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研究生: 陳鴻文
Hong-Wen Chen
論文名稱: 含第16族元素(S、Se、Te)之過渡金屬(Mn、Fe、Ru)團簇化合物的合成與其化性、物性的研究
指導教授: 謝明惠
Shieh, Ming-Huey
學位類別: 碩士
Master
系所名稱: 化學系
Department of Chemistry
論文出版年: 2004
畢業學年度: 92
語文別: 中文
論文頁數: 261
中文關鍵詞: 金屬團簇化合物
英文關鍵詞: Transition Metal
論文種類: 學術論文
相關次數: 點閱:131下載:9
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  • [Et4N]2[SeFe3(CO)9]與Cu+ 試劑的反應,不同的Cu+ 來源,可生成不同的產物:與[Cu(CH3CN)4]BF4的反應可生成{[SeFe3(CO)9]2
    -Cu}3-,與CuOAc反應可生成{[SeFe3(CO)9]2Cu2(μ-OAc)}3-。另外混合dppm與dppe於[SeFe3(CO)9]2-與[Cu(CH3CN)4]BF4的反應中,利用反應溶劑以及反應物比例的不同,可生成一系列含Cu片段的化合物(μ5-Se)Fe3(CO)9Cu2(μ-dppm)(L) (L = CH3CN, THF)、SeFe3(CO)9Cu2
    -(μ-dppe)、{[SeFe3(CO)9]2Cu2(μ-dppe)}2-和{[SeFe3(CO)8]Cu2(μ-dppm)
    -(μ-dppm)}。
    以Se powder和Mn2(CO)10於鹼性溶液中在室溫下反應,不同的濃度及反應時間,可得到不同的結果:於0.9 M KOH下以Se: Mn = 1: 1比例反應一小時,可得到[Se10Mn6(CO)18]4-;若將KOH濃度提高至4 M,則可得到[Se2Mn3(CO)9]2-。以Se: Mn = 10: 6比例,於0.9 M KOH和4 M KOH濃度下反應一小時,皆可得到[Se10Mn6(CO)18]4-;若延長反應時間至十天,於0.9 M KOH下可得[Se5Mn4(CO)12]2-,而於4 M KOH下可得到[Se6Mn6(CO)18]4-,二者皆為新型結構之化合物。

    The reactions of [Et4N]2[SeFe3(CO)9] with different Cu+ reagents resulted in different products. When [Et4N]2[SeFe3(CO)9] reacted with
    [Cu(CH3CN)4]BF4 and CuOAc, {[SeFe3(CO)9]2Cu}3- and {[SeFe3 -(CO)9]2Cu2(μ-OAc)}3- were obtained, respectively. On the other hand, if [SeFe3(CO)9]2- was treated with [Cu(CH3CN)4]BF4/dppm or dppe in varied ratios and different solvents, a series of copper-incorporated E-Fe clusters: (μ5-Se)Fe3(CO)9Cu2(μ-dppm)(L) (L = CH3CN, THF), SeFe3 -(CO)9Cu2(μ-dppe), {[SeFe3(CO)9]2Cu2(μ-dppe)}2-, and {[SeFe3(CO)8]
    -Cu2(μ-dppm)(μ-dppm)} were produced.
    The reactions of Se powder with Mn2(CO)10/KOH/MeOH solution in varied reaction condition were systematically studied. While Se powder reacted with 0.5 eq Mn2(CO)10 in 0.9 M KOH/MeOH solution for 1 hr to produce [Se10Mn6(CO)18]4-, the similar reaction in 4 M KOH/MeOH solution gave [Se2Mn3(CO)9]2-. In the case of Se: Mn in the ratio of 10: 6, the reaction of Se with Mn2(CO)10 in 0.9 M or 4 M of KOH/MeOH for 1 hr led to formation of the new complex [Se10Mn6(CO)18]4-. However, if the reactions proceeded for ten days in 0.9 M and 4 M of KOH/MeOH solutions for ten days, [Se5Mn4(CO)12]2- and [Se6Mn6(CO)18]4- were obtained, both of which represent novel types of complexes in the Se-Mn-CO system.

