n(24)和{[Ce(HPBIDC)(H_2O)_2]·H_2O}_n(25)。利用H_4BBIDC和不同的含N共配体与d~(10)金属作用得到了6个三维柱撑型化合物，{[Cd_3(BBIDC)_3]·H_2O}_n(26)，{[Zn(BBIDC)1/2(BIMB)1/2]·H_2O}_n(27)，{[Zn(BBIDC)1/2(bix)1/2]·H_2O}_n(28)，{[Zn2(BBIDC)1/2(bytz)_2]·H_2O}_n(29)，{[Cd_2(BBIDC)1/2(bytz)_2]·3H_2O}_n(30)和{[Cd_2(BBIDC)1/2(tmpt)_2]·3H_2O}_n(31)。化合物22和23均是由H_4PBIDC配体和ZnII离子所构筑，但是不同阴离子导致两种不同的二维层状结构。尽管辅助的BIMB配体被使用，化合物24仍然只展示了一个二维结构。当具有较高配位数CeIII离子被使用时，一个三维(4,4)-混连接化合物25被获得。化合物26~31均为三维柱撑骨架结构，其中在26结构中，柱和层是由两种不同配位构型的H_4BBIDC配体所承担。而在其它的化合物中用于支撑的柱都为辅助的含N配体。对由d~(10)金属构筑的化合物的荧光性质进行了研究。
The target of this thesis is to construct novel coordination polymers on the basis of sixdifferent kinds of imidazole-4,5-dicarboxylic acid derivative ligands(2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylic acid,2-(4-carboxyphenyl)-1H-imidazole-4,5-dicarboxylic acid,2,4'-bi(1H-imidazole)-4,5-dicarboxylic acid,1,1'-(ethane-1,2-diyl)bis(1H-imidazole-4,5-dicarboxylic acid),1,1'-(propane-1,3-diyl)bis(1H-imidazole-4,5-dicarboxylic acid),1,1'-(butane-1,4-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)) and d~(10)transition metal ions aswell as lanthanide ions. The study on synthetic conditions and rules for these new compounds,topological analyses, and the exploration of relationships between structures and propertiesfor these new compounds are also carried out.
Thirty-one new coordination compounds have been synthesized on the basis ofhydrothermal and solvothermal synthesis methods, and structurally characterized byelemental analyses, IR, PXRD, TG and single crystal X-ray diffractions. The thermalstabilities and fluorescent activity of these compounds have been studied.
1. Eight new compounds on the basis of2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylicacid (H_4PIDC) ligand, N-containing and carboxylate coligands with different configurationshave been hydrothermally synthesized and structurally characterized including five2D and3D complexes,[Cd_2(HPIDC)_2(bipy)]_n(1),{[Cd_3(HPIDC)_2(btc)(H_2O)]·2H_2O}_n(2),{[Cd_2(HPIDC)_2(bdc)_(1/2)(H_2O)Cl]·H_2O}_n(3),{[Cd_2(PIDC)(Ac)(H_2O)]·H_2O}_n(4) and[Zn2(HPIDC)(ox)(H_2O)_2]n(5) constructed by transition metals, and two3D frameworks,{[Eu(HPIDC)(ox)1/2H_2O]·2H_2O}_n(6) and {[Tb(HPIDC)(ox)1/2H_2O]·2H_2O}_n(7) built bylanthanide metals. Owing to the chelating bipy ligand passivate the metal centers, socompound1only exhibits a2D layer structure formed by the inter-linking left-andright-handed helices. Compound2is a2D layer structure with the (4,4) grid topology.Compound3and4display3D (3,4)–connected and (3,4,5)–connected frameworksconstructed from ligands connecting rod-shaped SBUs. Compound5demonstrates aCd(SO4)_2network, which constructed by H_4PIDC, H_2ox and d~(10)metal. Compound6and7areisomorphic and exhibits classical α–Po network. In addition, the luminescent properties ofthese compounds are also investigated.
