新的含酰肼分子化合物的合成与结构性质研究
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摘要
本论文主要利用多羧酸与水合肼间的水热原位酰化反应，以不同的金属盐为原料，草酸为第二连接体，1,10-邻菲咯啉、2,2′-联吡啶等为辅助配体，合成出30个单(双)酰肼类配位化合物及2个酰肼分子，其中31个为新化合物。
1.利用水热原位酰化/还原反应，选取不同的芳香二甲酸，合成出9个芳香类单酰肼配位聚合物1-2，4-10及1个单酰肼分子3。1-3为含4,5-二氯邻苯二甲酰肼(DCPTH)的化合物。1是以phen为辅助配体，两种配位模式不同的DCPTH交替连接形成的单链Pb(Ⅱ)化合物。2是以bpy为辅助配体，DCPTH及4,5-二氯邻苯二甲酸根(dcph)混桥联的双链Cd(Ⅱ)化合物。值得注意的是，dcph分子也出现在该结构中，这是很罕见的。3为DCPTH配体。利用分子间氢键作用自组装为2-D超分子层。4-5为含3-甲基邻苯二甲酰肼(MPTH)的化合物。4是以phen为辅助配体，MPTH桥联的链状Pb(Ⅱ)化合物。5为MPTH配位的双核Cd(Ⅱ)化合物。6-8为含3-氨基邻苯二甲酰肼(APTH)的化合物。有趣的是，APTH由3-硝基邻苯二甲酰肼(NPTH)经水热原位还原反应而得。6与8分别为APTH桥联的层状Pb(Ⅱ)/Mn(Ⅱ)化合物。7为APTH配位的双核Cd(Ⅱ)化合物。6的二维层沿c方向呈波浪形。7利用分子间氢键作用自组装为1-D超分子链。8中APTH上氨基氮原子也与Mn(Ⅱ)配位。9-10为4-羧基邻苯二甲酰肼(CPTH)桥联的层状Pb(Ⅱ)配位聚合物。有趣的是，10是CPTH连接Pb-O带形成的具有一维孔道的2-D层状化合物，分子中出现了罕见的(H2O)8水簇。
2.利用水热原位酰化反应，选取不同的吡啶二甲羧酸，合成出12个吡啶类单酰肼配位化合物11-22。14-15为单链结构，18-19为双链结构，其余均为单核分子，但它们均通过吡啶单酰肼间的氢键作用自组装为有趣的超分子网络结构。
3.利用水热原位酰化反应，选取不同的芳香四甲酸，合成出7个双酰肼类配位聚合物23-24，26-30及一个双酰肼分子25。23-25为含4,4′-氧代双邻苯二甲酰肼(ODPTH)的化合物。23为ODPTH配位的双核Pb(Ⅱ)分子，ODPTH呈V型排列。24为ODPTH桥联的链状Cd(Ⅱ)化合物。25为ODPTH配体，V型排列，利用氢键作用自组装为3-D超分子网络结构。26是唯一一例以phen为辅助配体，4,4′-双邻苯二甲酰肼(BPTH)桥联的双链Cd(Ⅱ)化合物。若将BPTH看作一个连接点，则双链呈楼梯状。27-29为含4,4′-酮腙双邻苯二甲酰肼(DPHKH)的化合物。值得注意的是，在27-29的合成中还发生了另外一种水热原位反应：即羰基与水合肼间的亲核加成反应。27为DPHKH配位的双核Pb(Ⅱ)化合物，Pb(Ⅱ)位于半球型配位场中。28与29分别是以phen为辅助配体，DPHKH桥联的链状Cd(Ⅱ)/Zn(Ⅱ)化合物。30是以phen为辅助配体，4,4′-亚砜双邻苯二甲酰肼(SDPTH)桥联的链状Cd(Ⅱ)化合物。
4.利用水热原位酰化反应，选取两种不同的芳香/吡啶二甲酸，同时向体系中掺入第二连接体草酸，合成出2个草酸根(ox)拓展的单酰肼Cd(Ⅱ)配位聚合物31-32。31是以bpy为辅助配体，ox-拓展的链状Cd~(2+)-PTH(PTH=邻苯二甲酰肼)化合物。32为ox-拓展的二维层状Cd~(2+)-PDH(PDH=2,3-吡啶二甲酰肼)配位聚合物，该层沿b方向呈波浪型，ox采取了特殊的μ6配位模式。
5.讨论了反应体系的pH值、有机胺等因素对晶体生长的影响。解析了单晶结构，分析了酰肼分子的配位模式、价态、探讨了反应机理。并对所合成的化合物进行了元素分析、红外、XRD、热重、荧光、磁性等表征，利用DFT理论计算对发光机理进行探讨，为探索配位化合物结构与性能的关系积累了一定的理论数据。
The study on the novel coordination polymers is of current hot topic due to the structuraldiversity and the potential functional properties in adsorption, optics and magnetism. In situ ligandsynthesis has got considerable attention as an effective approach towards the crystal engineeringof coordination polymers. Some unusual organic ligands have been synthesized successfully,which are inaccessible or not easily obtainable via conventional methods. The hydrothermal in situacylation reactions between the organic polycarboxylic acids and N_2H_4H_2O is one of the mostimportant kinds, which provide a new approach to obtain a series of coordinated polymerscontaining novel structure and excellent properties. However, less attention has been paid to thisreaction until now.
