论文总字数：12366字
摘 要
2-乙酰基吡咯与2-(2-氨乙基)吡啶在无水乙醇中发生缩合反应得到了席夫碱（Schiff base）配体HL3。以三乙基胺作为碱，HL3在甲醇溶液中和和四氟合硼酸铜(Ⅱ)及硫氰酸铵作用，得到了硫氰根桥联的二核铜(Ⅱ)配合物[L32CuII2(μ1,3-NCS)2]（1）；和四氟合硼酸铜(Ⅱ)及叠氮酸钠作用，得到了叠氮酸根桥联的二核铜(Ⅱ)配合物[L32CuII2(μ1,3-N3)2]（2）。对配体和配合物进行了红外光谱、核磁共振和质谱等表征。单晶X-射线衍射测定表明配合物1是NCS-离子以μ1,3-方式桥联的二核铜（II）配合物[L32CuII2(μ1,3-NCS)2]，配合物2是叠氮酸根以μ1,3-方式桥联的二核铜（II）配合物[L32CuII2(μ1,3-N3)2]，且铜(II)的几何构型都为四方锥形。测定了配合物1和2的变温磁化率（m）对温度（T）变化的曲线。分析表明在配合物1和2的分子中，两个铜（II）离子之间存在通过拟卤素桥（-NCS-或-NNN-）存在反铁磁的耦合作用。对这些配体和配合物进行了红外光谱、质谱、核磁共振等表征。关键词：席夫碱，铜，吡咯，吡啶, 晶体结构，磁性
Abstract: A Schiff-base ligand HL3 was synthesized in absolute ethanol by condensation of 2-acetylpyrrole with 2-(2-aminoethyl)pyridine. The thiocyanato-bridged dinuclear copper(II) complex [L32CuII2(μ1,3-NCS)2] (1) was synthesized by mixing copper(II) tetrafluoroborate hydrate with HL3 and ammonium thiocyanate in methanol using triethyleneamine as a base. The azido-bridged dicopper(II) complex [L32CuII2(μ1,3-N3)2] (2) was synthesized by the reaction of copper(II) tetrafluoroboron hydrate with HL3 and sodium azide in methanol using triethyleneamine as a base. Single crystal X-ray diffraction determinations carried out on complexes 1 and 2 reveal that they are both doubly pseudohalide-bridged square pyramidal copper(II) dimers [L32CuII2(μ-X)2] (X = NCS, 1; X = N3, 2), and that the thiocyanate and azide groups bridge the two copper(II) ions in respective molecule in an end-to-end fashion. Variable temperature magnetic susceptibilities were recorded for 1 and 2. They are both show antiferromagnetic exchange. The ligand and complexes were characterized by IR, MS and UV-Vis.
Keywords: Schiff-base, copper, pyrrole, pyridine, crystal structure, magnetism
目录
1 前言……………………………………………………………………………3
2 实验部分……………………………………………………………………4
2.1 仪器与试剂…………………………………………………………4
2.1.1 仪器………………………………………………………………………4
2.1.2 药品与试剂……………………………………………………………4
2.2 配体及其配合物的合成…………………………………………5
2.2.1 HL3的合成……………………………………………………………5
2.2.2 含硫氰根配合物[L32CuII2(μ1,3-NCS)2](1)的合成………………………5
2.2.3 含叠氮酸根配合物[L32CuII2(μ1,3-N3)2](2)的合成……………………6
3 结果与讨论 …………………………………………………………………6
3.1 HL3的合成与表征…………………………………………………………6
3.2 含硫氰根配合物(1)的合成与表征………………………………………9
3.3 含叠氮酸根配合物（2）的合成与表征…………………………………11
3.4 配合物1和2的晶体结构…………………………………………………12
3.5 配合物1和2的磁性………………………………………………………14
结论……………………………………………………………16
参考文献………………………………………………………………17
致谢……………………………………………………………………19
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