含氮、氧配体及多核配合物的设计合成、结构和性质
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摘要
多核金属配合物已成为当今配位化学研究领域中最活跃的热门课题之一,不仅是因为它们具有纳米尺寸的分子结构,而且还表现出有趣的光、电、磁以及催化等性质。目前的研究绝大多数集中在过渡金属配合物上,过渡-稀土金属配合物的研究相对较少。本论文设计合成了以下过渡金属配合物和过渡-稀土金属多核配合物,并对其结构和性质进行了研究。主要内容如下:
(1)以3-羧基水杨醛和2-甲基-2-氨基-1,3-丙二醇为原料,通过缩合反应制得了一种新的Schiff碱配体H4L1[H4L1=3-羧基水杨醛缩二羟甲基甲胺],利用该配体与Co盐反应,得到了三个四核钴的配合物[Co(HL1)]_4·4H_2O (1)、[Co(HL1)]_4·2CH_3OH·1.32H_2O (2)和[Co_2 (L1)(N_3)]_2·4CH_3OH (3),其中(3)是一个具有混合价态的配合物。通过元素分析、红外光谱、紫外-可见光谱和X-射线单晶衍射对其晶体结构进行了表征。
(2)以3-羧基水杨醛作为主配体(H_2L2) ,加入一些适当的辅助配体,与Cu(ClO_4)_2·6H_2O反应,得到了四个铜的配合物[(CuL2)(2,2’-bpy)(H_2O)] (4)、{[(CuL2)(2,2’- bpy)]_2Cu(2,2’-bpy)·2ClO_4}_n (5)、[Cu(HL2)(L2)(2,2’-bpy)]_2 (6)和[(CuL2)_2·(bbi)·2ClO_4·4H_2O] (7)[bbi=1,1’-(1,4-Butanediyl)bis(imidazole)]。通过元素分析、红外光谱、紫外-可见光谱和X-射线单晶衍射对其晶体结构进行了表征。变温磁化率测定表明配合物(5)和(7)的金属离子之间均为反铁磁相互作用。
(3)用3-羧基水杨醛和二丙烯三胺为原料,通过合反应制得了一种含有多个配位点的柔性配体H_5L3[H_5L3=N-N’-二-(3-羧基水杨醛)缩二丙烯三胺],利用该配体合成了配合物[Cu(H2_L3)] (8)和一维螺旋链配合物{[(Cu_2L3)(H_2O)]_2·5H_2O}_n (9)。通过元素分析、红外光谱、紫外-可见光谱、荧光光谱、X-射线单晶衍射以及热分析对配合物的结构、性质进行了研究。
(4)用3-羧基水杨醛和三乙基四胺反应制得了一种结构新颖的多齿席夫碱配体H_6L4[H_6L4=N,N′,N″-三-(3-羧基水杨醛)缩三乙基四胺],利用该配体与MnCl_2·4H_2O反应,通过分子自组装的方法得到了一个双核锰的化合物[Mn_2(HL4)]·DMF·1.13H_2O (10);同时合成了该配体的镍单核配合物NiL4,并以此单核配合物为金属单元片段,得到了一个过渡-稀土混合异金属的六核配合物[Ni_2Eu(L4)(H_2O)_2]_2.9H_2O (11),通过X-射线单晶衍射分别测定了配合物的结构,并对其性质进行了研究。
Polynuclear metal complexes is one of the most active research topics of current coordination chemistry, not only because of their nanoscale and aesthetically pleasing molecular structures, but also because of their interesting luminescent, electronic, magnetic and catalytic properties. However, most of the works have so far been focused on polynuclear transistion metal complexes, while heterometallic 3d-4f clusters have seldom explored. In view of thinking, we have designed and synthesized several transition metal complexes and 3d-4f polynuclear clusters, and the crystal structure and properties were investigated. The main contents are following:
(1) Through condensing 3-carboxysalicylidene and 2-methyl-2-amino-1,3-propanediol, one new Schiff base H4L1[H4L1=(E)-3-((1,3-dihydroxy-2-methylpropan-2-ylimino)methyl)-2-hydroxybenzoic acid], using the ligand, we have synthesized three cobalt complexes [Co(HL1)]_4·4H_2O (1), [Co(HL1)]_4·2CH_3OH·1.32H_2O (2) and [Co_2(L1)(N_3)]_2·4CH_3OH (3), complex 3 is a mixed-valence tetranuclear cobalt clusters. Their crystal structures were characterized by elemental analysis, IR, UV and X-ray diffraction.
