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研究生： 余蕙茹
Yu, Hui-Ru
論文名稱： 銅-鑭系金屬團簇之合成、結構及磁性研究
Syntheses, structures, and magnetic properties of heterometallic copper(II)-lanthanide complexes
指導教授： 蔡惠蓮
Tsai, Hui-Lien
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2018
畢業學年度： 106
語文別： 英文
論文頁數： 264
中文關鍵詞： 單分子磁鐵 、銅-鑭系混金屬化合物 、β-雙酮
外文關鍵詞： Single molecule magnets (SMMs), Cu/Ln complexes, β-diketone
相關次數： 點閱：86  下載：1 
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    • 本文分成三個章節。章節一:利用HL與Ln(ClO4)3和CuCl2合成出一系列的化合物[CuIILnIII(μ2-ClO4)(L)2(MeOH)2(H2O)Cl](ClO4) (Ln = Y(1·Y), Gd(2·Gd), Tb(3·Tb), Dy(4·Dy)和Ho(5·Ho))，並以X光單晶繞射確定其分子結構。從直流(dc)磁化率測量，顯示化合物2·Gd、3·Tb、4·Dy和5·Ho具有分子內鐵磁性(ferromagnetic)作用力。從交流(ac)磁化率測量，顯示3·Tb、4·Dy及5·Ho在零磁場下具有磁緩現象(slow magnetic relaxation)。化合物3·Tb、4·Dy及5·Ho的磁異向能(Ueff)分別為56.25 K、222.03 K及21.19 K。而4·Dy的磁異向能是目前銅-鑭系單分子磁鐵中最高的。
    章節二：我們合成出一系列的一維鏈狀(1D-chain) 化合物{[CuIILnIII(μ2−NO3)2(L)2(η2−NO3)]·xH2O·yEt2O}n (Ln = Y(6·Y), Dy(7·Dy), Ho(8·Ho), Er(9·Er))，並以X光單晶繞射確定其結構。分子間藉由硝酸根的氧(O11)沿著a軸橋接雙核單體形成一維鏈狀化合物。從直流(dc)磁化率測量，顯示化合物7·Dy具有鐵磁性(ferromagnetic)作用力。交流(ac)磁化率的測量中，化合物8·Ho在零磁場下觀測到磁緩現象，其磁異向能(Ueff)為3.33 K；化合物7·Dy則在外加1000 Oe磁場下，觀測到磁緩現象，其磁異向能為15.40 K。
    章節三：使用Gd(OAc)3或Tb(OAc)3與HL和CuCl2合成四核[CuII3LnIII(μ3-OH)(μ2-Cl)2(L)3(MeOH)Cl3]∙H2O (Ln = Gd(10·Gd), Tb(11·Tb))化合物；在相同反應條件下，Dy(OAc)3或Er(OAc)3則得到六核[CuII4LnIII2(μ3-OH)2(μ2-Cl)2(μ2-OAc)2(L)4(MeOH)2Cl4]∙wH2O·xEt2O·yMeOH·zMeCN (Ln = Dy(12·Dy), Er(13·Er))化合物，並以X光單晶繞射確定兩者結構。從直流(dc)磁化率測量，顯示化合物10·Gd具有分子內同時存在鐵磁性和反鐵磁性的作用力。在交流磁化率的量測中，11·Tb及12·Dy在零外加磁場環境中可觀測到磁緩現象，其磁異向能(Ueff)分別為2.28 K和40.19 K。

