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研究生：	楊振宜 Yang, Chen-I
論文名稱：	多核錳分子磁鐵之製備與鑑定 Preparation and characterization of polynuclear manganese molecular magnets
指導教授：	蔡惠蓮 Tsai, Hui-Lien
學位類別：	博士 Doctor
系所名稱：	理學院 - 化學系 Department of Chemistry
論文出版年：	2007
畢業學年度：	95
語文別：	英文
論文頁數：	279
中文關鍵詞：	單分子磁鐵、水楊醛肟、磁滯迴路、交流磁化率、直流磁化率、X光單晶繞射、吡啶雙酮基
外文關鍵詞：	X-ray crystallography, hysteresis loop, AC, pyridine-containing β-dikentone, DC, single-molecule magnet, salicylaldoxime
相關次數：	點閱：82 下載：5
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本論文，對Mn8Fe4、Mn4、Mn6、Mn5及Mn8團簇化合物之合成及其磁性的研究，分四部份。第一部分：在鹵素酸環境下以MnO4- 與Fe2+ 反應可得中心結構具有四個MnIII、四個FeIII及四個MnIV離子的團簇化合物: [Mn8Fe4(O2CCH2Cl)16(H2O)4] (1)、 [Mn8Fe4(O2CCH2Br)16(H2O)4] (2)及[Mn8Fe4(O2CCHCl2)16(H2O)4] (3)，其結構皆經由X光單晶繞射確認。直流磁化率與交流磁化率的測量均顯示化合物1、2及3為基態S = 4的單分子磁鐵。第二部分：利用2,6-bis(hydroymethyl)-p-cresol (H3L) 與MnII 離子反應得到四核錳團簇化合物: [Mn4(HL)4(MeOH)4Cl2] (4)、[Mn4(HL)4(MeOH)4Br2] (5)及 [Mn4(HL)4(DMF)2(H2O)2(NCS)2] (6) ，其結構皆經由X光單晶繞射確認。直流磁化率與交流磁化率的測量，均顯示化合物4、5及6中錳離子間的鐵磁性作用力形成基態S = 9的單分子磁鐵性質。第三部分：以含吡啶雙酮基(1-phenyl-3-(2-pyridyl)propane-1,3-dione (HL1) 或 1-(2-pyridly)-3-(p-tolyl)propane-1,3-dione (HL2))與中心結構為[Mn3O]6+之三核錳錯合物反應，可得到四核錳錯合物[Mn4O(O2CCCl3)6L12] (7)、 [Mn4O(O2CCCl3)6L22] (8)及六核錳錯合物[Mn6O2(O2CPh)8L13] (9)、 [Mn6O2(O2CPh)8L23] (10)，其結構皆經X光單晶繞射確認。直流磁化率測量顯示化合物7、8具有基態S = 1，而化合物9、10具有基態S = 7/2，同時交流磁化率及單晶磁滯迴路的量測均顯示化合物9及10為新型態之單分子磁鐵。第四部分：利用水楊醛肟(salicyladoxime, H2salox)可製備(NEt4)3[Mn5O(salox)3(N3)6Cl2] (11)、(NEt4)2[Mn8O2(salox)6(N3)6(MeOH)3] (12)、[Mn6O2(salox)6(MeOH)6(NCNCONH2)2] (13)及[Mn6O2(salox)6(EtOH)4(H2O)2Cl2] (14)。化合物11、12、13及14之結構皆利用X光單晶繞射確認，並且由磁性量測證明其分子磁鐵之性質。

This work describes the preparation of Mn8Fe4, Mn4, Mn6, Mn5, and Mn8 complexes and their characterization by X-ray crystallography, DC, AC and hysteresis magnetic measurements. Synthetic methodology for preparation of a new class of mixed-metal SMM has been developed. The complexes [Mn8Fe4(O2CCH2Cl)16(H2O)4] (1), [Mn8Fe4(O2CCH2Br)16(H2O)4] (2) and [Mn8Fe4(O2CCHCl2)16(H2O)4] (3) can be synthesized from the reaction of MnO4- with Fe2+ in the presence of haloacetic acid. All three of these complexes contain 4 MnIII, 4 FeIII and 4 MnIV ions and have been characterized by X-ray crystallography. DC and AC magnetic studies indicate the complexes are new SMMs with an S = 4 ground spin state. The reactions of 2,6-bis(hydroymethyl)-p-cresol (H3L) with MnII ions yield the tetranuclear complexes of [Mn4(HL)4(MeOH)4Cl2] (4), [Mn4(HL)4(MeOH)4Br2] (5) and [Mn4(HL)4(DMF)2(H2O)2(NCS)2] (6). The structures of complexes 4, 5 and 6 are determined by X-ray crystallography. DC and AC magnetic studies indicate the complexes 4, 5 and 6 display ferromagnetic interaction between four Mn ions resulting an S = 9 ground spin state and SMM properties. Treatments with pyridine-containing -dikentone, 1-phenyl-3-(2-pyridyl)propane-1,3-dione (HL1) or 1-(2-pyridly)-3-(p-tolyl)propane-1,3-dione (HL2), with trinuclear complexes containing Mn3O6+ produce tetranuclear complexes, [Mn4O(O2CCCl3)6L12] (7) and [Mn4O(O2CCCl3)6L22] (8), and hexanuclear complexes [Mn6O2(O2CPh)8L13] (9), and [Mn6O2(O2CPh)8L23] (10). The structures of these complexes are determined by X-ray crystallography. DC magnetic studies indicate the tetra- and hexanuclear complexes have an S = 1 and S = 7/2 ground spin state, respectively, while the latter are evidenced as new class of SMMs by AC and single-crystal hysteresis magnetic studies. Four new polynuclear manganese complexes, (NEt4)3[Mn5O(salox)3(N3)6Cl2] (11), (NEt4)2[Mn8O2(salox)6(N3)6(MeOH)3] (12), [Mn6O2(salox)6(MeOH)6(NCNCONH2)2] (13), and [Mn6O2(salox)6(EtOH)4(H2O)2Cl2] (14) are prepared by using salicylaldoxime (H2salox) as a chelating group. The structures of these complexes are determined by X-ray crystallography and molecular magnet properties of complexes are evidenced by magnetic measurements.