2. We have successfully synthesized two new ligands, namely2-(4-carboxyphenyl)-1H-imidazole-4,5-dicarboxylic acid (H_4CpIDC) and2,4'-bi(1H-imidazole)-4,5-dicarboxylic acid (H_4BIDC). Five new compounds, [Cd_3(HCpIDC)_2(H_2O)6]n(8),[Cd(H_2CpIDC)(H_2O)]n(9),{[Cd_2(CpIDC)(2,2'–bpy)_2]·2H_2O}_n(10),{[Zn3(HCpIDC)_2(4,4'–bipy)(H_2O)]·4H_2O}_n(11) and {[Zn2(CpIDC)(BIMB)]·H_2O}_n(12)were obtained by using H_4CpIDC as ligand. Four new compounds,{[Cd_2(H_2BIDC)_2(H_2O)_2]·5H_2O}_n(13),[Cd(H_2BIDC)]n(14),[Zn3(BIMB)_2(HBIDC)_2]n(15)and {[Cd4(BIMB)_4(H_2BIDC)_4]·6H_2O]}_n(16) were constructed by H_4BIDC ligand. Compound8is a1D zig-zag chain formed by H_4CpIDC linking CdIIions. Compound9and10exhibitsthe2D (3,3)-connected and (4,4)-connected layer structure, which built by H_4BIDC linkingbinuclear and mononuclear CdII, respectively. Compound11and12are formed fromH_4CpIDC and different linear coligands bridging ZnIIions, and they possess (4,4)-connectedand (3,4,6)-connected3D network. Compounds13and14are formed by H_4BBIDC linkingCdIIions. Different reaction solvents lead to the different structure of compounds13and14.Compound13is2D (4,4) network, while compound14displays a3D (3,3)-connectedframework. Both compound15and16constructed by H_4BBIDC and BIMB connecting d~(10)metal centers, but different metal centers result in two different framework. They are3Dpillared (3,4)-connected and (6,6)-connected networks, respetively. Furthermore, thethermostability and luminescent properties of these compounds have been studied.
3. A flexible ligand,1,1'-(ethane-1,2-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)(H_4EBIDC), was synthesized by introducing the alkyl chain between the twoimidazole-4,5-carboxylic acid groups. Five new compounds,{[Zn_4(EBIDC)_2(bbi)_3/2(H_2O)]·7H_2O}_n(17),{[Zn_4(EBIDC)_2(bix)_2]·7H_2O}_n(18),{[Zn_8(EBIDC)_4(bpyb)_3(H_2O)_2]·7H_2O}_n(19),{[Zn2(EBIDC)(BIMB)]·H_2O}_n(20) and{[Zn_8(EBIDC)_4(bbi)_3]·7H_2O}_n(21) were hydrothermally synthesized based on H_4EBIDCligand, divers neutral N-containing coligands and ZnIIions. In these compounds, H_4EBIDCligands links ZnIIions generating a cage-like [Zn_4(EBIDC)_2] SBU. Different secondaryligands further connects the [Zn_4(EBIDC)_2] SBUs leading to the different structures.Compound17displays a1D ladder-like structure. Compound18possesses a3D frameworkconstructed from inter-locking1D chains. Compounds19exhibits a2D three-foldinterpenetrating (3,3)-connected net. Compound20and21are3D eight-fold interpenetratingdiamond net and non-interpenetrating (4,6)-connected net, respectively. The luminescentproperties of these compounds and ligand have been investigated.
4. Two new flexible organic ligands,1,1'-(propane-1,3-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)(H_4PBIDC) and1,1'-(butane-1,4-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)(H_4BBIDC) were synthesizedby extending the length of the alkyl chain. We have successfully construced ten newcompounds by employing the two ligands with different coligand and metals (transition metaland lanthanide metal) under hydrothermal condition including four2D and3D complexes,[Zn(H_2PBIDC)(H_2O)]n(22),{[Zn2(H_2PBIDC)_2(H_2O)_2]·H_2O}_n(23)，[Cd(H_2PBIDC)(BIMB)]n (24) and {[Ce(HPBIDC)(H_2O)_2]·H_2O}_n(25) formed by H_4PBIDC, and six3D pillared-typecomplexes,{[Cd_3(BBIDC)3]·H_2O}_n(26),{[Zn(BBIDC)1/2(BIMB)1/2]·H_2O}_n(27),{[Zn(BBIDC)1/2(bix)1/2]·H_2O}_n(28),{[Zn2(BBIDC)1/2(bytz)_2]·H_2O}_n(29),{[Cd_2(BBIDC)1/2(bytz)_2]·3H_2O}_n(30) and {[Cd_2(BBIDC)1/2(tmpt)_2]·3H_2O}_n(31) constructedby H_4BBIDC. Both compounds22and23are formed by H_4PBIDC ligands linking ZnII, butthey exhibits two different2D layer structure. Although the assistant ligand BIMB was used,the framework of24still dispalys a2D structure. When using CeIIIas the metal centers, a3D(4,4)-connected compound25was obtained. Compound26~31are3D pillared-typecomplexes. In the framework of26, H_4BBIDC ligands with two different coordinationconfigurations can be viewed as the layer-like and pillar-like building units, respectively. Incompounds27~31, layer-like building units were built from H_4BBIDC bridging metals andthe N-containing coligands play the supporting role in the whole framework. The fluorescentstudies on those compounds based on d~(10)metals are also discussed.