(2) Using the ligand H_2L2 [H_2L2=3-carboxysalicylidene] and Cu(ClO_4)_2·6H_2O, under the right conditions to add some ancillary ligands, the compounds [(CuL2)(2,2’-bpy)(H_2O)] (4), {[(CuL2)(2,2’-bpy)]_2Cu(2,2’-bpy)·2ClO_4}_n (5), [Cu(HL2)(L2)(2,2’-bpy)]_2 (6) and [(CuL2)_2(bbi)·2ClO_4·4H_2O] (7)[bbi=1,1’-(1,4-Butanediyl)bis(imidazole)] have been synthesized. Their crystal structures were characterized by elemental analysis, IR, UV and X-ray diffraction. Magnetic susceptibility of measurements for (5) and (7) indicaste that the interaction between metal ions are antiferromagnetic.
(3) Using 3-carboxysalicylidene and N~1-(3-aminopropyl)propane-1,3-diamine, we have prepared the flexible ligand H_5L3[H_5L3=3,3′-(1Z,1′Z)-(3,3′-azanediylbis(propane-3,1-diyl)bis(azan-1-yl-1-ylidene))bis(methan-1-yl-1-ylidene)bis(2-hydroxybenzoic acid)], the compounds [Cu(H_2L3)] (8) and 1D helical chain {[(Cu_2L3)(H_2O)]_2·5H_2O}_n (9) were synthesized from H_5L3. Their structures were characterized by elemental analysis, IR, UV, fluorescence spectroscopy, X-ray diffraction and thermal analysis.
(4) Through condensing 3-carboxysalicylidene and triethylenetetramine, a new Schiff base ligand H_6L4 [H_6L4 = 3,3',3''-(1E,1'E,1''E)-(2,2',2''-nitrilotris(ethane-2,1- diyl)tris(azan-1-yl-1-ylidene))tris(methan-1-yl-1-ylidene)tris(2-hydroxybenzoic acid)] has been synthesized. Taking advantage of the MnCl_2·4H_2O, a binuclear manganese complex [Mn_2(HL4)]·DMF·1.13H_2O (10) as been obtained. While the mononuclear complex of nickel has also been obtained, through the self-assembly of mononuclear complex, we have synthesized heterohexanuclear complexes [Ni_2Eu(L4)(H_2O)_2]2.9H_2O (11), we studied their spectacular structures and properties.
(1)以3-羧基水杨醛和2-甲基-2-氨基-1,3-丙二醇为原料,通过缩合反应制得了一种新的Schiff碱配体H4L1[H4L1=3-羧基水杨醛缩二羟甲基甲胺],利用该配体与Co盐反应,得到了三个四核钴的配合物[Co(HL1)]_4·4H_2O (1)、[Co(HL1)]_4·2CH_3OH·1.32H_2O (2)和[Co_2 (L1)(N_3)]_2·4CH_3OH (3),其中(3)是一个具有混合价态的配合物。通过元素分析、红外光谱、紫外-可见光谱和X-射线单晶衍射对其晶体结构进行了表征。
(2)以3-羧基水杨醛作为主配体(H_2L2) ,加入一些适当的辅助配体,与Cu(ClO_4)_2·6H_2O反应,得到了四个铜的配合物[(CuL2)(2,2’-bpy)(H_2O)] (4)、{[(CuL2)(2,2’- bpy)]_2Cu(2,2’-bpy)·2ClO_4}_n (5)、[Cu(HL2)(L2)(2,2’-bpy)]_2 (6)和[(CuL2)_2·(bbi)·2ClO_4·4H_2O] (7)[bbi=1,1’-(1,4-Butanediyl)bis(imidazole)]。通过元素分析、红外光谱、紫外-可见光谱和X-射线单晶衍射对其晶体结构进行了表征。变温磁化率测定表明配合物(5)和(7)的金属离子之间均为反铁磁相互作用。
(3)用3-羧基水杨醛和二丙烯三胺为原料,通过合反应制得了一种含有多个配位点的柔性配体H_5L3[H_5L3=N-N’-二-(3-羧基水杨醛)缩二丙烯三胺],利用该配体合成了配合物[Cu(H2_L3)] (8)和一维螺旋链配合物{[(Cu_2L3)(H_2O)]_2·5H_2O}_n (9)。通过元素分析、红外光谱、紫外-可见光谱、荧光光谱、X-射线单晶衍射以及热分析对配合物的结构、性质进行了研究。
(4)用3-羧基水杨醛和三乙基四胺反应制得了一种结构新颖的多齿席夫碱配体H_6L4[H_6L4=N,N′,N″-三-(3-羧基水杨醛)缩三乙基四胺],利用该配体与MnCl_2·4H_2O反应,通过分子自组装的方法得到了一个双核锰的化合物[Mn_2(HL4)]·DMF·1.13H_2O (10);同时合成了该配体的镍单核配合物NiL4,并以此单核配合物为金属单元片段,得到了一个过渡-稀土混合异金属的六核配合物[Ni_2Eu(L4)(H_2O)_2]_2.9H_2O (11),通过X-射线单晶衍射分别测定了配合物的结构,并对其性质进行了研究。