    1. 前言……………………………………………………… 1 1.1-1 背景……………………………………………………… 1 1.1-2 磁性……………………………………………………… 9 1.2 研究目標…………………………………………………13 2. 實驗……………………………………………………… 14 2.1 一般方法………………………………………………… 14 2.1-1 實驗過程………………………………………………… 14 2.1-2 光譜儀器………………………………………… 15 2.1-3 實驗溶劑…………………………………………………15 2.1-4 使用藥品………………………………………………… 16 2.1-5 縮寫表……………………………………………………16 2.2 Na2SO3和Ru3(CO)12與[Cu(CH3CN)4]BF4的反應………………… 18 2.3 [PPN]2[Te10Fe8(CO)20]和[Cu(CH3CN)4]BF4的反應……………… 18 2.4 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4的反應……………………19 2.4-1 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4以1: 1比例反應………19 2.4-2 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4以1: 2比例反應………20 2.5 [Et4N]2[SeFe3(CO)9]和CuOAc的反應........................ 20 2.6 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppe的反應…………… 21 2.6-1 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppe以1: 2: 1比例在THF下反應……………………………………………………21 2.6-2 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppe以1: 2: 1比例 在CH2Cl2下反應…22 2.6-3 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppe以1: 2: 1比例在CH3CN下反應………………………………………………………23 2.6-4 [SeFe3(CO)9]Cu2(μ-dppe)與{[SeFe3(CO)9]2Cu2(μ-dppe)} -[Cu(dppe)2]2的轉換反應……………………………………………24 2.7 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppm的反應……………25 2.7-1 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppm以1: 2: 1比例 在THF下反應………………………………………………………25 2.7-2 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppm以1: 2: 1比例 在CH2Cl2下反應……………………………………………………26 2.8 {[SeFe3(CO)8]Cu2(μ-dppm)(μ-dppm)}的合成………………………26 2.8-1 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppm以1: 2: 2比例反應……………………………………………………26 2.8-2 [SeFe3(CO)9]Cu2(μ-dppm)(THF)和dppm的反應…………………27 2.9 [PPh4]2[SeFe3(CO)9] 和[Cu(CH3CN)4]BF4/dppm以1: 2: 1比例 在長時間下反應………………………………………………………28 2.10 [PPh4]2[SeFe3(CO)9]和CuBr以1: 7比例反應………………………29 2.11 以強鹼(KOH~4 M)活化Mn2(CO)10後和Se powder反應………… 29 2.11-1 以Se: Mn = 1: 1的比例反應………………………………………29 2.11-2 以Se: Mn =10: 6的比例反應………………………………………31 2.12 以弱鹼(KOH~0.9 M)活化Mn2(CO)10後和Se powder反應…………34 2.12-1 以Se: Mn = 1: 1的比例反應……………………………………34 2.12-2 以Se: Mn = 10: 6的比例反應……………………………………36 2.13 [PPN]4[Se10Mn6(CO)18]與CH2Cl2的反應……………………………37 2.14 [Et4N]4[Se10Mn6(CO)18]與Mn2(CO)10/KOH的反應……… 38 2.15 [Et4N]4[Se6Mn6(CO)18]與Mn2(CO)10的反應……………… 40 2.16 [Et4N]4[Se6Mn6(CO)18]與Mn2(CO)10/KOH的反應………40 2.17 [Et4N]4[Se6Mn6(CO)18]與Se powder的反應………………41 2.18 [PPN]2[S2Ru3Cr(CO)10]之合成……………………………………42 2.19 [PPN]2[Se2Ru3Cr(CO)10]之合成……………………………………42 2.20 [PPN]2[Te2Mn2Fe (CO)9]之合成……………………………………43 2.21 [Et4N]2[Ru4Cu2Br2(CO)13]的晶體結構解析……………………45 2.22 Te2Fe3(CO)8(dppp)的晶體結構解析………………………49 2.23 [Et4N]3{[SeFe3(CO)9]2Cu}的晶體結構解析……………………52 2.24 [Et4N]3{[SeFe3(CO)9]2Cu2(OAc)}的晶體結構解析……………58 2.25 [SeFe3(CO)9]Cu2(dppe)的晶體結構解析………………………65 2.26 {[SeFe3(CO)9]2Cu2(dppe)}[Cu(dppe)2]2的晶體結構解析………69 2.27 [SeFe3(CO)9]Cu2(dppm)(THF)的晶體結構解析…………73 2.28 [SeFe3(CO)9]Cu2(dppm)(CH3CN)的晶體結構解析……………77 2.29 [SeFe3(CO)8]Cu2(dppm)(dppm)的晶體結構解析………………81 2.30 SeFe3(CO)6(dppm)2的晶體結構解析…………………………85 2.31 [PPh4]2{[SeFe3(CO)9]2Cu4Br2}的晶體結構解析……………… 89 2.32 [Et4N]4[Se6Mn6(CO)18]的晶體結構解析………………………93 2.33 [Et4N]2[Se8Mn4(CO)12(CH2)2]的晶體結構解析………………… 96 2.34 [Et4N]4[Se6Mn6(CO)18(CH2)]的晶體結構解析………………… 99 2.35 [Et4N]2[Se5Mn4(CO)12]的晶體結構解析………………………103 2.36 [PPN]2[S2Ru3Cr(CO)10]的磁性分析………………………………110 2.37 [PPN]2[Se2Ru3Cr(CO)10]的磁性分析………………………………111 2.38 [PPN]2[Te2Mn2Fe(CO)9]的磁性分析………………………………112 2.39 [Et4N]4[Se10Mn6(CO)18]的磁性分析………………………………113 2.40 [Et4N]4[Se6Mn6(CO)18]的磁性分析………………………………114 3. 