Based on this mechanism, we synthesized thirty di(mono)acylhydrazidate-coordinatedcomplexes as well as two acylhydrazide molecules by the simple hydrothermal self-assembliesbetween metal salts, organic polycarboxylic acids and N_2H_4H_2O sometimes in the presence ofH_2ox, phen or bpy. We discussed the influence of pH and organic N-donor ligands etc. Not onlyresolved their single-crystal structure, also characterized them by element analysis, IR, XRD, TG,fluorescence spectra and magnetism. In order to understand the emission mechanism, the densityfunctional theory (DFT) calculations were carried out on the excited electronic states of somecompounds, which would supply theory basis between the relations of structures and functions forcoordination polymers. The paper includes seven chapters.
In the first chapter, firstly, we concisely introduced the concepts, histories and sorts ofcoordination polymers. Secondly, we emphasized the mechanism and sorts of thehydro(solvo)thermal in situ ligand syntheses. Finally, we explained the research significance,innovation and the results in this paper.
In the second chapter, we introduced the principle, methods and the reagent.
In the third chapter, nine aromatic-monoacylhydrazidate-coordinated polymers as well as onemonoacylhydrazide molecule have been synthesized from the hydrothermal in situ acylationreactions:[Pb_2(DCPTH)_4(phen)_2](1),[Cd_3(DCPTH)_2(dcph)_2(bpy)_2](2),[H(DCPTH)](3),[Pb_2(MPTH)_4(phen)_2](4),[Cd_2(MPTH)_4(phen)_2] H_2O (5),[Pb(APTH)_2]0.25H_2O (6),[Cd_2(APTH)_4(phen)_2]2H_2O (7),[Mn(APTH)_2(H_2O)](8),[Pb(CPTH)(phen)](9),[Pb_4(OH)_2(H_2O)_3(CPTH)_3]·2H_2O (10)(DCPTH=4,5-dichlorophthalhydrazidate, dcph=4,5-dichlorophthalate, MPTH=3-methylphthalhydrazidate, APTH=3-amiophthalhydrazidate,CPTH=4-carboxylphthalhydrazidate, phen=1,10-phenanthroline, bpy=2,2′-bipyridine). In them, APTH derived from the hydrothermal in situ reduction reaction of NPTH(3-nitrophthalhydrazidate), whereas the others derived respectively from the hydrothermal in situacylation reactions of corresponding organic polycarboxylic acids with hydrazine hydrate.Compounds1-3are containing DCPTH complexes. Compound1is a DCPTH-bridged chainedPb(Ⅱ) compound, with ancillary phen. It propagated into a3-D supramolecular network via π πinteractions and hydrogen-bonded interactions. Compound2is a DCPTH and dcph mixed bridgedchained Cd(Ⅱ) compound, with ancillary bpy. It is interesting that dcph also appeared in the finalframework of it. The π π interactions and hydrogen-bonded interactions make the crystalstructure