利用水热合成和溶剂热合成技术，合成了31种新型的金属–有机配位聚合物，通过元素分析，IR，PXRD，TG和单晶X–射线衍射对晶体结构进行了表征，对化合物的热稳定性、光致发光性质进行了初步研究。
1.利用2–(4–吡啶基)–4,5–咪唑二羧酸(H_3PIDC)和不同构型的含N和羧酸共配体与d~(10)过渡金属，以及镧系金属离子在水热条件下反应，成功得到7个不同维数的配位化合物，其中包括5个由过渡金属构筑的二维和三维化合物[Cd_2(HPIDC)_2(bipy)]_n(1)，{[Cd_3(HPIDC)_2(btc)(H_2O)]·2H_2O}_n(2),{[Cd_2(HPIDC)_2(bdc)_(1/2)(H_2O)Cl]·H_2O}_n(3),{[Cd_2(PIDC)(Ac)(H_2O)]·H_2O}_n(4)，[Zn2(HPIDC)(ox)(H_2O)_2]n(5)，2个由镧系金属构筑的三维骨架结构{[Eu(HPIDC)(ox)1/2H_2O]·2H_2O}_n(6)，{[Tb(HPIDC)(ox)1/2H_2O]·2H_2O}_n(7)，并且考察了辅助配体的引入对最终化合物网络结构的影响。螯合配体bipy的引入钝化了金属中心，化合物1只形成了由左右手螺旋链连接所构成二维层状结构。化合物2是一个(4,4)格子状的二维层状结构，尽管多齿的btc配体被使用，但仍然没能使骨架向高维扩展。化合物3和4都是由配体连接柱状的次级构筑单元所构成，分别拥有(3,4)-连接和(3,4,5)-连接的三维骨架结构。化合物5则是一个由H_3PIDC，草酸和d~(10)金属共同构筑的三维CdSO4网络。同构的化合物6和7均是由H_3PIDC和草酸共同连接镧系金属离子所构成，在骨架中两种配体均以线性方式连接金属离子，整个骨架展示了三维α-Po网络。对7个化合物的固态荧光性质进行了研究。
2.合成了两种新的咪唑二羧酸衍生配体，2–(4–羧苯基)–4,5–咪唑二羧酸(H_4CpIDC)和2,4'–双咪唑–4,5–二羧酸(H_4BIDC)配体，利用它们与不同的含N共配体和d~(10)过渡金属离子在水热条件和低温混合溶剂热条件作用，成功得到了9个化合物，其中包括5个由H_4CpIDC配体构筑的化合物[Cd_3(HCpIDC)_2(H_2O)6]n(8)，[Cd(H_2CpIDC)(H_2O)]n(9),{[Cd_2(CpIDC)(2,2'–bpy)_2]·2H_2O}_n(10)，{[Zn3(HCpIDC)_2(4,4'–bipy)(H_2O)]·4H_2O}_n(11)，{[Zn2(CpIDC)(BIMB)]·H_2O}_n(12)，4个由H_4BIDC配体构筑的化合物，{[Cd_2(H_2BIDC)_2(H_2O)_2]·5H_2O}_n(13)，[Cd(H_2BIDC)]n(14)，[Zn3(BIMB)_2(HBIDC)_2]n(15)，{[Cd4(BIMB)_4(H_2BIDC)_4]·6H_2O]}_n(16)。化合物8是由H_4CpIDC连接金属CdII离子形成的一维Z字型链状结构。化合物9是由双核过渡金属和H_4CpIDC构筑的(3,3)连接的二维层状结构。化合物10是H_4CpIDC和辅助的2,2'-bipy共同连接CdII离子形成的具有(4,4)格子拓扑的二维层状结构。化合物11和12由H_4CpIDC和不同长度的线性桥连共配体连接金属ZnII离子所形成的(4,4)-连接和(3,4,6)-连接的三维网络。化合物13和14都是由H_4BIDC配体和金属CdII离子所构筑，但是不同反应溶剂导致了不同骨架结构。化合物13是的二维(4,4)格子结构，而化合物14是一个三维(3,3)-混连接骨架结构。化合物15和16是由H_4BIDC配体，BIMB共配体和d~(10)金属离子共同构筑的化合物。但是不同金属中心导致了两种截然不同三维骨架。化合物15展示了(3,4)-混连接的三维柱撑型骨架。化合物16则是一个三维(6,6)-连接骨架结构。同时对这些化合物的热稳定性和荧光性质进行了研究。
