以席夫碱和香草醛配体构筑3d-4f、3d-3d金属配位簇合物的合成、结构及磁性

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英文题名：Synthesis, Structures and Magnetic Properties of 3d-4f and 3d-3d Coordination Clusters Based on Schiff Base and Vanillin Ligands 作者：杨丹丹 论文级别：硕士 学科专业名称：化学 中文关键词：配位簇合物 ; 3d-4f ; 3d混金属 ; 单晶结构 ; 磁性 英文关键词：coordination compound ; 3d-4f ; 3d hetero-metal cluster ; crystal structure ; magnetic properties 学位年度：2011 导师：常菲 学科代码：070304 学位授予单位：内蒙古大学 论文提交日期：2011-06-01

摘要

本论文以设计合成金属配位簇合物、研究其磁性为目标,利用三个主配体：①四齿席夫碱H2salhyeten(水杨醛缩N-羟乙基乙二胺)；②三齿席夫碱H2salamp(水杨醛缩2-氨基-2-甲基-1-丙醇)；③双齿香草醛vanillin(3-甲氧基-4-羟基-苯甲醛),与过渡(3d)及稀土(4f)金属盐反应,通过辅助配体调节,采用溶液均相法、溶剂热法、常温扩散等方法首次合成出31个化合物,对其中的19个化合物进行了X-射线单晶衍射测试,分析结果如下：
     1:[Fe7Ⅲ(Salhyeten)6(μ3-O)3(CNS)]·(CH3OH)n(CNS)2
     2:[C2Ⅲ(Salhyeten)2(N3)2]
     3:[CrⅢ(Hsalhyeten)2](NO3)
     4:[Fe4ⅡFeⅢ(Salamp)4(μ5-O)(CNS)(μ2-OHCH3)4]
     5:[Fe4ⅡFeⅢLnⅢ(Salamp)4(μ4-O)2(Pic)(NO3)(CH3OH)6](CH3OH)(H2O) (Ln=Dy(5)、La(5a)、Pr(5b)、Nd(5c)、Sm(5d)、Eu(5e)、Gd(5f)、Tb(5g)、Er(5h)、Yb(5i))
     6:[Fe4ⅡLn2Ⅲ(μ4-O)2(Salamp)4(μ2-OHCH3)4(μ-OHCH3)2(H2O)4(CNS)2] (Ln=Sm(6)、La(6a)、Pr(6b)、Nd(6c)、Eu(6d、Gd(6e))
     7:[Co4ⅢLn2Ⅲ(Salamp)4(μ3-OCH3)2(μ-OCH3)2(μ-O2CCH3)6(CH3OH)2] (Ln=Nd(7)、Pr(7a))
     8:[Cu4Ⅱ(salamp)4]·3H2O
     9:[Cu4ⅡCo2Ⅱ(salamp)4(μ2-N3)4(μ3-OHCH3)2(CH3OH)2]
     10:[Co2ⅡNi2(Salamp)2(μ2-N3)2(μ-N3)2(μ3-OHCH3)2(μ-OHCH3)4]
     11:[Co4Ⅱ(Salamp)2(μ2-N3)2(μ-N3)2(μ3-OHCH3)2(μ-OHCH3)4]
     12:[Mn2Ⅲ(Salamp)2(amp)(N3)]·CH3OH
     13:[Co2Ⅲ(Salamp)2(amp)(CNS)]·CH3OH
     14:[Ni4Ⅱ(vanillin)4(μ3-OHCH3)4(μ-OHCH3)4]
     15:[Co4Ⅱ(vanillin)4(μ3-OHCH3)4(μ-OHCH3)4]
     16:[Cu4Ⅱ(vanillin)4(μ3-OHCH3)4(μ-OHCH3)4]
     配合物1是具有贝壳构型的[FeⅢ7]配位簇合物,其中六个Fe3+通过边桥基O离子桥联形成六圆环结构,另一个罕见四配位的Fe3+处于六圆环中间,磁性测试结果表明配合物分子中存在铁磁相互作用；配合物4是[Fe4ⅡFeⅢ]类型的四方锥构型五核混价铁簇合物,构型中有一个比较罕见的μ5-O离子；配合物5是[Fe4ⅡFeⅢLnⅢ]类型的六核3d-4f八面体构型配位簇合物,目前文献报道中还没有[Fe5Ln]类型的Fe系3d-4f簇合物,其中Ln3+处于八面体轴向位置的一个顶点处,磁性测试结果表明配合物分子中存在反铁磁相互作用；配合物6是[Fe4ⅡLn2Ⅲ]类型的蝴蝶构型六核3d-4f异金属配位簇合物,分子中有两个CNS-分别与稀土离子以端基方式配位,在文献中较少见,磁性测试结果表明配合物分子中存在反铁磁相互作用。配合物7是[Co4ⅢNd2Ⅲ]类型的六核3d-4f配位簇合物,具有哑铃型的骨架结构。
     配合物8是具有开放立方烷结构的[CUⅡ4],四个Cu2+均是四配位构型；配合物9是[Cu4ⅡCo2Ⅱ]类型的六核3d混金属配位簇合物,Cu2+与C02+之间是以席夫碱配体的醇羟基O离子和EO型叠氮离子桥联,Cu2+与Co2+之间的这种桥联构型在文献中很少见；配合物10是[Co2ⅡNi2Ⅱ]类型的缺角双立方烷构型四核3d混金属配位簇合物,金属离子之间是通过配体及甲醇的醇羟基O和以EO型桥联的叠氮离子桥联,磁性测试结果表明配合物分子中存在铁磁相互作用；配合物11是和配合物10结构相同的[CoⅡ4]配位簇合物。配合物2、12、13均是双核[Co2Ⅲ]、[Mn2Ⅲ]配合物。配合物3是单核[CrⅢ]配合物。配合物14、15、16均是类立方烷构型的四核[M4Ⅱ](M=Ni、Co、Cu)簇合物。
