以氮杂环化合物为模板的稀土配位聚合物的合成、结构及性能研究
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摘要
本论文以氮杂环化合物作为模板，在水热条件下，成功合成了二十一个结构新颖的稀土配位聚合物，测定并解析了它们的单晶结构，对它们进行了元素分析、红外光谱、热重分析等表征，并对所合成的部分化合物的紫外-可见吸收光谱和发光性能进行研究。具体内容如下：
1.以4,4′-联吡啶为模板合成了一系列结构新颖的稀土配位聚合物{(bpy)[Re(ip)1.5(H_2O)4]}n（Re=Pr(1)、Nd(2)、Sm(3)、Eu(4)和Gd(5)，bpy=4,4′-联吡啶，ip=间苯二甲酸二价阴离子）。这一系列化合物是同构的。它们是由一维（1D）的梯形链通过氢键形成的三维（3D）框架结构。4,4′-联吡啶作为客体模板与配位水分子形成氢键，位于框架通道中间。在不同波长的紫外光激发下，化合物4发出纯度高的红色的强光。
2.以咪唑阳离子为模板合成了一系列结构新颖的稀土配位聚合物{(Him)[Re(ip)_2(H_2O)]}n（Re=Sm(6)、Eu(7)、Gd(8)和Tb(9)，Him=咪唑阳离子，ip=间苯二甲酸二价阴离子）和{[Re2(ip)_3(H_2O)_2]·H_2O}n（Re=Er(10)，ip=间苯二甲酸二价阴离子）。化合物6、7和9是同构的，化合物8与它们的结构相似。在化合物6-9中，间苯二甲酸配体与金属离子连接成蜂窝状的三维（3D）结构。咪唑阳离子与间苯二甲酸离子形成氢键，位于通道中间。化合物10的三维（3D）的框架结构是由二维（2D）的层状结构通过氢键形成的。层状结构中存在左旋和右旋的双螺旋链。在不同波长的紫外光激发下，化合物7和9分别发出纯度高的红色和绿色强光。
3.以2,2′-联吡啶为辅助配体和模板合成了一系列结构新颖的稀土配位聚合物{(bpy)[Re(ip)(Hip)(bpy)]}_n（Re=Eu(11)、Ho(13)、Er(14)和Yb(15)，bpy=2,2′-联吡啶，ip=间苯二甲酸二价阴离子，Hip=间苯二甲酸一价阴离子）和{(bpy)0.5[Re(ip)(Hip)(bpy)]}n（Re=Tb(12)，bpy=2,2′-联吡啶，ip=间苯二甲酸二价阴离子，Hip=间苯二甲酸一价阴离子）。在化合物11中，间苯二甲酸配体与金属离子连接成二维（2D）的层状结构。一部分2,2′-联吡啶参与配位，另一部分2,2′-联吡啶作为客体模板位于层与层之间。客体模板2,2′-联吡啶与配位的2,2′-联吡啶存在π-π堆积作用。二维层状结构通过π-π堆积作用进一步连接成三维的框架结构。化合物12的结构与化合物11相似。在化合物13-15中，间苯二甲酸配体与金属离子连接成一维（1D）的双链结构。一部分2,2′-联吡啶参与配位，另一部分2,2′-联吡啶作为客体模板位于双链结构周围。客体模板2,2′-联吡啶与间苯二甲酸配体存在π-π堆积作用。双链结构通过π-π堆积作用进一步连接成三维的框架结构。这是首次合成2,2′-联吡啶既是配体又是模板的稀土配位聚合物。在不同波长的紫外光激发下，化合物11和12分别发出纯度高的红色和绿色强光。
4.以1,10-邻菲啰啉为辅助配体，由1,10-邻菲啰啉通过原位反应产生的2,2′-联吡啶作模板合成了一种结构新颖的稀土配位聚合物{(bpy)_(0.5)[Re_3(ip)_4(phen)_4(H_2O)]·2H_2O}n（Re=Dy(16)，bpy=2,2′-联吡啶，ip=间苯二甲酸二价阴离子，phen=1,10-邻菲啰啉）。在化合物16中，间苯二甲酸配体与金属离子连接成层状结构，2,2′-联吡啶作为模板位于层与层之间。1,10-邻菲啰啉与金属离子螯合，2,2′-联吡啶与1,10-邻菲啰啉存在π-π堆积作用。层状结构通过π-π堆积作用进一步连接成三维的框架结构。这是首次在稀土配位聚合物中发现中心离子有混合化合价，首次发现1,10-邻菲啰啉在金属离子的存在下可生成2,2′-联吡啶。在不同波长的紫外光激发下，化合物16发出蓝色光。
5.以间苯二甲酸和2-吡啶甲酸为混合配体，以2,2′-联吡啶或咪唑为模板合成了一系列结构新颖的稀土配位聚合物[Re_2(ip)_2(pic)_2]_n（Re=Pr(17)、Nd(18)、Eu(19)、Tb(20)和Ho(21)，ip=间苯二甲酸二价阴离子，pic=2-吡啶甲酸阴离子）。这一系列化合物是同构的。间苯二甲酸配体与金属离子分别连接成单链和双链，2-吡啶甲酸将这些单链和双链分别连接成层状结构，两种层状结构通过共用金属离子进一步相互连接成三维（3D）的网状结构。在不同波长的紫外光激发下，化合物19和20分别发出纯度高的红色和绿色强光。
本论文成功地将模板法用于间苯二甲酸配位聚合物的合成，对于合成含其它配体、结构新颖的配位聚合物，特别是合成配位聚合物同分异构体有重要的指导作用。