3.通过在两个咪唑二羧酸基团之间引入烷基链，成合了一个柔性配体1,2–双(4,5–咪唑二羧酸)乙烷(H_4EBIDC)。利用其和不同的含N有机共配体与ZnII离子在水热条件下反应得到5个从一维到三维的配位化合物，{[Zn_4(EBIDC)_2(bbi)_3/2(H_2O)]·7H_2O}_n(17)，{[Zn_4(EBIDC)_2(bix)_2]·7H_2O}_n(18)，{[Zn_8(EBIDC)_4(bpb)_3(H_2O)_2]·7H_2O}_n(19)，{[Zn2(EBIDC)(BIMB)]·H_2O}_n(20)，{[Zn_8(EBIDC)_4(bbi)_3]·7H_2O}_n(21)。在化合物17~21中，H_4EBIDC配体连接ZnII离子都形成笼状的[Zn_4(EBIDC)_2]次级构筑单元，次级构筑单元被不同的中性辅助配体连接形成不同的骨架结构。化合物17展示了一维梯状结构，而化合物18同样是一维链状结构，但是链与链之间进一步互锁成了三维骨架结构。化合物19是一个三重互穿的二维层状结构。化合物20展示了一个具有八重互穿的金刚石网络结构。化合物21与化合物17采用了相似的合成方法，但是不同金属锌盐，导致了不同的骨架。化合物21是一个三维(4,6)-连接的网络结构。对化合物和配体的荧光性质进行了研究。
4.通过延长烷基链的长度，合成了两个新的带有双咪唑二羧酸基团的柔性配体，1,3–双(4,5–咪唑二羧酸)丙烷(H_4PBIDC)和1,4–双(4,5–咪唑二羧酸)丁烷(H_4BBIDC)。利用H_4PBIDC配体与过渡金属离子和镧系金属离子成功构筑了4个二维和三维化合物，[Zn(H_2PBIDC)(H_2O)]n(22)，{[Zn2(H_2PBIDC)_2(H_2O)_2]·H_2O}_n(23)，[Cd(H_2PBIDC)(BIMB)]n(24)和{[Ce(HPBIDC)(H_2O)_2]·H_2O}_n(25)。利用H_4BBIDC和不同的含N共配体与d~(10)金属作用得到了6个三维柱撑型化合物，{[Cd_3(BBIDC)_3]·H_2O}_n(26)，{[Zn(BBIDC)1/2(BIMB)1/2]·H_2O}_n(27)，{[Zn(BBIDC)1/2(bix)1/2]·H_2O}_n(28)，{[Zn2(BBIDC)1/2(bytz)_2]·H_2O}_n(29)，{[Cd_2(BBIDC)1/2(bytz)_2]·3H_2O}_n(30)和{[Cd_2(BBIDC)1/2(tmpt)_2]·3H_2O}_n(31)。化合物22和23均是由H_4PBIDC配体和ZnII离子所构筑，但是不同阴离子导致两种不同的二维层状结构。尽管辅助的BIMB配体被使用，化合物24仍然只展示了一个二维结构。当具有较高配位数CeIII离子被使用时，一个三维(4,4)-混连接化合物25被获得。化合物26~31均为三维柱撑骨架结构，其中在26结构中，柱和层是由两种不同配位构型的H_4BBIDC配体所承担。而在其它的化合物中用于支撑的柱都为辅助的含N配体。对由d~(10)金属构筑的化合物的荧光性质进行了研究。
The target of this thesis is to construct novel coordination polymers on the basis of sixdifferent kinds of imidazole-4,5-dicarboxylic acid derivative ligands(2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylic acid,2-(4-carboxyphenyl)-1H-imidazole-4,5-dicarboxylic acid,2,4'-bi(1H-imidazole)-4,5-dicarboxylic acid,1,1'-(ethane-1,2-diyl)bis(1H-imidazole-4,5-dicarboxylic acid),1,1'-(propane-1,3-diyl)bis(1H-imidazole-4,5-dicarboxylic acid),1,1'-(butane-1,4-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)) and d~(10)transition metal ions aswell as lanthanide ions. The study on synthetic conditions and rules for these new compounds,topological analyses, and the exploration of relationships between structures and propertiesfor these new compounds are also carried out.
