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研究生：	林羽珊 Lin, Yu-Shan
論文名稱：	鈷-鑭系金屬簇之合成、結構及磁性研究 Syntheses, structures, and magnetic properties of heterometallic cobalt(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：	2017
畢業學年度：	105
語文別：	英文
論文頁數：	237
中文關鍵詞：	鈷–鑭系金屬錯合物、β–雙酮、單分子磁鐵
外文關鍵詞：	CoII–LnIII complex, β-diketone, single molecule magnets
相關次數：	點閱：58 下載：5
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本文分三部分，第一部分利用β-雙酮化合物(L1) 分別與Co(II) 及
Ln(III) 金屬離子反應，進而合成出一系列3d-4f 雙核混金屬錯合物
[CoIILnIII(L1)2(μ2-ClO4)(H2O)4](ClO4)2·H2O，且利用單晶X光繞射確認其結構，其中，在金屬配位環境上，透過過氯酸根離子以雙牙基橋接的方式連結Co(II)與Ln(III)金屬離子。從直流磁化率(direct current susceptibility, dc)測量顯示化合物1·Tb3·Ho 金屬間存有鐵磁性(ferromagnetic)作用力，而4·Er 分子間則是存有反鐵磁性(antiferromagnetic)作用力。從交流磁化率(alternating current susceptibility, ac)的量測顯示，化合物1·Tb-3·Ho 在未有外加磁場下皆有觀察到磁緩現象的發生。第二部分利用β-雙酮化合物(L2)與Co(II)及Ln(III)金屬離子反應，合成出一系列3d-4f 雙核混金屬錯合物[CoIILnIII(L2)2(MeOH)2(H2O)2Cl2]Cl·MeOH，從直流磁化率量測顯示化合物6·Tb-8·Ho 金屬間存有鐵磁性作用力，且5·Y 化合物中Co(II)之間存有自旋-軌域偶合(Spin-orbital coupling)作用力。由交流磁化率的量測顯示，化合物6·Tb-8·Ho 在未有外加磁場下皆可觀察到磁緩現象的發生，5·Y 化合物在外加磁場後，能發現一個受到磁場誘導，而產生的單分子磁鐵(single molecule magnets, SMMs)行為，值得一提的是，7·Dy 在鈷-鑭系單分子磁鐵系列中，為具有相當高異向能(Ueff = 155.43 K) 的化合物。第三部分利用β-雙酮化合物(L3)與Co(II)及Ln(III)金屬離子反應，得到一系列四核混金屬錯合物
[CoII2LnIII2(L3)2(μ3-OMe)2(MeOH)2(NO3)2(OAc)4]·xH2O·yMeOH。從直流磁化率測量顯示化合物9·Y 分子間存有自旋-軌域偶合(Spin-orbital coupling)作用力，而10·Gd 化合物Co(II)與Gd(III)金屬之間存有鐵磁性作用力。並且透過交流磁化率磁性量測得其11·Tb 與12·Dy 單分子磁鐵的磁緩現象及量子穿隧效應。