     对所有配合物进行了红外光谱、元素分析、X-射线单晶衍射分析测试,另外对配合物1、5、5f、5g、5h、6、6e、10进行了磁性测试分析,对配合物1、4、5、6、6e、9、10、14进行了1HNMR测试,对配合物1、4、5、6、9、10、15进行了XRD粉末衍射测试,对配合物1、4、5、6、9、10进行了XPS光电子能谱分析,对配合物5、5d、5e、5g、6、6d进行了荧光光谱测试,对配合物6、9、10进行了ICP测试分析。
Thirty-one new compounds were synthesized by reactions of transition and lanthanide metal salts with three key ligands, and associated ligands respectively, under solution reaction, solvothermal and solution diffuse conditions. The nineteen compounds chosen from them were determined by X-ray single crystal diffraction. The three key ligands include:①tetradentate H2salhyeten (salicylidene-N-(2-hydroxyethyl)ethylenedi-amine);②tridentate H2salamp (salicylidene-2-amino-2-methyl-1-propanol);③Didentate Vanillin(3-methoxy-4-hydroxybenzaldehyde). The formulas of the compounds are as follows:
     1:[Fe7Ⅲ(Salhyeten)6(μ3-O)3(CNS)]·(CH3OH)n(CNS)2
     2:[Co2Ⅲ(Salhyeten)2(N3)2]
     3:[CrⅢ(Hsalhyeten)2](NO3)
     4:[Fe4ⅡFeⅢ(Salamp)4(μ5-O)(CNS)(μ2-OHCH3)4]
     5:[Fe4ⅡFeⅢLnⅢ(Salamp)4(μ4-O)2(Pic)(NO3)(CH3OH)6](CH3OH)(H2O) (Ln= Dy(5), La(5a), Pr(5b), Nd(5c), m(5d), Eu(5e), Gd(5f), Tb(5g), Er(5h),Yb(5i))
     6:[Fe4ⅡLn2Ⅲ(μ4-O)2(Salamp)4(μ2-OHCH3)4(μ-OHCH3)2(H2O)4(CNS)2] (Ln= Sm(6), La(6a), Pr(6b), Nd(6c), Eu(6d), Gd(6e))
     7:[Co4ⅢLn2Ⅲ(salamp)4(μ3-OCH3)2(μ-OCH3)2(μ-O2CCH3)6(CH3OH)2] (Ln= Nd(7), Pr(7a))
     8:[Cu4Ⅱ(salamp)4]·3H2O
     9:[Cu4ⅡCo2Ⅱ(salamp)4(μ2-N3)4(μ3-OHCH3)2(CH3OH)2]
     10:[Co2ⅡNi2Ⅱ(Salamp)2(μ2-N3)2(μ-N3)2(μ3-OHCH3)2(μ-OHCH3)4]
     11:[Co4Ⅱ(Salamp)2(μ2-N3)2(μ-N3)2(μ3-OHCH3)2(μ-OHCH3)4]
     12:[Mn2Ⅲ(Salamp)2(amp)(N3)·CH3OH
     13:[Co2Ⅲ(Salamp)2(amp)(CNS)]·CH3OH
     14:[Ni4Ⅱ(vanillin)4(μ3-OHCH3)4(μ-OHCH3)4]
     15:[Co4Ⅱ(vanillin)4(μ3-OHCH3)4(μ-OHCH3)4]
     16:[Cu4Ⅱ(vanillin)4(μ3-OHCH3)4(μ-OHCH3)4]