more stabilizing. Compound3is only a monoacylhydrazide ligands. It propagated into a2-D supramolecular layer structure via intermolecular N-H O interactions between the acylaminogroups. Compounds4-5are containing MPTH inorganic coordination polymers. Compound4is aMPTH-bridged chained Pb(Ⅱ) compound, with ancillary phen. It propagated into a2-Dsupramolecular layer via π π interactions. Compound5is a MPTH-coordinated dinuclear Cd(Ⅱ)compound. It propagated into a1-D supramolecular chain via the O Ow interaction between theacylamino O atom and the lattice water molecule. Compounds6-8are containing APTH inorganiccoordination polymers. Compound6and8are APTH-bridged layered Pb(Ⅱ)/Mn(Ⅱ) coordinationpolymers. Compound7is an APTH-containing dinuclear Cd(Ⅱ) complex with ancillary phenmolecule. The2-D layer of compound6shows a wave-type, running down the c direction. It self-assembles into a3-D supramolecular network via the intermolecular N-H O interactions.Compound7self-assembles into a1-D supramolecular chain via hydrogen-bonded. Interestingly,in compound8, the amino N atom of APTH Ⅱ is also involved in the coordination to the Mn(Ⅱ)center. Compound9-10are CPTH-bridged layered Pb(Ⅱ) coordination polymers. Compound9self-assembles into a3-D supramolecular chain via π π interactions. Compound10areCPTH-bridged layered Pb(Ⅱ) coordination polymer with1-D Pb-O ribbons.There is a (H_2O)8dimer. It self-assembles into a3-D supramolecular network via hydrogen-bonded.
In the fourth chapter, twelve pyridine-monoacylhydrazidate-coordinated complexes havebeen synthesized from the hydrothermal in situ acylation reactions:[Zn(PDH)_2(H_2O)_2](11),[Cd(PDH)_2(H_2O)_2](12),[Pb(MPDH)_2](13),[Cd(MPDH)_2](14),[Mn(MPDH)_2](15),[Co(MPDH)_2(H_2O)_2]2H_2O (16),[Zn(MPDH)_2(H_2O)_2]2H_2O (17),[Pb_2(EPDH)_4(H_2O)](18),[Cd(EPDH)_2(H_2O)](19),[Mn(EPDH)_2(H_2O)_2](20),[Co(EPDH)_2(H_2O)_2](21),[Zn(EPDH)_2(H_2O)_2](22),(PDH=pyridine-2,3-dicarboxylhydrazidate, MPDH=6-methylpyridine-2,3-dicarboxylhydrazidate, EPDH=5-ethylpyridine-2,3-dicarboxylhydrazidate).Note that the acylhydrazidate all derived respectively from the hydrothermal in situ acylationreactions of corresponding organic polycarboxylic acids with hydrazine hydrate. Compounds14-15are1-D single-chained and18-19are1-D double-chained coordination polymers, the othersare the mononuclear molecular entities, but they all further self-assemble into the interestingsupramolecular networks via hydrogen-bonded interactions between pyridine-monoacyl hydrazidate ligands.