In this dissertation,21rare earth coordination polymers in different structures havebeen synthesized via hydrothermal method and using nitrogen heterocyclic compounds astemplates. Their single-crystal structures have been determinated and analyzed, and theyhave been characterized by using elemental analyses, infrared spectra and thermogravimetric(TG) analyses. The absorption spectra and luminescence spectra of some of the compoundshave also been studied. The details are summarized as following:
1. A series of novel rare earth coordination polymers {(bpy)[Re(ip)1.5(H_2O)4]}n(Re=Pr(1), Nd(2), Sm(3), Eu(4) and Gd(5), bpy=4,4′-bipyridine, ip=isophthalate) have beensynthesized by using4,4′-bipyridine molecules as templates. This series of compounds areisostructural. Their three-dimensional (3D) networks are formed by one-dimensional (1D)ladder-shaped chains through hydrogen bonds. The channel regions of the networks are hostto4,4′-bipyridine molecules which serve as guest-templates. These4,4′-bipyridine moleculesshow hydrogen bond participation with metal-bound water molecules. The emission spectrashow that4emits intense sharp red light when it is excited by different wavelengthultraviolet light.
2. A series of novel rare earth coordination polymers {(Him)[Re(ip)_2(H_2O)]}_n(Re=Sm(6), Eu(7), Gd(8) and Tb(9), Him=imdazole cation, ip=isophthalate) and{[Re_2(ip)_3(H_2O)_2]·H_2O}n(Re=Er(10), ip=isophthalate) have been synthesized by usingimdazole cations as templates. The compounds6,7and9are isostructural. The structure ofcompound8is similar to the structures of compounds6,7and9. In the compounds6-9, theisophthalate ligands link the metal ions to form three-dimensional (3D) honeycomb-likeframeworks. The channel regions of the frameworks are host to imdazole cations whichserve as guest-templates. These imdazole cations show hydrogen bond participation with theisophthalate ligands. The three-dimensional (3D) network of the compound10is formed bytwo-dimensional (2D) layers through hydrogen bonds. There are left-and right-handeddouble helical chains in the layers of the compound10. The emission spectra show that7emits intense sharp red light and9emits intense sharp green light when they are excited bydifferent wavelength ultraviolet light.