Polynuclear metal complexes is one of the most active research topics of current coordination chemistry, not only because of their nanoscale and aesthetically pleasing molecular structures, but also because of their interesting luminescent, electronic, magnetic and catalytic properties. However, most of the works have so far been focused on polynuclear transistion metal complexes, while heterometallic 3d-4f clusters have seldom explored. In view of thinking, we have designed and synthesized several transition metal complexes and 3d-4f polynuclear clusters, and the crystal structure and properties were investigated. The main contents are following:
(1) Through condensing 3-carboxysalicylidene and 2-methyl-2-amino-1,3-propanediol, one new Schiff base H4L1[H4L1=(E)-3-((1,3-dihydroxy-2-methylpropan-2-ylimino)methyl)-2-hydroxybenzoic acid], using the ligand, we have synthesized three cobalt complexes [Co(HL1)]_4·4H_2O (1), [Co(HL1)]_4·2CH_3OH·1.32H_2O (2) and [Co_2(L1)(N_3)]_2·4CH_3OH (3), complex 3 is a mixed-valence tetranuclear cobalt clusters. Their crystal structures were characterized by elemental analysis, IR, UV and X-ray diffraction.
(2) Using the ligand H_2L2 [H_2L2=3-carboxysalicylidene] and Cu(ClO_4)_2·6H_2O, under the right conditions to add some ancillary ligands, the compounds [(CuL2)(2,2’-bpy)(H_2O)] (4), {[(CuL2)(2,2’-bpy)]_2Cu(2,2’-bpy)·2ClO_4}_n (5), [Cu(HL2)(L2)(2,2’-bpy)]_2 (6) and [(CuL2)_2(bbi)·2ClO_4·4H_2O] (7)[bbi=1,1’-(1,4-Butanediyl)bis(imidazole)] have been synthesized. Their crystal structures were characterized by elemental analysis, IR, UV and X-ray diffraction. Magnetic susceptibility of measurements for (5) and (7) indicaste that the interaction between metal ions are antiferromagnetic.
(3) Using 3-carboxysalicylidene and N~1-(3-aminopropyl)propane-1,3-diamine, we have prepared the flexible ligand H_5L3[H_5L3=3,3′-(1Z,1′Z)-(3,3′-azanediylbis(propane-3,1-diyl)bis(azan-1-yl-1-ylidene))bis(methan-1-yl-1-ylidene)bis(2-hydroxybenzoic acid)], the compounds [Cu(H_2L3)] (8) and 1D helical chain {[(Cu_2L3)(H_2O)]_2·5H_2O}_n (9) were synthesized from H_5L3. Their structures were characterized by elemental analysis, IR, UV, fluorescence spectroscopy, X-ray diffraction and thermal analysis.
(4) Through condensing 3-carboxysalicylidene and triethylenetetramine, a new Schiff base ligand H_6L4 [H_6L4 = 3,3',3''-(1E,1'E,1''E)-(2,2',2''-nitrilotris(ethane-2,1- diyl)tris(azan-1-yl-1-ylidene))tris(methan-1-yl-1-ylidene)tris(2-hydroxybenzoic acid)] has been synthesized. Taking advantage of the MnCl_2·4H_2O, a binuclear manganese complex [Mn_2(HL4)]·DMF·1.13H_2O (10) as been obtained. While the mononuclear complex of nickel has also been obtained, through the self-assembly of mononuclear complex, we have synthesized heterohexanuclear complexes [Ni_2Eu(L4)(H_2O)_2]2.9H_2O (11), we studied their spectacular structures and properties.
引文
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