In the fifth chapter, seven diacylhydrazidate-coordinated polymers as well as onediacylhydrazide molecule have been synthesized from the hydrothermal in situ acylation reactions:[Pb_2(ODPTH)_2(phen)_2(H_2O)_2](23),[Cd(ODPTH)(phen)]0.25H_2O (24),[H_2(ODPTH)](25),[Cd(BPTH)(phen)]3.75H_2O (26),[Pb_2(DPHKH)_2(phen)_2]2H_2O (27),[Cd_2(DPHKH)_2(phen)]1.75H_2O (28),[Zn_3(DPHKH)_2(HDPHKH)_2(phen)_2]8H_2O (29),[Cd(SDPTH)(phen)(H_2O)] H_2O (30)(ODPTH=4,4′-oxydiphthalhydrazidate, BPTH=4,4′-biphthalhydrazidate, DPHKH=4,4′-diphthalhydrazidatoketone hydrazone, SDPTH=4,4′-sulfoyldiphthalhydrazidate). Note that the diacylhydrazidate molecules in compounds23-30originated from the in situ acylation reactions between organic polycarboxylic acids andN_2H_4H_2O. Interestingly, another kind of ligand in situ reaction was found in the formation processof DPHKH in compounds27-29: the nucleophilic addition reaction of the keto with N_2H_4H_2O.Compounds23-25are containing ODPTH complexes. Compound23is an ODPTH-coordinateddinuclear Pb(Ⅱ) complex. It self-assembles into a2-D supramolecular layers via hydrogen-bonded.Compound24is an ODPTH-bridged chained Cd(Ⅱ) compound. Via the π π interactions betweenthe adjacent phen rings, the1-D chains further self-assemble into a2-D supramolecular sheet.Compound25is a new organic diacylhydrazide molecule. ODPTH shows a V-shape. Itself-assembles into a3-D supramolecular network through weak interactions. Compound26is aunique BPTH-bridged1-D double-chain Cd(Ⅱ) compound. Compounds27-29are containingDPHKH inorganic coordination polymers. Compound27is a DPHKH-coordinated Pb(Ⅱ)dinuclear compound. Pb(Ⅱ) is involved in a hemisphere-coordinated site. It is only extended into a1-D supramolecular chain owning to only one acylamino group head-to-head hydrogen bonds tothe adjacent acylamino group producing a hydrogen-bonded dimmer. Compound28and29areDPHKH-propagated chained Cd(Ⅱ)/Zn(Ⅱ) compounds with auxiliary phen molecule. Compound30is a SDPTH-extended chained Cd(Ⅱ) compound with auxiliary phen molecule.
In the sixth chapter, two ox-extended Cd_2+-monoacylhydrazidate coordinated polymers havebeen first synthesized from the hydrothermal in situ acylation reactions:[Cd_2(ox)0.5(HPTH)(PTH)(bpy)_2](31),[Cd_2(ox)(PDH)_2] H_2O (32)(PTH=phthalhydrazidate, PDH=pyridine-2,3-dicarboxylhydrazidate, bpy=2,2′-bipyridine). Note that the acylhydrazidate allderived respectively from the hydrothermal in situ acylation reactions of corresponding organicpolycarboxylic acids with hydrazine hydrate. Compound31is an ox-extended chained Cd_2+-PTHcoordination polymer with ancillary bpy molecules. Neighboring bpy molecules between thechains form the π π packing, propagate the one-dimensional chains into a two-dimensionalsupramolecular layer. Compound32is an ox-propagated layered Cd_2+-PDH coordination polymer.The layer exhibits a wave-like shape, extending along the b-axial direction. Noteworthily, oxexhibits a special μ6coordination mode.
The solid-state fluorescence spectra show compounds1-3,5,7,9-14,17-19,22-25,30,32 possess good fluorescence emissions. They are the potential fluorescence materials. DFTcalculations have been applied to better understand the emission mechanism of compounds3,11,13,17,32. Two kinds of new charge-transfer paths are found in acylhydrazidate-coordinatedcompounds. Photoluminescence property in aqueous solutions have been studied on compounds4-5，23-25，27-30, all possess good fluorescence emissions, the charge transfer within the phenmolecule should be responsible for the emissions. Magnetic susceptibility datas for compounds8and20indicate antiferromagnetic interactions between Mn(Ⅱ) centers.