3. A series of novel rare earth coordination polymers {(bpy)[Re(ip)(Hip)(bpy)]}n(Re=Eu(11), Ho(13), Er(14) and Yb(15), bpy=2,2′-bipyridine, ip=isophthalic acid dianion,Hip=isophthalic acid monoanion) and {(bpy)0.5[Re(ip)(Hip)(bpy)]}n(Re=Tb(12),bpy=2,2′-bipyridine, ip=isophthalic acid dianion, Hip=isophthalic acid monoanion) havebeen synthesized by using2,2′-bipyridine molecules as auxiliary ligands and templates. Inthe compound11, the isophthalate ligands link the metal ions to form two-dimensional (2D)layer structures. A part of2,2′-bipyridine molecules serve as auxiliary ligands while theother serve as guest-templates which located between the layers. There are π-π stackinginteractions between coordinated2,2′-bipyridine molecules and guest-template2,2′-bipyridine molecules. The three-dimensional (3D) network of the compound11isformed by two-dimensional (2D) layers through π-π stacking interactions. The structure ofcompound12is similar to the structure of compounds11. In the compound13-15, theisophthalate ligands link the metal ions to form one-dimensional (1D) double chains. A partof2,2′-bipyridine molecules serve as auxiliary ligands while the other serve asguest-templates which located around the double chains. There are π-π stacking interactionsbetween guest-template2,2′-bipyridine molecules and isophthalate ligands. Thethree-dimensional (3D) networks of the compound13-15are formed by one-dimensional(1D) double chains through π-π stacking interactions. This is the first time to synthesize rareearth coordination polymers in which2,2′-bipyridine molecules serve as auxiliary ligandsand templates. The emission spectra show that11emits intense sharp red light and12emitsintense sharp green light when they are excited by different wavelength ultraviolet light.
4. A novel rare earth coordination polymer {(bpy)0.5[Re3(ip)4(phen)4(H_2O)]·2H_2O}n(Re=Dy(16), bpy=2,2′-bipyridine, ip=isophthalate, phen=1,10-phenanthroline) have beensynthesized by using1,10-phenanthroline molecules as auxiliary ligands and2,2′-bipyridinemolecules formed in situ reaction as templates. In the compound16, the isophthalate ligandslink the metal ions to form two-dimensional (2D) layer structures. The2,2′-bipyridinemolecules serve as guest-templates which located between the layers.1,10-phenanthrolinemolecules chelate metal ions. There are π-π stacking interactions between guest-template2,2′-bipyridine molecules and1,10-phenanthroline molecules. The three-dimensional (3D)network of the compound16is formed by two-dimensional (2D) layers through π-π stacking interactions. This is the first time to synthesize mixed-valence rare earth coordinationpolymer, and the first time to find1,10-phenanthroline can be transformed into2,2′-bipyridine under hydrothermal conditions in the presence of metal ions. The emissionspectra show that16emits blue light when it is excited by different wavelength ultravioletlight.
5. A series of novel rare earth coordination polymers [Re2(ip)2(pic)2]n(Re=Pr(17),Nd(18), Eu(19), Tb(20) and Ho(21), ip=isophthalate, pic=picolinate) have been synthesizedby using isophthalate ligands and picolinate ligands as mixed ligands, and2,2′-bipyridinemolecules or imdazole cations as templates. This series of compounds are isostructural. Theisophthalate ligands link the metal ions to form one-dimensional (1D) single chains anddouble chains, respectively. The picolinate ligands link these single chains and double chainsto form two kinds of layer structures, respectively. Two kinds of layer structures are furtherlinked by sharing metal ions to form the three-dimensional (3D) net structure. The emissionspectra show that19emits intense sharp red light and20emits intense sharp green lightwhen they are excited by different wavelength ultraviolet light.