    This work contains three chapters. First, a series of heterometallic complexes ([CuIILnIII(μ2-ClO4)(L)2(MeOH)2(H2O)Cl](ClO4) (Ln = Y(1·Y), Gd(2·Gd), Tb(3·Tb), Dy(4·Dy) and Ho(5·Ho)) were synthesized by using HL, Ln(ClO4)3 and CuCl2. The molecular structures of complexes 1·Y–5·Ho were confirmed by single crystal X-ray crystallography. The dc magnetic susceptibility measurements show the presence of ferromagnetic interactions in complexes 2·Gd–5·Ho. For the ac magnetic susceptibility measurements, complexes 3·Tb, 4·Dy, and 5·Ho were found to exhibit single-molecule-magnet (SMM) behaviors with energy barrier values (Ueff) of 56.25, 222.03, and 21.19 K, respectively, under zero applied field. The complex 4·Dy shows the highest anisotropy barrier (222.03 K) in Cu/Ln-based single molecule magnets.
    For the second part, the reaction of HL with Cu(NO3)2 and Ln(NO3)3 were found to give a series of one-dimensional heterometallic complexes {[CuIILnIII(μ2−NO3)2(L)2(η2−NO3)]·xH2O·yEt2O}n (Ln = Y(6·Y), Dy(7·Dy), Ho(8·Ho), Er(9·Er)). The molecular structures of complexes 6·Y–9·Er were confirmed by single crystal X-ray crystallography. The coordination polymeric systems appear due to the bridging coordination of the nitrate ions, which connect successive [Cu1Ln1] units along a-axis. The dc magnetic susceptibility measurements of 6·Y–9·Er show the presence of ferromagnetic interactions in complex 7·Dy. For the ac magnetic susceptibility measurements, complexes 7·Dy and 8·Ho were found to exhibit SMM behaviors with energy barrier values of 3.33 K (1000 Oe) and 15.40 K (0 Oe), respectively.
    For the last part, two types of Cu/Ln heterometallic complexes [CuII3LnIII(μ3-OH)(μ2-Cl)2(L)3(MeOH)Cl3]∙H2O (Ln = Gd(10·Gd), Tb(11·Tb)) and [CuII4LnIII2(μ3-OH)2(μ2-Cl)2(μ2-OAc)2(L)4(MeOH)2Cl4] ∙wH2O·xEt2O·yMeOH·zMeCN (Ln = Dy(12·Dy), Er(13·Er)) were synthesized under the same reaction conditions and structurally characterized. The dc magnetic susceptibility measurements of 10·Gd display the presence of multiple interactions in complex 10·Gd. For the ac magnetic susceptibility measurements, complexes 11·Tb, and 12·Dy were found to exhibit SMM behaviors with energy barrier (Ueff) of 2.28,and 40.19 K, respectively, under zero applied field.

    Contents 中文摘要 I Abstract III 誌謝 V Contents VI List of Tables IX List of Figures XV List of Schemes XXX Abbreviation 1 Introduction 2 Chapter 1 Syntheses, Structures and Magnetic Properties of dinuclear CuIILnIII complexes: [CuIILnIII(μ2–ClO4)(L)2(MeOH)2(H2O)Cl](ClO4) Ln = Y(1·Y), Gd(2·Gd), Tb(3·Tb), Dy(4·Dy), Ho(5·Ho) 11 I.1. Experimental Section 12 I.1.1. Synthesis 12 I.1.2. X-ray Crystallography 15 I.1.3. Physical measurements 17 I.2. Results and discussion 18 I.2.1. Synthesis and phase identification 18 I.2.2. Description of structure 21 I.2.3. Magnetic properties 33 Chapter 2 Syntheses, Structures and Magnetic Properties of 1-D chain compounds: {[CuIILnIII(μ2−NO3)2(L)2(η2−NO3)]·xH2O·yEt2O}n Ln = Y(6·Y), Dy(7·Dy), Ho(8·Ho), Er(9·Er) (x = 0.7, y = 0.3 for 6·Y, 7·Dy and 8·Ho; x = 0.75, y = 0.25 for 9·Er) 89 II.1. Experimental Section 90 II.1.1. Synthesis 90 II.1.2. X-ray Crystallography 93 II.1.3. Physical measurements 95 II.2. Results and discussion 96 II.2.1. Synthesis and phase identification 96 II.2. Description of structure 99 II.2.3. Magnetic properties 109 II.3. Conclusions 136 Chapter 3 Syntheses, Structures and Magnetic Properties of tetranuclear and hexanuclear complexes: [CuII3LnIII(μ3-OH)(μ2-Cl)2(L)3(MeOH)Cl3]∙H2O Ln = Gd(10·Gd), Tb(11·Tb) [CuII4LnIII2(μ3-OH)2(μ2-Cl)2(μ2-OAc)2(L)4 (MeOH)2Cl4]∙wH2O·xEt2O·yMeOH·zMeCN Ln = Dy(12·Dy), Er(13·Er) (w = 1.8, x = 0.7, y = 0, z = 0.5 for 12·Dy and w = 0.5, x = 1, y = 0.5, z = 0 for 13·Er) 137 III.1. Experimental Section 138 III.1.1. Synthesis 138 III.1.2. X-ray Crystallography 141 III.1.3. Physical measurements 143 III.2. Results and discussion 144 III.2.1. Synthesis and phase identification 144 III.2.2. Description of structure 151 III.2.3. Magnetic properties 174 III.3. Conclusions 211 References 212 Appendix 223

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