In the seventh chapter, a brief conclusion and outlook are given.
1.利用水热原位酰化/还原反应，选取不同的芳香二甲酸，合成出9个芳香类单酰肼配位聚合物1-2，4-10及1个单酰肼分子3。1-3为含4,5-二氯邻苯二甲酰肼(DCPTH)的化合物。1是以phen为辅助配体，两种配位模式不同的DCPTH交替连接形成的单链Pb(Ⅱ)化合物。2是以bpy为辅助配体，DCPTH及4,5-二氯邻苯二甲酸根(dcph)混桥联的双链Cd(Ⅱ)化合物。值得注意的是，dcph分子也出现在该结构中，这是很罕见的。3为DCPTH配体。利用分子间氢键作用自组装为2-D超分子层。4-5为含3-甲基邻苯二甲酰肼(MPTH)的化合物。4是以phen为辅助配体，MPTH桥联的链状Pb(Ⅱ)化合物。5为MPTH配位的双核Cd(Ⅱ)化合物。6-8为含3-氨基邻苯二甲酰肼(APTH)的化合物。有趣的是，APTH由3-硝基邻苯二甲酰肼(NPTH)经水热原位还原反应而得。6与8分别为APTH桥联的层状Pb(Ⅱ)/Mn(Ⅱ)化合物。7为APTH配位的双核Cd(Ⅱ)化合物。6的二维层沿c方向呈波浪形。7利用分子间氢键作用自组装为1-D超分子链。8中APTH上氨基氮原子也与Mn(Ⅱ)配位。9-10为4-羧基邻苯二甲酰肼(CPTH)桥联的层状Pb(Ⅱ)配位聚合物。有趣的是，10是CPTH连接Pb-O带形成的具有一维孔道的2-D层状化合物，分子中出现了罕见的(H2O)8水簇。
2.利用水热原位酰化反应，选取不同的吡啶二甲羧酸，合成出12个吡啶类单酰肼配位化合物11-22。14-15为单链结构，18-19为双链结构，其余均为单核分子，但它们均通过吡啶单酰肼间的氢键作用自组装为有趣的超分子网络结构。
3.利用水热原位酰化反应，选取不同的芳香四甲酸，合成出7个双酰肼类配位聚合物23-24，26-30及一个双酰肼分子25。23-25为含4,4′-氧代双邻苯二甲酰肼(ODPTH)的化合物。23为ODPTH配位的双核Pb(Ⅱ)分子，ODPTH呈V型排列。24为ODPTH桥联的链状Cd(Ⅱ)化合物。25为ODPTH配体，V型排列，利用氢键作用自组装为3-D超分子网络结构。26是唯一一例以phen为辅助配体，4,4′-双邻苯二甲酰肼(BPTH)桥联的双链Cd(Ⅱ)化合物。若将BPTH看作一个连接点，则双链呈楼梯状。27-29为含4,4′-酮腙双邻苯二甲酰肼(DPHKH)的化合物。值得注意的是，在27-29的合成中还发生了另外一种水热原位反应：即羰基与水合肼间的亲核加成反应。27为DPHKH配位的双核Pb(Ⅱ)化合物，Pb(Ⅱ)位于半球型配位场中。28与29分别是以phen为辅助配体，DPHKH桥联的链状Cd(Ⅱ)/Zn(Ⅱ)化合物。30是以phen为辅助配体，4,4′-亚砜双邻苯二甲酰肼(SDPTH)桥联的链状Cd(Ⅱ)化合物。
4.利用水热原位酰化反应，选取两种不同的芳香/吡啶二甲酸，同时向体系中掺入第二连接体草酸，合成出2个草酸根(ox)拓展的单酰肼Cd(Ⅱ)配位聚合物31-32。31是以bpy为辅助配体，ox-拓展的链状Cd~(2+)-PTH(PTH=邻苯二甲酰肼)化合物。32为ox-拓展的二维层状Cd~(2+)-PDH(PDH=2,3-吡啶二甲酰肼)配位聚合物，该层沿b方向呈波浪型，ox采取了特殊的μ6配位模式。
5.讨论了反应体系的pH值、有机胺等因素对晶体生长的影响。解析了单晶结构，分析了酰肼分子的配位模式、价态、探讨了反应机理。并对所合成的化合物进行了元素分析、红外、XRD、热重、荧光、磁性等表征，利用DFT理论计算对发光机理进行探讨，为探索配位化合物结构与性能的关系积累了一定的理论数据。
The study on the novel coordination polymers is of current hot topic due to the structuraldiversity and the potential functional properties in adsorption, optics and magnetism. In situ ligandsynthesis has got considerable attention as an effective approach towards the crystal engineeringof coordination polymers. Some unusual organic ligands have been synthesized successfully,which are inaccessible or not easily obtainable via conventional methods. The hydrothermal in situacylation reactions between the organic polycarboxylic acids and N_2H_4H_2O is one of the mostimportant kinds, which provide a new approach to obtain a series of coordinated polymerscontaining novel structure and excellent properties. However, less attention has been paid to thisreaction until now.
