臺灣博碩士論文加值系統

本論文的研究重點在於以80℃類似水熱法的環境下，使其在均相中溫和反應合成新的無機/有機配位高分子化合物。本研究成功的合成出九個新的高分子化合物，並利用X光單晶繞射儀(single crystal X-ray diffractometer)進行結構鑑定。Cd(adipate)(H2O)2(1)之空間群為單斜晶系C2/c，晶格參數a = 16.507(2) Å，b = 5.585(0) Å，c = 11.074(1) Å，β= 95.17(1)°，V = 1016.3(2) Å3。Cd3(citrate)2(H2O)2(2)之空間群為單斜晶系P21/c，晶格參數a = 6.108(1) Å，b = 15.316(2) Å，c = 9.787(1) Å，β= 102.89(1)°，V = 892.5(2) Å3。Co(adipate)(bpe)(3) [bpe = 1,2-bis(4-pyridyl)ethane]之空間群為三斜晶系P-1，晶格參數a = 8.482(1) Å，b = 9.374(1) Å，c = 11.409(1) Å，α= 98.42(1)°，β= 95.17(1)°，γ= 106.07(1)°，V = 854.1(2) Å3。Mn(adipate)(bpe)(4)之空間群為三斜晶系P-1，晶格參數a = 8.433(1) Å，b = 9.406(1) Å，c = 11.476(2) Å，α= 97.02(1)°，β= 94.66(2)°，γ= 105.15(1)°，V = 866.0(2) Å3。Co(adipate)(trans-bpe)(5) [trans-bpe = trans-1,2-bis -(4-pyridyl)ethylene]之空間群為三斜晶系P-1，晶格參數a = 8.297(1) Å，b = 9.096(2) Å，c = 11.343(2) Å，α= 96.96(1)°，β= 96.24(2)°，γ= 103.40(1)°，V = 818.3(3) Å3。Mn(adipate)(trans-bpe)(6)之空間群為三斜晶系P-1，晶格參數a = 8.217(1) Å，b = 9.150(1) Å，c = 11.384(3) Å，α= 95.88(1)°，β= 95.65(2)°，γ= 102.54(1)°，V = 824.63(22) Å3。Co(adipate)(bpd)1.5(H2O)2•H2O(7)[bpd = 1,4-bis(3-pyridyl)-2,3-diaza -1,3-butadiene]之空間群為三斜晶系P-1，晶格參數a = 9.233(2) Å，b = 11.284(1) Å，c = 13.703(1) Å，α= 79.45(1)°，β= 73.11(1)°，γ= 75.28(1)°，V = 1312.0(3) Å3。Co3(citrate)2(4,4’-bipy)4(H2O)2•4H2O(8) [4,4’-bipy = 4,4’-bipyridine]之空間群為三斜晶系P-1，晶格參數a = 10.850(1) Å，b = 11.534(2) Å，c = 13.608(1) Å，α= 66.17(1)°，β= 81.40(1)°，γ= 63.15(1)°，V = 1388.7(3) Å3。[Co(trans-bpe)(H2O)4] [Co2(citrate)2(trans-bpe)(H2O)2]•2H2O(9)之空間群為三斜晶系P-1，晶格參數a = 8.270(1) Å，b = 9.861(1) Å，c = 13.634(1) Å，α= 83.42(1)°，β= 78.46(1)°，γ= 79.02(1)°，V = 1388.7(3) Å3。
化合物(1)為一維鏈狀結構，(2)經由檸檬酸根以T型的形式和Cd(1)形成階梯狀結構，再藉由Cd(2)連接成為二維層狀結構，化合物(3)~(6)為相似的結構，其不同之處在於以[MII(adipate)]平面(M = Co, Mn)藉由有機中性配基形成三維空間結構時，(3)~(4)是利用bpe而(5)~(6)則是利用trans-bpe，而這四個配位化合物是以交錯的形式存在。化合物(7)為[Co(adipate)(H2O)2]鏈狀結構以bpd為連結分子形成二維層狀結構。化合物(8)以[Co3(citrate)2(H2O)2]形成一維鏈狀，然後再經由4,4’-bipy連接形成一多孔狀之三維空間結構，具有小分子吸附的能力，利用熱重分析儀作如甲醇、乙醇和苯等一些小分子的吸附-脫附實驗。而化合物(9)則是由二個一維鏈狀結構[Co(trans-bpe)(H2O)4]2+和[Co2(citrate)2(trans-bpe)(H2O)2]2-所組成。