Thirty-one new coordination compounds have been synthesized on the basis ofhydrothermal and solvothermal synthesis methods, and structurally characterized byelemental analyses, IR, PXRD, TG and single crystal X-ray diffractions. The thermalstabilities and fluorescent activity of these compounds have been studied.
1. Eight new compounds on the basis of2-(pyridin-4-yl)-1H-imidazole-4,5-dicarboxylicacid (H_4PIDC) ligand, N-containing and carboxylate coligands with different configurationshave been hydrothermally synthesized and structurally characterized including five2D and3D complexes,[Cd_2(HPIDC)_2(bipy)]_n(1),{[Cd_3(HPIDC)_2(btc)(H_2O)]·2H_2O}_n(2),{[Cd_2(HPIDC)_2(bdc)_(1/2)(H_2O)Cl]·H_2O}_n(3),{[Cd_2(PIDC)(Ac)(H_2O)]·H_2O}_n(4) and[Zn2(HPIDC)(ox)(H_2O)_2]n(5) constructed by transition metals, and two3D frameworks,{[Eu(HPIDC)(ox)1/2H_2O]·2H_2O}_n(6) and {[Tb(HPIDC)(ox)1/2H_2O]·2H_2O}_n(7) built bylanthanide metals. Owing to the chelating bipy ligand passivate the metal centers, socompound1only exhibits a2D layer structure formed by the inter-linking left-andright-handed helices. Compound2is a2D layer structure with the (4,4) grid topology.Compound3and4display3D (3,4)–connected and (3,4,5)–connected frameworksconstructed from ligands connecting rod-shaped SBUs. Compound5demonstrates aCd(SO4)_2network, which constructed by H_4PIDC, H_2ox and d~(10)metal. Compound6and7areisomorphic and exhibits classical α–Po network. In addition, the luminescent properties ofthese compounds are also investigated.
2. We have successfully synthesized two new ligands, namely2-(4-carboxyphenyl)-1H-imidazole-4,5-dicarboxylic acid (H_4CpIDC) and2,4'-bi(1H-imidazole)-4,5-dicarboxylic acid (H_4BIDC). Five new compounds, [Cd_3(HCpIDC)_2(H_2O)6]n(8),[Cd(H_2CpIDC)(H_2O)]n(9),{[Cd_2(CpIDC)(2,2'–bpy)_2]·2H_2O}_n(10),{[Zn3(HCpIDC)_2(4,4'–bipy)(H_2O)]·4H_2O}_n(11) and {[Zn2(CpIDC)(BIMB)]·H_2O}_n(12)were obtained by using H_4CpIDC as ligand. Four new compounds,{[Cd_2(H_2BIDC)_2(H_2O)_2]·5H_2O}_n(13),[Cd(H_2BIDC)]n(14),[Zn3(BIMB)_2(HBIDC)_2]n(15)and {[Cd4(BIMB)_4(H_2BIDC)_4]·6H_2O]}_n(16) were constructed by H_4BIDC ligand. Compound8is a1D zig-zag chain formed by H_4CpIDC linking CdIIions. Compound9and10exhibitsthe2D (3,3)-connected and (4,4)-connected layer structure, which built by H_4BIDC linkingbinuclear and mononuclear CdII, respectively. Compound11and12are formed fromH_4CpIDC and different linear coligands bridging ZnIIions, and they possess (4,4)-connectedand (3,4,6)-connected3D network. Compounds13and14are formed by H_4BBIDC linkingCdIIions. Different reaction solvents lead to the different structure of compounds13and14.Compound13is2D (4,4) network, while compound14displays a3D (3,3)-connectedframework. Both compound15and16constructed by H_4BBIDC and BIMB connecting d~(10)metal centers, but different metal centers result in two different framework. They are3Dpillared (3,4)-connected and (6,6)-connected networks, respetively. Furthermore, thethermostability and luminescent properties of these compounds have been studied.