Based on this mechanism, we synthesized thirty di(mono)acylhydrazidate-coordinatedcomplexes as well as two acylhydrazide molecules by the simple hydrothermal self-assembliesbetween metal salts, organic polycarboxylic acids and N_2H_4H_2O sometimes in the presence ofH_2ox, phen or bpy. We discussed the influence of pH and organic N-donor ligands etc. Not onlyresolved their single-crystal structure, also characterized them by element analysis, IR, XRD, TG,fluorescence spectra and magnetism. In order to understand the emission mechanism, the densityfunctional theory (DFT) calculations were carried out on the excited electronic states of somecompounds, which would supply theory basis between the relations of structures and functions forcoordination polymers. The paper includes seven chapters.
In the first chapter, firstly, we concisely introduced the concepts, histories and sorts ofcoordination polymers. Secondly, we emphasized the mechanism and sorts of thehydro(solvo)thermal in situ ligand syntheses. Finally, we explained the research significance,innovation and the results in this paper.
In the second chapter, we introduced the principle, methods and the reagent.
In the third chapter, nine aromatic-monoacylhydrazidate-coordinated polymers as well as onemonoacylhydrazide molecule have been synthesized from the hydrothermal in situ acylationreactions:[Pb_2(DCPTH)_4(phen)_2](1),[Cd_3(DCPTH)_2(dcph)_2(bpy)_2](2),[H(DCPTH)](3),[Pb_2(MPTH)_4(phen)_2](4),[Cd_2(MPTH)_4(phen)_2] H_2O (5),[Pb(APTH)_2]0.25H_2O (6),[Cd_2(APTH)_4(phen)_2]2H_2O (7),[Mn(APTH)_2(H_2O)](8),[Pb(CPTH)(phen)](9),[Pb_4(OH)_2(H_2O)_3(CPTH)_3]·2H_2O (10)(DCPTH=4,5-dichlorophthalhydrazidate, dcph=4,5-dichlorophthalate, MPTH=3-methylphthalhydrazidate, APTH=3-amiophthalhydrazidate,CPTH=4-carboxylphthalhydrazidate, phen=1,10-phenanthroline, bpy=2,2′-bipyridine). In them, APTH derived from the hydrothermal in situ reduction reaction of NPTH(3-nitrophthalhydrazidate), whereas the others derived respectively from the hydrothermal in situacylation reactions of corresponding organic polycarboxylic acids with hydrazine hydrate.Compounds1-3are containing DCPTH complexes. Compound1is a DCPTH-bridged chainedPb(Ⅱ) compound, with ancillary phen. It propagated into a3-D supramolecular network via π πinteractions and hydrogen-bonded interactions. Compound2is a DCPTH and dcph mixed bridgedchained Cd(Ⅱ) compound, with ancillary bpy. It is interesting that dcph also appeared in the finalframework of it. The π π interactions and hydrogen-bonded interactions make the crystalstructure more stabilizing. Compound3is only a