     Compound 1 consists of shell-like heptanuclear [Fe7Ⅲ] cluster, in which sixμ2-alcohol groups bridge the six Fe ions to form a circle surrounding a central Fe3+ ion though threeμ3-O ions. Magnetic susceptibility measurements revealed that compound 1 displays ferromagnetic interactions between the metal iron ions. Compound 4 is a mixed-valence pentanuclear [Fe4ⅡFeⅢ] cluster, and the iron ions adopt the regular square-based pyramidal arrangement. Each edge of the square-based pyramid is bridged byμ2-O of methanol, and one unusualμ5-O ion inside square pyramidal lies over basal plane. Compound 5 [Fe4ⅡFeⅢLnⅢ] is the first 3d-4f hexanuclear hetero-metal cluster with a distorted-octahedron structure. Ln3+ and Fe3+ arranged in the axis position of the octahedron. Magnetic susceptibility measurements revealed that both exhibit antiferromagnetic interactions between the metal ions. Compound 6 [Fe4ⅡLn2Ⅲ] is a butterfly-like hexanuclear 3d-4f hetero-metal cluster. Two CNS- ions coordinate to the two lanthanide ions respectively. Magnetic susceptibility measurements revealed that antiferromagnetic exchange interactions between the metal centers was observed. Compound 7 [Co4ⅢNd2Ⅲ] is a hexanuclear 3d-4f hetero-metal cluster with a dumbbell-like structure.
     Compound 8 is a tetranuclear [Cu4Ⅱ] with open-cube structure, and four Cu2+ ions are all plane-quadrangle geometry. Compound 9 [Cu4ⅡCo2Ⅱ] is a hexanuclear 3d hetero-metal cluster. A defective tetra-cube is formed by Cu and Co ions bridging by methoxy, phenoxy, fourμ2-N3-, and alcohol moieties. Compound 10 [Co2ⅡNi2Ⅱ] is a tetranuclear 3d hetero-metal cluster with defective double-cube framwork. Magnetic susceptibility measurements revealed that compound 10 has an ferromagnetic interactions between the metal ions. Compound 11 has the same structure as compound 10, only the Ni ions are all substituted by Co ions. Compound 12,13 and 14 are dinulear coordination complex based on Mn2+ or Co2+. Compound 1 is a mononulear chromium complex. Compound 14,15 and 16 are isostuctural tetranuclear [M4Ⅱ](M=Ni, Co, Cu) cluster with cube-like structure.
     The crystal structures are determined by X-ray single crystal diffraction, and chemical composition, functional groups, magnetism and fluorescence are characterized by IR and element analysis, MPMS XL-5(1,5,5f,5g,5h,6,6e,10), 1HNMR(1,4,5,6,6e,9,10,14), XRD(1,4,5,6,9,10,15), XPS(1,4,5,6,9,10), ICP(6,9,10), fluorescence(5,5d,5e,5g,6,6d) et al.

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