This work contains three parts. The first part, a series of heterometallic CoII–LnIII dinuclear [CoIILnIII(L1)2(μ2-ClO4)(H2O)4](ClO4)2·H2O (LnIII = TbIII (1·Tb), DyIII (2·Dy), HoIII (3·Ho), and ErIII (4·Er)) complexes have been synthesized by using multidentate ligands (L1). The structures of these compounds were determined by X-ray crystallography. Structural studies demonstrate that the metal centers are bridged by perchlorate ligands, leading to a [CoIILnIII(μ2-ClO4)] core. Direct current (DC) magnetic susceptibility measurements reveal the presence of intramolecular ferromagnetic interactions in complexes 1·Tb-3·Ho. However, intermolecular antiferromagnetic interactions exhibit in complex 4·Er. Alternating current (AC) magnetic susceptibility data indicate complexes 1·Tb-3·Ho exhibiting slow relaxations of the magnetization without dc field. In the second part, a series of heterometallic Co-Ln dinuclear [CoIILnIII(L2)2(MeOH)2(H2O)2Cl2]Cl·MeOH (LnIII = YIII (5·Y), TbIII (6·Tb), DyIII (7·Dy), and HoIII (8·Ho)) complexes have been obtained by using multidentate ligands (L2). The structures of these compounds were determined by X-ray crystallography. DC magnetic susceptibility measurements reveal the presence of intramolecular ferromagnetic interactions between CoII and LnIII ions in complexes 6·Tb-8·Ho. AC magnetic susceptibility data indicate complexes 6·Tb-8·Ho exhibit out-of-phase signals at zero dc field. Besides, the ac magnetic susceptibility data for complex 5·Y show a frequency-dependent relaxation under an applied field of 800 Oe. This performance is consistent with field-induce SMM behaviors for high spin CoII ions. Moreover, for the complex 7·Dy, single molecule magnet (SMM) behavior is displayed with a large thermally activated anisotropy barrier of 155.43 K without dc field. It is the great Ueff (155.43 K) compare to all CoII-LnIII complexes that have been found so far. The third part, a novel series of defective dicubane 3d–4f tetranuclear [CoII2LnIII2(L3)2(μ3-OMe)2(MeOH)2(NO3)2(OAc)4]·xH2O·yMeOH (LnIII = YIII (9·Y), GdIII (10·Gd), TbIII (11·Tb), and DyIII (12·Dy); x = 0, y = 4 for 9·Y and 11·Tb; x = 2, y = 2 for 10·Gd and 12·Dy) complexes have been synthesized by using multidentate ligands (L3). DC magnetic susceptibility measurements reveal that the presence of spin-orbital coupling interactions in complexes 9·Y and ferromagnetic interactions between CoII and GdIII ions in complexes 10·Gd. AC magnetic susceptibility data indicate that complexes 11·Tb and 12·Dy exhibit slow relaxation and QTM of the magnetization.

中文摘要 I
Abstract III
誌謝 V
Contents VI
Lists of Tables VIII
Lists of Figures XI
Introduction 1
Chapter 1 Syntheses, Structures and Magnetic Properties of Dinuclear CoIILnIII Complexes:
[CoIILnIII(L1)2(μ2-ClO4)(H2O)4](ClO4)2·H2O (LnIII = Tb, Dy, Ho and Er)
I. Experimental Section 13
I.1. Synthesis 13
I.2. X-ray crystallography 17
I.3. Physical measurements 20
II. Results and discussion 21
II.1. Synthesis 21
II.2. Description of structure 23
II.3. Magnetic properties 40
III. Conclusion 74
Chapter 2 Syntheses, Structures and Magnetic Properties of 
Dinuclear CoIILnIII Complexes:
[CoIILnIII(L2)2(MeOH)2(H2O)2Cl2]Cl·MeOH (LnIII = Y, Tb,
Dy, and Ho)
I. Experimental Section 76
I.1. Synthesis 76
I.2. X-ray crystallography 80
I.3. Physical measurements 83
II. Results and discussion 84
II.1. Synthesis 84
II.2. Description of structure 86
II.3. Magnetic properties 105
III. Conclusion 149
Chapter 3 Syntheses, Structures and Magnetic Properties of Tetranuclear CoII2LnIII2 Complexes:
[CoII2LnIII2(L3)2(μ3-OMe)2(MeOH)2(NO3)2(OAc)4]·xH2O·yMe
OH (LnIII = Y, Gd, Tb and Dy)
I. Experimental Section 151
I.1. Synthesis 151
I.2. X-ray crystallography 154
I.3. Physical measurements 158
II. Results and discussion 159
II.1. Synthesis 159
II.2. Description of structure 161
II.3. Magnetic properties 183
III. Conclusion 214
References 215
Appendix 225
                                    

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