論文使用權限 Thesis access permission:校內校外均不公開 not available
開放時間 Available:
校內 Campus:永不公開 not available
校外 Off-campus:永不公開 not available
論文名稱 Title |
苯酚膦化物鐵、鋅錯合物之製備及結構鑑定 Preparation and Structural Characterization of Iron and Zinc Complexes Containing a Chelating Phenolato Phosphine Ligand |
||
系所名稱 Department |
|||
畢業學年期 Year, semester |
語文別 Language |
||
學位類別 Degree |
頁數 Number of pages |
265 |
|
研究生 Author |
|||
指導教授 Advisor |
|||
召集委員 Convenor |
|||
口試委員 Advisory Committee |
|||
口試日期 Date of Exam |
2009-12-03 |
繳交日期 Date of Submission |
2010-02-02 |
關鍵字 Keywords |
鋅、鐵、苯酚膦化物 Phenolato Phosphine Ligand, Zinc, Iron |
||
統計 Statistics |
本論文已被瀏覽 5675 次,被下載 0 次 The thesis/dissertation has been browsed 5675 times, has been downloaded 0 times. |
中文摘要 |
我們利用實驗室先前所合成的(Ph-OPO)Na2•(DME)2的化合物作為ligand,分別與一當量和0.5當量的FeCl2反應,都順利合成出兩個順磁性錯合物,也分別做了Evans method和SQUID的實驗,分別對其液態和固態做磁性上的測量,並且也進一步加以討論其磁性現象。 接著我們將原有的H2(Ph-OPO),做進一步的設計,把在donor atom磷上的取代基,由phenyl改為tert-butyl,得到一新的雙苯酚磷化物2,2’-tert-butylphosphinobis(4,6-di-tert-butylphenolate) [(tBu-OPO)2-],嘗試藉由取代基不同的立體障礙與陰電效應,希望能夠得到不同結果,並且拿H2(Ph-OPO)與H2(tBu-OPO),跟一系列鋅(Zn)金屬化合物的反應,利用X-ray及不同核種的NMR鑑定其組成。 |
Abstract |
none |
目次 Table of Contents |
苯酚膦化物鐵、鋅錯合物 壹、緒論..................................................................................................................1 貳、結果與討論......................................................................................................4 1. [(Ph-OPO)Fe]2·(THF)2的合成與鑑定......................................................4 2. (Ph-OPOH)2Fe·(THF)2的合成與鑑定.....................................................14 3. Zn(tBu-OPOLi)2·(THF)2的合成與鑑定…………………………..……20 4. Zn(tBu-OPOH)2·CH3CN的合成與鑑定..................................................26 5. Zn(Ph-OPOH)2的合成與鑑定.................................................................31 6. Zn2(tBu-OPO)2·THF的合成與鑑定........................................................33 7. Zn2(Ph-OPO)2·(THF)2的合成與鑑定......................................................40 參、結論................................................................................................................46 肆、實驗部分........................................................................................................37 一、一般程序............................................................................. ................49 二、儀器........................................................................................................49 三、實驗步驟................................................................................................50 1. 合成2-bromo-4,6-di-tert-butyl-phenol (HYS1-200) .....................51 2. 合成 (Ph-OPO)H2 (HYS1-155)......................................................51 3. 合成(Ph-OPO)Na2·(DME)2 (HYS1-107) .......................................51 4. 合成H2(tBu-OPO) (HYS2-228) ...................................................52 5. 合成[(Ph-OPO)Fe]2·(THF)2 (HYS1-221) ......................................52 6. 合成(Ph-OPOH)2Fe·(THF)2 (HYS2-245) ......................................53 7. 合成Zn(tBu-OPOLi)2·(THF)2 (HYS2-206) …...............................53 8. 合成Zn(tBu-OPOH)2·CH3CN (HYS2-202)....................................54 9. 合成Zn(Ph-OPOH)2 (HYS2-252、253) .........................................55 10. 合成Zn2(tBu-OPO)2·THF (HYS2-223) .........................................56 11. 合成Zn2(Ph-OPO)2·(THF)2 (HYS2-251) ......................................57 伍、參考文獻........................................................................................................58 |
參考文獻 References |