monoacylhydrazide ligands. It propagated into a2-D supramolecular layer structure via intermolecular N-H O interactions between the acylaminogroups. Compounds4-5are containing MPTH inorganic coordination polymers. Compound4is aMPTH-bridged chained Pb(Ⅱ) compound, with ancillary phen. It propagated into a2-Dsupramolecular layer via π π interactions. Compound5is a MPTH-coordinated dinuclear Cd(Ⅱ)compound. It propagated into a1-D supramolecular chain via the O Ow interaction between theacylamino O atom and the lattice water molecule. Compounds6-8are containing APTH inorganiccoordination polymers. Compound6and8are APTH-bridged layered Pb(Ⅱ)/Mn(Ⅱ) coordinationpolymers. Compound7is an APTH-containing dinuclear Cd(Ⅱ) complex with ancillary phenmolecule. The2-D layer of compound6shows a wave-type, running down the c direction. It self-assembles into a3-D supramolecular network via the intermolecular N-H O interactions.Compound7self-assembles into a1-D supramolecular chain via hydrogen-bonded. Interestingly,in compound8, the amino N atom of APTH Ⅱ is also involved in the coordination to the Mn(Ⅱ)center. Compound9-10are CPTH-bridged layered Pb(Ⅱ) coordination polymers. Compound9self-assembles into a3-D supramolecular chain via π π interactions. Compound10areCPTH-bridged layered Pb(Ⅱ) coordination polymer with1-D Pb-O ribbons.There is a (H_2O)8dimer. It self-assembles into a3-D supramolecular network via hydrogen-bonded.
In the fourth chapter, twelve pyridine-monoacylhydrazidate-coordinated complexes havebeen synthesized from the hydrothermal in situ acylation reactions:[Zn(PDH)_2(H_2O)_2](11),[Cd(PDH)_2(H_2O)_2](12),[Pb(MPDH)_2](13),[Cd(MPDH)_2](14),[Mn(MPDH)_2](15),[Co(MPDH)_2(H_2O)_2]2H_2O (16),[Zn(MPDH)_2(H_2O)_2]2H_2O (17),[Pb_2(EPDH)_4(H_2O)](18),[Cd(EPDH)_2(H_2O)](19),[Mn(EPDH)_2(H_2O)_2](20),[Co(EPDH)_2(H_2O)_2](21),[Zn(EPDH)_2(H_2O)_2](22),(PDH=pyridine-2,3-dicarboxylhydrazidate, MPDH=6-methylpyridine-2,3-dicarboxylhydrazidate, EPDH=5-ethylpyridine-2,3-dicarboxylhydrazidate).Note that the acylhydrazidate all derived respectively from the hydrothermal in situ acylationreactions of corresponding organic polycarboxylic acids with hydrazine hydrate. Compounds14-15are1-D single-chained and18-19are1-D double-chained coordination polymers, the othersare the mononuclear molecular entities, but they all further self-assemble into the interestingsupramolecular networks via hydrogen-bonded interactions between pyridine-monoacyl hydrazidate ligands.