We have successfully used templates to synthesize coordination polymers withisophthalate ligands in this dissertation. We believe this dissertation has an importantguiding function for the syntheses of novel coordination polymers with other ligands,especially for the syntheses of isomers of coordination polymers.
1.以4,4′-联吡啶为模板合成了一系列结构新颖的稀土配位聚合物{(bpy)[Re(ip)1.5(H_2O)4]}n（Re=Pr(1)、Nd(2)、Sm(3)、Eu(4)和Gd(5)，bpy=4,4′-联吡啶，ip=间苯二甲酸二价阴离子）。这一系列化合物是同构的。它们是由一维（1D）的梯形链通过氢键形成的三维（3D）框架结构。4,4′-联吡啶作为客体模板与配位水分子形成氢键，位于框架通道中间。在不同波长的紫外光激发下，化合物4发出纯度高的红色的强光。
2.以咪唑阳离子为模板合成了一系列结构新颖的稀土配位聚合物{(Him)[Re(ip)_2(H_2O)]}n（Re=Sm(6)、Eu(7)、Gd(8)和Tb(9)，Him=咪唑阳离子，ip=间苯二甲酸二价阴离子）和{[Re2(ip)_3(H_2O)_2]·H_2O}n（Re=Er(10)，ip=间苯二甲酸二价阴离子）。化合物6、7和9是同构的，化合物8与它们的结构相似。在化合物6-9中，间苯二甲酸配体与金属离子连接成蜂窝状的三维（3D）结构。咪唑阳离子与间苯二甲酸离子形成氢键，位于通道中间。化合物10的三维（3D）的框架结构是由二维（2D）的层状结构通过氢键形成的。层状结构中存在左旋和右旋的双螺旋链。在不同波长的紫外光激发下，化合物7和9分别发出纯度高的红色和绿色强光。
3.以2,2′-联吡啶为辅助配体和模板合成了一系列结构新颖的稀土配位聚合物{(bpy)[Re(ip)(Hip)(bpy)]}_n（Re=Eu(11)、Ho(13)、Er(14)和Yb(15)，bpy=2,2′-联吡啶，ip=间苯二甲酸二价阴离子，Hip=间苯二甲酸一价阴离子）和{(bpy)0.5[Re(ip)(Hip)(bpy)]}n（Re=Tb(12)，bpy=2,2′-联吡啶，ip=间苯二甲酸二价阴离子，Hip=间苯二甲酸一价阴离子）。在化合物11中，间苯二甲酸配体与金属离子连接成二维（2D）的层状结构。一部分2,2′-联吡啶参与配位，另一部分2,2′-联吡啶作为客体模板位于层与层之间。客体模板2,2′-联吡啶与配位的2,2′-联吡啶存在π-π堆积作用。二维层状结构通过π-π堆积作用进一步连接成三维的框架结构。化合物12的结构与化合物11相似。在化合物13-15中，间苯二甲酸配体与金属离子连接成一维（1D）的双链结构。一部分2,2′-联吡啶参与配位，另一部分2,2′-联吡啶作为客体模板位于双链结构周围。客体模板2,2′-联吡啶与间苯二甲酸配体存在π-π堆积作用。双链结构通过π-π堆积作用进一步连接成三维的框架结构。这是首次合成2,2′-联吡啶既是配体又是模板的稀土配位聚合物。在不同波长的紫外光激发下，化合物11和12分别发出纯度高的红色和绿色强光。
4.以1,10-邻菲啰啉为辅助配体，由1,10-邻菲啰啉通过原位反应产生的2,2′-联吡啶作模板合成了一种结构新颖的稀土配位聚合物{(bpy)_(0.5)[Re_3(ip)_4(phen)_4(H_2O)]·2H_2O}n（Re=Dy(16)，bpy=2,2′-联吡啶，ip=间苯二甲酸二价阴离子，phen=1,10-邻菲啰啉）。在化合物16中，间苯二甲酸配体与金属离子连接成层状结构，2,2′-联吡啶作为模板位于层与层之间。1,10-邻菲啰啉与金属离子螯合，2,2′-联吡啶与1,10-邻菲啰啉存在π-π堆积作用。层状结构通过π-π堆积作用进一步连接成三维的框架结构。这是首次在稀土配位聚合物中发现中心离子有混合化合价，首次发现1,10-邻菲啰啉在金属离子的存在下可生成2,2′-联吡啶。在不同波长的紫外光激发下，化合物16发出蓝色光。
5.以间苯二甲酸和2-吡啶甲酸为混合配体，以2,2′-联吡啶或咪唑为模板合成了一系列结构新颖的稀土配位聚合物[Re_2(ip)_2(pic)_2]_n（Re=Pr(17)、Nd(18)、Eu(19)、Tb(20)和Ho(21)，ip=间苯二甲酸二价阴离子，pic=2-吡啶甲酸阴离子）。这一系列化合物是同构的。间苯二甲酸配体与金属离子分别连接成单链和双链，2-吡啶甲酸将这些单链和双链分别连接成层状结构，两种层状结构通过共用金属离子进一步相互连接成三维（3D）的网状结构。在不同波长的紫外光激发下，化合物19和20分别发出纯度高的红色和绿色强光。
本论文成功地将模板法用于间苯二甲酸配位聚合物的合成，对于合成含其它配体、结构新颖的配位聚合物，特别是合成配位聚合物同分异构体有重要的指导作用。