參考文獻 [1] Fryzuk, M. D.; Johnson, S. A. Coord. Chem. Rev. 2000, 200-202, 379. [2] Fryzuk, M. D. Chem. Rec. 2003, 3, 2. [3] Shaver, M. P.; Fryzuk, M. D. AdV. Synth. Catal. 2003, 345, 1061. [4] MacKay, B. A.; Fryzuk, M. D. Chem. Rev. 2004, 104, 385. [5] Fryzuk, M. D.; Johnson, S. A.; Patrick, B. O.; Albinati, A.; Mason, S. A.; Koetzle, T. F. J. Am. Chem. Soc. 2001, 123, 3960. [6] Studt, F.; MacKay, B.; Fryzuk, M. D.; Tuczek, F. J. Am. Chem. Soc. 2003, 126, 280. [7] Studt, F.; Johnson, S. A.; MacKay, B.; Patrick, B. O.; Fryzuk, M. D.; Tuczek, F. Chem.-Eur. J. 2005, 11, 385. [8] Fryzuk, M. D.; MacKay, B. A.; Johnson, S. A.; Patrick, B. O. Angew. Chem., Int. Ed. 2002, 41, 3709. [9] Schrock.R. R, Acc. Chem. Res. 1997, 30, 9. [10] Zanetii. N.C; Schrock. R. R; Davis. W. M. Angew. Chem. Int. Ed. Engl. 1995. 34. 2044. [11] Cummins.C. C; Lec. J; Schrock. R. R. Angew. Chem. Int. Ed. Engl. 1992. 31. 1501. [12] Cummins. C. C; Schrock. R. R; Davis, W. M. Angew. Chem. Int. Ed. Engl. 1993, 32, 756. [13] Cummins. C. C.; Schrock. R. R.; Davis. W. M.; Freundich. J. S, J. Am. Chem. Soc., 1994, 116, 6476. [14] Cummins. C. C; Schrock. R. R.; Davis. W. M. Inorg Chem, 1994, 33, 1488. [15] Kol. M; Schrock.R. R; Kempe. R; Davis. W. M. J. Am. Chem. Soc. 1994. 116. 4382. [16] Cummins. C. C.; Schrock. R. R.; Davis. W. M.; Freundich. J. S, J. Am. Chem. Soc ,1996, 118, 3643. [17] Lopez. L. P.; Schrock. R. R; Bonitatebus. P .J. Inorg. Chim. Acta, 2006, 359, 4730 [18] Nomura. K.; Schrock. R. R. Inorg Chem, 1996, 35, 3695. [19] Yandulov. D. V.; Schrock, R. R. J. Am. Chem. Soc, 2002, 124, 6252. [20] Yandulov. D. V.; Schrock, R. R. SCIENCE, 2003, 301, 76. [21] Ritleng. V;Yandulov. D. V;Weare. W. W; Schrock. R. R;Hock. A. S; Davis. W. M. J. Am. Chem. Soc. 2004. 126. 6150.. [22] Smythe. N. C; Schrock. R. R; Muller. P; Weare. W. W. Inorg Chem, 2006, 45, 9197. [23] Liang, L.-C. Coord. Chem. Rev. 2006, 250, 1152–1177. [24] Chien, P.-S.; Liang, L.-C. Inorg. Chem. 2005, 44, 5147–5151. [25] Huang, M.-H.; Liang, L.-C. Organometallics 2004, 23, 2813–2816. [26] Lee, W.-Y.; Liang, L.-C. Dalton Trans. 2005, 1952–1956. [27] Liang, L.-C.; Lin, J.-M.;Hung,C.-H. Organometallics 2003, 22, 3007–3009. [28] Liang, L.-C.; Lee, W.-Y.; Hung, C.-H. Inorg. Chem. 2003, 42, 5471–5473. [29] Liang, L.-C.; Huang, M.-H.; Hung, C.-H. Inorg. Chem. 2004, 43, 2166–2174. [30] Liang, L.-C.; Lee, W.-Y.; Yin, C.-C. Organometallics 2004, 23, 3538–3547. [31] Liang, L.-C.; Chien, P.-S.; Huang, M.-H. Organometallics 2005, 24, 353–357. [32] Liang, L.-C.; Lin, J.-M.; Lee,W.-Y. Chem. Commun. 2005, 2462–2464. [33] Liang, L.-C.; Chien, P.-S.; Lin, J.-M.; Huang, M.-H.; Huang, Y.-L.; Liao, J.-H. Organometallics 2006, 25, 1399–1411. [34] Liang, L.-C.; Chien, P.-S.; Huang, Y.-L. J. Am. Chem. Soc. 2006, 128, 15562–15563. [35] Chang, Y.-N.; Liang, L.-C. Inorg. Chim. Acta 2007, 360, 136–142. [36] Liang,L.-C.;Chang,Y.-N.;Lee,H.M. Inorg.Chem. 2007, 46, 2666–2673. [37] Liang, L.-C.; Chien, P.-S.; Lee, P.-Y.; Lin, J.-M.; Huang, Y.-L. Dalton Trans. 2008, 3320–3327. [38] Liang, L.-C.; Chien, P.-S.; Lee, P.-Y. Organometallics 2008, 27, 3082–3093. [39] Liang, L.-C.; Chang, Y.-N.; Chen, H.-S.; Lee, H. M. Inorg. Chem. 2007, 46, 7587–7593. [40] Liang, L.-C.; Cheng, L.-C.; Tsai, T.-L.; Hu, C.-H.; Guo, W.-H. Inorg. Chem. 2009, 48, 5697-5703. [41] Siefert, R.; Weyhermuller, T.; Chaudhuri, P. J. Chem. Soc., Dalton Trans. 2000, 4656-4663. [42] 張御甯(2006) 「Metal Complexes of a Chelating Diphenolate Phosphine Ligand」,國立中山大學化學所碩士論文. [43] 陳漢陞(2008) 「Preparation and Structure Characterization of Metal Complexes Containing a Chelating Phenolato orAmido Ligand」,國立中山大學化學所碩士論文. [44] 許毓麟 梁蘭昌實驗室碩士班研究生 [45] Clementi, E.; Raimondi, D. L.; Reinhardt, W. P. J. Chem. Phys. 1967,47, 1300. [46] Hendrich, M. P.; Day, E. P.; Wang, C.-P.; Synder, B. S.; Holm, R. H.; Munck, E. Inorg. Chem. 1994, 33, 2848-2856. |
電子全文 Fulltext |
本電子全文僅授權使用者為學術研究之目的,進行個人非營利性質之檢索、閱讀、列印。請遵守中華民國著作權法之相關規定,切勿任意重製、散佈、改作、轉貼、播送,以免觸法。 論文使用權限 Thesis access permission:校內校外均不公開 not available 開放時間 Available: 校內 Campus:永不公開 not available 校外 Off-campus:永不公開 not available 您的 IP(校外) 位址是 3.142.98.108 論文開放下載的時間是 校外不公開 Your IP address is 3.142.98.108 This thesis will be available to you on Indicate off-campus access is not available. |
紙本論文 Printed copies |
紙本論文的公開資訊在102學年度以後相對較為完整。如果需要查詢101學年度以前的紙本論文公開資訊,請聯繫圖資處紙本論文服務櫃台。如有不便之處敬請見諒。 開放時間 available 已公開 available |
QR Code |