Nine novel coordination polymers: Cd(adipate)(H2O)2(1), Cd3(citrate)2(H2O)2(2), M(adipate)(bpe) [M=Co(3)、Mn(4)], M(adipate)(trans-bpe) [M=Co(5)、Mn(6)] , Co(adipate)(bpd)1.5(H2O)2•H2O(7), Co3(citrate)2(4,4’-bipy)4(H2O)2•4H2O(8) and [Co(trans-bpe)(H2O)4][Co2(citrate)2(trans-bpe)(H2O)2]•2H2O(9) (bpe = 1,2-bis -(4-pyridyl)ethane, trans-bpe = trans-1,2-bis(4-pyridyl)ethylene, bpd = 1,4-bis(3 -pyridyl)-2,3-diaza-1,3-butadiene, 4,4’-bipy = 4,4’-bipyridine), were synthesized at 80℃ in drying oven and characterized by X-ray crystallographic techniques. (1) crystallizes in triclinic space group P-1 with a = 16.507(2) Å, b = 5.585(0) Å, c = 11.074(1) Å, β= 95.17(1)°, V = 1016.3(2) Å3. (2) crystallizes in triclinic space group P-1 with a = 6.108(1) Å, b = 15.316(2) Å, c = 9.787(1) Å, β= 102.89(1)°, V = 892.5(2) Å3. (3) crystallizes in triclinic space group P-1 with a = 8.482(1) Å, b = 9.374(1) Å, c = 11.409(1) Å, α= 98.42(1)°, β= 95.17(1)°, γ= 106.07(1)°, V = 854.1(2) Å3. (4) crystallizes in triclinic space group P-1 with a = 8.433(1) Å, b = 9.406(1) Å, c = 11.476(2) Å, α= 97.02(1)°, β= 94.66(2)°, γ= 105.15(1)°, V = 866.0(2) Å3. (5) crystallizes in triclinic space group P-1 with a = 8.297(1) Å, b = 9.096(2) Å, c = 11.343(2) Å, α= 96.96(1)°, β= 96.24(2)°, γ= 103.40(1)°, V = 818.3(3) Å3. (6) crystallizes in triclinic space group P-1 with a = 8.217(1) Å, b = 9.150(1) Å, c = 11.384(3) Å, α= 95.88(1)°, β= 95.65(2)°, γ= 102.54(1)°, V = 824.63(22) Å3. (7) crystallizes in triclinic space group P-1 with a = 9.233(2) Å, b = 11.284(1) Å, c = 13.703(1) Å, α= 79.45(1)°, β= 73.11(1)°, γ= 75.28(1)°, V = 1312.0(3) Å3, V = 824.63(22) Å3. (8) crystallizes in triclinic space group P-1 with a = 10.850(1) Å, b = 11.534(2) Å, c = 13.608(1) Å, α= 66.17(1)°, β= 81.40(1)°, γ= 63.15(1)°, V = 1388.7(3) Å3. (9) crystallizes in triclinic space group P-1 with a = 8.270(1) Å, b = 9.861(1) Å, c = 13.634(1) Å, α= 83.42(1)°, β= 78.46(1)°, γ= 79.02(1)°, V = 1388.7(3) Å3.
The structure of (1) consists of one-dimensional chains built up by [Cd(H2O)2]2+ units bridged by adipates. (2) is constructed by Cd(1) and T-shaped citrate, forming a ladder-like chains cross-linked by Cd(2) to form two-dimensional layers. Compounds (3)~(6) have similar structures which contain two sets of interpenetrated open frameworks. (3)-(4) are constructed by [Co(adipate)] sheets cross-linked by 1,2-bis(4-pyridyl)-ethane to form three-dimensional coordination networks and compounds (5)-(6) form 3-D frameworks by trans-1,2-bis(4-pyridyl)ethene. (7) adopts a two-dimensional framework, formed by [Co(adipate)(H2O)2] chains cross-linked by 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene ligands. (8) consists of a porous three-dimensional framework built up by [Co3(citrate)2(H2O)2] moieties cross-linked by 4,4’-bipy ligands. Its sorption-desorption behaviors of some small molecules such as methanol, ethanol and benzene etc have investigated. (9) consists two one-dimensional chains, cationic [Co(trans-bpe)(H2O)4]2+ and anionic [Co2(citrate)2(trans-bpe)(H2O)2]2-.

中英文摘要----------------------------------------------- 1
第一章 緒論---------------------------------------------- 5
第二章 有機-無機配位高分子化合物之開發
2.1實驗儀器-------------------------------------- 13
2.2藥品出處-------------------------------------- 14
2.3實驗步驟-------------------------------------- 15
2.4紅外吸收光譜---------------------------------- 21
2.5 X光單晶繞射實驗及構造解析-------------------- 28
2.6 X光粉末繞射圖-------------------------------- 35
2.7熱分析---------------------------------------- 49
2.8磁性分析-------------------------------------- 57
第三章 結果與討論--------------------------------------- 59
第四章 結論--------------------------------------------- 86
參考文獻------------------------------------------------ 87
附圖---------------------------------------------------- 94
附表--------------------------------------------------- 109

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