In this dissertation,21rare earth coordination polymers in different structures havebeen synthesized via hydrothermal method and using nitrogen heterocyclic compounds astemplates. Their single-crystal structures have been determinated and analyzed, and theyhave been characterized by using elemental analyses, infrared spectra and thermogravimetric(TG) analyses. The absorption spectra and luminescence spectra of some of the compoundshave also been studied. The details are summarized as following:
1. A series of novel rare earth coordination polymers {(bpy)[Re(ip)1.5(H_2O)4]}n(Re=Pr(1), Nd(2), Sm(3), Eu(4) and Gd(5), bpy=4,4′-bipyridine, ip=isophthalate) have beensynthesized by using4,4′-bipyridine molecules as templates. This series of compounds areisostructural. Their three-dimensional (3D) networks are formed by one-dimensional (1D)ladder-shaped chains through hydrogen bonds. The channel regions of the networks are hostto4,4′-bipyridine molecules which serve as guest-templates. These4,4′-bipyridine moleculesshow hydrogen bond participation with metal-bound water molecules. The emission spectrashow that4emits intense sharp red light when it is excited by different wavelengthultraviolet light.
2. A series of novel rare earth coordination polymers {(Him)[Re(ip)_2(H_2O)]}_n(Re=Sm(6), Eu(7), Gd(8) and Tb(9), Him=imdazole cation, ip=isophthalate) and{[Re_2(ip)_3(H_2O)_2]·H_2O}n(Re=Er(10), ip=isophthalate) have been synthesized by usingimdazole cations as templates. The compounds6,7and9are isostructural. The structure ofcompound8is similar to the structures of compounds6,7and9. In the compounds6-9, theisophthalate ligands link the metal ions to form three-dimensional (3D) honeycomb-likeframeworks. The channel regions of the frameworks are host to imdazole cations whichserve as guest-templates. These imdazole cations show hydrogen bond participation with theisophthalate ligands. The three-dimensional (3D) network of the compound10is formed bytwo-dimensional (2D) layers through hydrogen bonds. There are left-and right-handeddouble helical chains in the layers of the compound10. The emission spectra show that7emits intense sharp red light and9emits intense sharp green light when they are excited bydifferent wavelength ultraviolet light.