3. A flexible ligand,1,1'-(ethane-1,2-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)(H_4EBIDC), was synthesized by introducing the alkyl chain between the twoimidazole-4,5-carboxylic acid groups. Five new compounds,{[Zn_4(EBIDC)_2(bbi)_3/2(H_2O)]·7H_2O}_n(17),{[Zn_4(EBIDC)_2(bix)_2]·7H_2O}_n(18),{[Zn_8(EBIDC)_4(bpyb)_3(H_2O)_2]·7H_2O}_n(19),{[Zn2(EBIDC)(BIMB)]·H_2O}_n(20) and{[Zn_8(EBIDC)_4(bbi)_3]·7H_2O}_n(21) were hydrothermally synthesized based on H_4EBIDCligand, divers neutral N-containing coligands and ZnIIions. In these compounds, H_4EBIDCligands links ZnIIions generating a cage-like [Zn_4(EBIDC)_2] SBU. Different secondaryligands further connects the [Zn_4(EBIDC)_2] SBUs leading to the different structures.Compound17displays a1D ladder-like structure. Compound18possesses a3D frameworkconstructed from inter-locking1D chains. Compounds19exhibits a2D three-foldinterpenetrating (3,3)-connected net. Compound20and21are3D eight-fold interpenetratingdiamond net and non-interpenetrating (4,6)-connected net, respectively. The luminescentproperties of these compounds and ligand have been investigated.
4. Two new flexible organic ligands,1,1'-(propane-1,3-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)(H_4PBIDC) and1,1'-(butane-1,4-diyl)bis(1H-imidazole-4,5-dicarboxylic acid)(H_4BBIDC) were synthesizedby extending the length of the alkyl chain. We have successfully construced ten newcompounds by employing the two ligands with different coligand and metals (transition metaland lanthanide metal) under hydrothermal condition including four2D and3D complexes,[Zn(H_2PBIDC)(H_2O)]n(22),{[Zn2(H_2PBIDC)_2(H_2O)_2]·H_2O}_n(23)，[Cd(H_2PBIDC)(BIMB)]n (24) and {[Ce(HPBIDC)(H_2O)_2]·H_2O}_n(25) formed by H_4PBIDC, and six3D pillared-typecomplexes,{[Cd_3(BBIDC)3]·H_2O}_n(26),{[Zn(BBIDC)1/2(BIMB)1/2]·H_2O}_n(27),{[Zn(BBIDC)1/2(bix)1/2]·H_2O}_n(28),{[Zn2(BBIDC)1/2(bytz)_2]·H_2O}_n(29),{[Cd_2(BBIDC)1/2(bytz)_2]·3H_2O}_n(30) and {[Cd_2(BBIDC)1/2(tmpt)_2]·3H_2O}_n(31) constructedby H_4BBIDC. Both compounds22and23are formed by H_4PBIDC ligands linking ZnII, butthey exhibits two different2D layer structure. Although the assistant ligand BIMB was used,the framework of24still dispalys a2D structure. When using CeIIIas the metal centers, a3D(4,4)-connected compound25was obtained. Compound26~31are3D pillared-typecomplexes. In the framework of26, H_4BBIDC ligands with two different coordinationconfigurations can be viewed as the layer-like and pillar-like building units, respectively. Incompounds27~31, layer-like building units were built from H_4BBIDC bridging metals andthe N-containing coligands play the supporting role in the whole framework. The fluorescentstudies on those compounds based on d~(10)metals are also discussed.
引文
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