Abstract in Chinese…………. …………..………………………………………	I
Abstract …………………. …………..………………………………………….	III
Acknowledgement ……………………...…………………………………..……	IV
Contents ………………………...………………………………………………..	V
List of tables…...………………………...….……………………………………	VIII
List of figures…….……………..……………………………………………..…	X
Abbreviation……………………………………………………………………...	XVIII
自述………………………………………………………………………………	278
General introduction……………….…………………………………...………	1
Chapter 1  Single-Molecule Magnets: [Mn8Fe4O12(O2CR)16(H2O)4] (R = CH2Cl, CH2Br, CHCl2).........................................................................................................12
I	Introduction………………………………………….……......................	13
II	Experimental Section ………………………………………….……......	13
	II. 1. Synthesis. ……………………..…………………………….…….	13
	II. 2. X-ray Crystallography ……………………..…………….……….	15
	II. 3. Physical Measurements……………………..……………..………	15
III	Results and Discussion ………….……………………………...………	18
	III. 1. Synthesis……………………………………………………….…	18
	III. 2. Description of Structures………………………………..………	19
	III. 3. DC magnetic susceptibilities……………………………………..	38
	III. 4. Variable Field DC Magnetization Measurements………………...	40
	III. 5. AC magnetic susceptibilities……………………………………..	47
IV	Concluding Comments………………………………………...………..	48

Chapter 2 Synthesizes, Structures and Magnetic Properties of Tetranuclear Manganese Single-Molecule Magnets…………………………………………………………..52
I	Introduction ……………………………………………………….……	53
II	Experimental Section ………………………………………………...…	53
	II. 1. Synthesis. ……………………..………………………………..…	53
	II. 2. X-ray Crystallography ……………………..…………………...…	53
	II. 3. Physical Measurements……………………………………………	56
III	Results and Discussion ………….…………………………………...…	57
	III. 1. Synthesis…………………………………………………….……	57
	III. 2. Description of Structures……………………...…………..…….	57
	III. 3. DC Magnetic Susceptibilities ……………………………….…..	70
	III. 4. Variable Field DC Magnetization Measurements………………...	77
	III. 5. AC Magnetic Susceptibilities………………………...………….	82
IV	Concluding Comments……………………………………...…………..	88

Chapter 3 Tetra- and Hexanuclear Manganese Complexes from the Flexibility of Pyridine- containing b-diketone Ligands.…………………………………………89
I	Introduction …………………………………………………………….	90
II	Experimental Section ……………………………………...…………....	91
	II. 1. Synthesis. …………………………………………………...…….	91
	II. 2. X-ray Crystallography …………………..……………...…………	93
	II. 3. Physical Measurements…………………………………...……….	94
	II. 4. Other Studies………………………………………………………	94
III	Results and Discussion……….………………………………...……….	95
	III. 1. Synthesis…………………………………………………….……	95
	III. 2. Description of Structures……………………………...………...	96
	III. 3. Magnetic Properties of Complexes 7 and 8………………….…	116
	III. 4. Magnetic Properties of Complexes 9 and 10……………..………	118
	III. 5. Single-Crystal Hysteresis Studies………………………………...	126
IV	Concluding Comments………………………………………………….	128

Chapter 4 Polynuclear Manganese Molecular Magnets from Chelating of Salicylaldoxime.......................................................................................................131
I	Introduction …………………………………………………………….	132
II	Experimental Section ……………………………………………….…..	132
	II. 1. Synthesis. ……………………..…………………….…………….	132
	II. 2. X-ray Crystallography …………………………….………………	134
	II. 3. Physical Measurements………………………………..……….….	135
III	Results and Discussion ……..…….…………………………....……….	135
	III. 1. Synthesis…………………………………………….……………	135
	III. 2. Description of Structures………………………….………...……	138
	III.3. Magnetic Properties of Complex 11………………………...…….	159
	III. 4. Magnetic Properties of Complex 12….………….……...……….	176
	III. 5. Magnetic Properties of Complexes 13 and 14………….………...	184
IV	Concluding Comments………………………………………………	192
Reference………………………………………………………………………...	194
Appendix A Expanded van Vleck Equation of a [MnII2MnIII2] Complex with a Butterfly Core……………………………………………………………………...205
Appendix B Expanded van Vleck Equation of a [MnII2MnIII2] Complex with a Tetrahedron Core…………………………………………………………………...208
Appendix C Expanded van Vleck Equation of a [MnII2MnIII3] Complex with a Trigonal Bipyramid Core…………………………………………………………..................212
Appendix D Atomic Coordinates and Equivalent Isotropic Displacement   Parameters for Complexes 1-14…………….……………………………..………..217
                                    

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