3. A series of novel rare earth coordination polymers {(bpy)[Re(ip)(Hip)(bpy)]}n(Re=Eu(11), Ho(13), Er(14) and Yb(15), bpy=2,2′-bipyridine, ip=isophthalic acid dianion,Hip=isophthalic acid monoanion) and {(bpy)0.5[Re(ip)(Hip)(bpy)]}n(Re=Tb(12),bpy=2,2′-bipyridine, ip=isophthalic acid dianion, Hip=isophthalic acid monoanion) havebeen synthesized by using2,2′-bipyridine molecules as auxiliary ligands and templates. Inthe compound11, the isophthalate ligands link the metal ions to form two-dimensional (2D)layer structures. A part of2,2′-bipyridine molecules serve as auxiliary ligands while theother serve as guest-templates which located between the layers. There are π-π stackinginteractions between coordinated2,2′-bipyridine molecules and guest-template2,2′-bipyridine molecules. The three-dimensional (3D) network of the compound11isformed by two-dimensional (2D) layers through π-π stacking interactions. The structure ofcompound12is similar to the structure of compounds11. In the compound13-15, theisophthalate ligands link the metal ions to form one-dimensional (1D) double chains. A partof2,2′-bipyridine molecules serve as auxiliary ligands while the other serve asguest-templates which located around the double chains. There are π-π stacking interactionsbetween guest-template2,2′-bipyridine molecules and isophthalate ligands. Thethree-dimensional (3D) networks of the compound13-15are formed by one-dimensional(1D) double chains through π-π stacking interactions. This is the first time to synthesize rareearth coordination polymers in which2,2′-bipyridine molecules serve as auxiliary ligandsand templates. The emission spectra show that11emits intense sharp red light and12emitsintense sharp green light when they are excited by different wavelength ultraviolet light.
4. A novel rare earth coordination polymer {(bpy)0.5[Re3(ip)4(phen)4(H_2O)]·2H_2O}n(Re=Dy(16), bpy=2,2′-bipyridine, ip=isophthalate, phen=1,10-phenanthroline) have beensynthesized by using1,10-phenanthroline molecules as auxiliary ligands and2,2′-bipyridinemolecules formed in situ reaction as templates. In the compound16, the isophthalate ligandslink the metal ions to form two-dimensional (2D) layer structures. The2,2′-bipyridinemolecules serve as guest-templates which located between the layers.1,10-phenanthrolinemolecules chelate metal ions. There are π-π stacking interactions between guest-template2,2′-bipyridine molecules and1,10-phenanthroline molecules. The three-dimensional (3D)network of the compound16is formed by two-dimensional (2D) layers through π-π stacking interactions. This is the first time to synthesize mixed-valence rare earth coordinationpolymer, and the first time to find1,10-phenanthroline can be transformed into2,2′-bipyridine under hydrothermal conditions in the presence of metal ions. The emissionspectra show that16emits blue light when it is excited by different wavelength ultravioletlight.
5. A series of novel rare earth coordination polymers [Re2(ip)2(pic)2]n(Re=Pr(17),Nd(18), Eu(19), Tb(20) and Ho(21), ip=isophthalate, pic=picolinate) have been synthesizedby using isophthalate ligands and picolinate ligands as mixed ligands, and2,2′-bipyridinemolecules or imdazole cations as templates. This series of compounds are isostructural. Theisophthalate ligands link the metal ions to form one-dimensional (1D) single chains anddouble chains, respectively. The picolinate ligands link these single chains and double chainsto form two kinds of layer structures, respectively. Two kinds of layer structures are furtherlinked by sharing metal ions to form the three-dimensional (3D) net structure. The emissionspectra show that19emits intense sharp red light and20emits intense sharp green lightwhen they are excited by different wavelength ultraviolet light.
We have successfully used templates to synthesize coordination polymers withisophthalate ligands in this dissertation. We believe this dissertation has an importantguiding function for the syntheses of novel coordination polymers with other ligands,especially for the syntheses of isomers of coordination polymers.
引文
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