In the fifth chapter, seven diacylhydrazidate-coordinated polymers as well as onediacylhydrazide molecule have been synthesized from the hydrothermal in situ acylation reactions:[Pb_2(ODPTH)_2(phen)_2(H_2O)_2](23),[Cd(ODPTH)(phen)]0.25H_2O (24),[H_2(ODPTH)](25),[Cd(BPTH)(phen)]3.75H_2O (26),[Pb_2(DPHKH)_2(phen)_2]2H_2O (27),[Cd_2(DPHKH)_2(phen)]1.75H_2O (28),[Zn_3(DPHKH)_2(HDPHKH)_2(phen)_2]8H_2O (29),[Cd(SDPTH)(phen)(H_2O)] H_2O (30)(ODPTH=4,4′-oxydiphthalhydrazidate, BPTH=4,4′-biphthalhydrazidate, DPHKH=4,4′-diphthalhydrazidatoketone hydrazone, SDPTH=4,4′-sulfoyldiphthalhydrazidate). Note that the diacylhydrazidate molecules in compounds23-30originated from the in situ acylation reactions between organic polycarboxylic acids andN_2H_4H_2O. Interestingly, another kind of ligand in situ reaction was found in the formation processof DPHKH in compounds27-29: the nucleophilic addition reaction of the keto with N_2H_4H_2O.Compounds23-25are containing ODPTH complexes. Compound23is an ODPTH-coordinateddinuclear Pb(Ⅱ) complex. It self-assembles into a2-D supramolecular layers via hydrogen-bonded.Compound24is an ODPTH-bridged chained Cd(Ⅱ) compound. Via the π π interactions betweenthe adjacent phen rings, the1-D chains further self-assemble into a2-D supramolecular sheet.Compound25is a new organic diacylhydrazide molecule. ODPTH shows a V-shape. Itself-assembles into a3-D supramolecular network through weak interactions. Compound26is aunique BPTH-bridged1-D double-chain Cd(Ⅱ) compound. Compounds27-29are containingDPHKH inorganic coordination polymers. Compound27is a DPHKH-coordinated Pb(Ⅱ)dinuclear compound. Pb(Ⅱ) is involved in a hemisphere-coordinated site. It is only extended into a1-D supramolecular chain owning to only one acylamino group head-to-head hydrogen bonds tothe adjacent acylamino group producing a hydrogen-bonded dimmer. Compound28and29areDPHKH-propagated chained Cd(Ⅱ)/Zn(Ⅱ) compounds with auxiliary phen molecule. Compound30is a SDPTH-extended chained Cd(Ⅱ) compound with auxiliary phen molecule.
In the sixth chapter, two ox-extended Cd_2+-monoacylhydrazidate coordinated polymers havebeen first synthesized from the hydrothermal in situ acylation reactions:[Cd_2(ox)0.5(HPTH)(PTH)(bpy)_2](31),[Cd_2(ox)(PDH)_2] H_2O (32)(PTH=phthalhydrazidate, PDH=pyridine-2,3-dicarboxylhydrazidate, bpy=2,2′-bipyridine). Note that the acylhydrazidate allderived respectively from the hydrothermal in situ acylation reactions of corresponding organicpolycarboxylic acids with hydrazine hydrate. Compound31is an ox-extended chained Cd_2+-PTHcoordination polymer with ancillary bpy molecules. Neighboring bpy molecules between thechains form the π π packing, propagate the one-dimensional chains into a two-dimensionalsupramolecular layer. Compound32is an ox-propagated layered Cd_2+-PDH coordination polymer.The layer exhibits a wave-like shape, extending along the b-axial direction. Noteworthily, oxexhibits a special μ6coordination mode.
The solid-state fluorescence spectra show compounds1-3,5,7,9-14,17-19,22-25,30,32 possess good fluorescence emissions. They are the potential fluorescence materials. DFTcalculations have been applied to better understand the emission mechanism of compounds3,11,13,17,32. Two kinds of new charge-transfer paths are found in acylhydrazidate-coordinatedcompounds. Photoluminescence property in aqueous solutions have been studied on compounds4-5，23-25，27-30, all possess good fluorescence emissions, the charge transfer within the phenmolecule should be responsible for the emissions. Magnetic susceptibility datas for compounds8and20indicate antiferromagnetic interactions between Mn(Ⅱ) centers.
In the seventh chapter, a brief conclusion and outlook are given.
引文
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