結果…………………………………………………………………… 115 3.1 E-M-CO與Cu+ 試劑的反應………………………………………… 115 3.1-1 Na2SO3和Ru3(CO)12與[Cu(CH3CN)4]BF4的反應…………………115 3.1-2 [PPN]2[Te10Fe8(CO)20]和[Cu(CH3CN)4]BF4的反應……………116 3.1-3 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4的反應 ………………117 3.1-4 [Et4N]2[SeFe3(CO)9]和CuOAc的反應......................118 3.1-5 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppm or dppe的反應119 3.1-6 {[SeFe3(CO)8]Cu2(μ-dppm)(μ-dppm)}的合成…………………124 3.1-7 SeFe3(CO)6(dppm)2的合成…………………………………………126 3.2 Se-Mn系統…………………………………………………………… 127 3.2-1 以Se: Mn = 1: 1的比例反應………………………………………127 3.2-2 以Se: Mn = 10: 6的比例反應…………………………………… 130 3.3 Se-Mn系統產物間的轉換反應……………………………… 133 3.3-1 [PPN]4[Se10Mn6(CO)18]與CH2Cl2的反應....................133 3.3-2 [Et4N]4[Se10Mn6(CO)18]與Mn2(CO)10的反應……………….. 134 3.3-3 [Et4N]4[Se6Mn6(CO)18]與Se powder的反應………………… 136 3.3-4 [Et4N]4[Se6Mn6(CO)18]與Mn2(CO)10的反應………………… 137 3.4 [Et4N]2[Ru4Cu2Br2(CO)13]的晶體結構……………………………140 3.5 Te2Fe3(CO)8(dppp)的晶體結構…………………………………... 142 3.6 [Et4N]3{[SeFe3(CO)9]2Cu}的晶體結構……………………………144 3.7 [Et4N]3{[SeFe3(CO)9]2Cu2(OAc)}的晶體結構……………………146 3.8 [SeFe3(CO)9]Cu2(dppe)的晶體結構…………………………………148 3.9 {[SeFe3(CO)9]2Cu2(dppe)}[Cu(dppe)2]2的晶體結構……………150 3.10 SeFe3(CO)9Cu2(μ-dppm)(THF)的晶體結構………………………152 3.11 [SeFe3(CO)9]Cu2(dppm)(CH3CN)的晶體結構………………………154 3.12 [SeFe3(CO)8]Cu2(dppm)(dppm)的晶體結構………………………156 3.13 SeFe3(CO)6(dppm)2的晶體結構……………………………………158 3.14 [PPh4]2{[SeFe3(CO)9]2Cu4Br2}的晶體結構………………………160 3.15 [Et4N]4[Se6Mn6(CO)18]的晶體結構………………………………162 3.16 [Et4N]2[Se8Mn4(CO)12(CH2)2]的晶體結構………………………165 3.17 [Et4N]4[Se6Mn6(CO)18(CH2)]的晶體結構…………………………168 3.18 [Et4N]2[Se5Mn4(CO)12]的晶體結構………………………………170 4. 討論…………………………………………………………………… 172 4.1 反應性探討…………………………………………………………… 172 4.1-1 [Et4N]2[SeFe3(CO)9]和Cu+ 試劑之反應性探討 172 4.1-2 [Et4N]2[SeFe3(CO)9]和[Cu(CH3CN)4]BF4/dppm or dppe之反應性探討………………………………………………………………………174 4.1-3 Se-Mn系統之反應性探討……………………………………………184 4.1-4 Se-Mn系統中產物的轉換反應之探討………………………………190 4.2 結構探討……………………………………………………………… 199 4.2-1 (μ5-Se)Fe3(CO)9Cu2(μ-dppm)(L) (L = THF, CH3CN)與(μ5-Se)Fe3(CO)8Cu2(μ-dppm)(μ-dppm)之結構探討......................199 4.2-2 {[SeFe3(CO)9]2Cu2(μ-dppe)}2-和{[SeFe3(CO)9]2Cu2(μ-OAc)}3-之結構探討…………202 4.2-3 [SeFe3(CO)9]Cu2(μ-dppe)、[{SeFe3(CO)9}2Cu4Br2]2-與SeFe3(CO)6(dppm)2之結構探討…………………………………………………204 4.2-4 {[SeFe3(CO)9]2Cu}3-之結構棎討…………………………………206 4.3 IR光譜分析…………………………………………………………...208 4.4 磁性探討……………………………………………………………… 212 4.4-1 E-M系統………………………………………………………………212 4.4-2 E-M-M’系統…………………………………………………………215 5. 結論…………………………………………………………………… 219 6. 參考文獻……………………………………………………………… 221 7. 附圖…………………………………………………………………… 229

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