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研究生:李振榮
研究生(外文):Lee Jen Rong
論文名稱:銠(Ⅲ)及銥(Ⅲ)金屬錯合物的合成、光物理及電化學性質的探討
論文名稱(外文):The Synthetic, Photophysical and Electrochemical Studies of Rh(III) and Ir(III) Complexes
指導教授:黃文亮黃文亮引用關係
指導教授(外文):Huang Wen Liang
學位類別:博士
校院名稱:國立成功大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
論文頁數:129
中文關鍵詞:二亞胺混配基放光磷光電荷轉移電化學
外文關鍵詞:diiminemixed-ligandLuminescencephosphorescencecharge transferElectrochemical
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摘 要
本研究第一部份合成了銠(III)及銥(III)金屬與下列配位子:1,10-phenanthroline (phen),2,2''-bipyridine (bipy),2,2''-dipyridylamine (HDPA),2-pyridyl N-methyl-2-imidazolyl ketone (pik),di-2-pyridyl ketone (dpk),phenyl-pyridin-2-ylmethylene-amine (PA),2-(arylazo) pyridine (Azpy) 等所形成的單二亞胺錯合物,以NMR光譜鑑定,並與一些文獻上所記載過的單配位錯合物相比較,發現我們的合成方法不管是在步驟或產率上均較文獻上來得簡單及有效,使得在往後的混配基錯合物的合成方法上具有較多的合成途徑。
第二部分合成了cis-[Rh(pik)2Cl2] +,第三部分合成cis-[Rh(dpk)2Cl2]+、cis-[Rh(dpk)(phen)Cl2] +及cis-[Rh(dpk)(bipy)Cl2]+等二亞胺酮錯合物,以MS、IR、和NMR光譜鑑定其組成及結構。四個錯合物的吸收光譜均呈現配子的pp*吸收,而屬於二亞胺酮的np*吸收則可能被埋在較強pp*吸收之下而無法觀察。在低能量區的電荷轉移及dd*過渡可能因為強度太弱而無法解析,這可由他們的放光極化光譜所呈現的偏極值(P值)轉變來佐證。在放光部分,四種錯合物在室溫均沒有偵測到放光。在低溫(77K)甲醇/乙醇(體積比4:1)混合溶劑中皆可在12 kK ~ 19 kK之間觀測到一個寬廣、對稱且不具結構性的放光帶,最強的放光帶則在16 kK ~ 15 kK 之間,半生期則大約數十個ms,並由其放光極化光譜呈現一斜率趨近於0的平坦曲線推測,這四種錯合物的放光屬於單一型態的dd*放光。在電化學方面則經由循環伏安法、定電位電解等方法,並藉由添加phenol的幫助,推測四個錯合物的最初兩個電子是還原在金屬上,且還原之後皆伴隨有兩個氯離子的脫落反應。而在cis-[Rh(pik)2Cl2] +及cis-[Rh(dpk)2Cl2]+中,第三個電子是還原在金屬上,而第四個電子則是還原在配子的CO上。在cis-[Rh(dpk)(phen)Cl2] +及cis-[Rh(dpk)(bipy)Cl2]+則發現第三及第四個電子皆還原在金屬上。
第四部分則是Ir(bzpy)(phen)Cl2 (bzpy = ortho-C-deprotonated form of 2-benzoylpyridine)的合成與鑑定,經由MS、IR及NMR光譜的幫助,推測所得化合物為bzpy以N-C-配位的cis-a結構,此錯合物在紫外-可見光能量範圍內可見明顯屬配位子pp* 躍遷的吸收峰線,在約25~28 kK有一中等強度的吸收,屬自旋允許的電荷轉移過渡。由激發極化光譜中的偏極值(P值),顯示其放光是源自於線性振動子。放光在低溫 77 K下,可偵測到在 16~22 kK範圍內出現不對稱而具結構性之放光,且生命期約在10 ms左右。在放光極化光譜上,由放光區間內斜率呈現平滑趨近於0之譜線判斷,此放光為單一型態。但在文獻中,ortho-metalated 錯合物有所謂的SBLCT(σ bond to ligand charge transfer)電荷轉移機構。因此,單從放光的研究是無法判斷放光型態是屬3MLCT或SBLCT放光。
在電化學研究方面,在0~-2.0 V vs. SCE可觀察到二個單電子還原波;在0~+2.0 V vs. SCE可觀察到一個氧化波。由於第一還原峰(Epc)I會因phenol的出現而有顯著的改變,因而推測第一單電子是還原到bzpy羰基上之p*軌域上。又因其氧化過程是一完全不可逆氧化波,由此可確定混配基型錯合物之過渡型態是屬SBLCT電荷轉移過渡。
Abstract
The research performed in this works constitutes four major parts. The synthetic methods of Rh(III) and Ir(III) complexes coordinated with various ligands including 1,10-phenanthroline (phen), 2,2''-bipyridine (bipy), 2,2''-dipyridyl-amine (HDPA), 2-pyridyl N-methyl-2-imidazolyl ketone (pik), di-2-pyridyl ketone (dpk), phenyl-pyridin-2-ylmethylene-amine (PA) or 2-(arylazo)pyridine (Azpy) are given in the first part. These compounds are characterized by NMR spectroscopic techniques. Compared with analogous studies in the literature, it has been found that our synthetic routes are more efficient and simplified. The study performed here, therefore, provides valuable information for chemists interested in synthesis of complexes coordinated with mixed ligands.
The photophysical and electrochemical studies, as well as the synthetic work, of cis-[Rh(pik)2Cl2] + are contained in the second part. The same studies performed on cis-[Rh(dpk)2Cl2]+, cis-[Rh(dpk)(phen)Cl2] + and cis-[Rh(dpk)- (bipy)Cl2]+ are given in the third part of this research. The compositions and conformer elucidations are accomplished by MS、IR、and NMR spectroscopic methods. Absorption, emission and polarization spectra of all these complexes are examined in detail to confirm the transition types and orbitals involved in the transition. Electrochemical experiments including cyclic voltammetry (CV) and controlled-potential electrolysis (CPE) have also been carried out to acquire supplementary and complementary information. The sites that accommodate electrons in electrochemical reactions are also thoroughly discussed.
The last part is focused on the Ir(bzpy)(phen)Cl2 (bzpy = ortho-C- deprotonated form of 2-benzoylpyridine) complex. Through MS, IR and NMR spectroscopies studies, we infer that (1) the bzpy ligand is attached to the metal ion with the N-C- coordination pattern and (2) the complex exhibits the cis-a conformation. This complex shows apparent absorption in the UV-vis region which is classified as the ligand pp* transition. The medium-intensity absorption observed in 25~28 kK is assigned as spin-allowed CT transition. The emission behavior observed at low temperature (77K) of this complex originated from linear oscillators according to the values of polarization obtained by excitation-polarization spectra. Electrochemical studies of this complex have also been undertaken. It is noteworthy that the electron transition can be verified via SBLCT (σbond to ligand charge transfer) mechanism, which cannot be distinguished by electronic spectroscopy alone.
目 錄
表目錄 I
圖目錄 II
壹、銠(III)及銥(III)金屬單二亞安胺錯合物的合成及鑑定 1
一、緒論 1
二、實驗部分 3
I、儀器設備 3
II、藥品 3
III、合成 4
三、結果與討論 12
I、合成方面 12
II、鑑定方面 13
四、結論 15
五、參考文獻 16
貳、銠(III)金屬不對稱二亞胺酮錯合物的合成、
光物理及電化學性質的探討 42
一、緒論 42
二、實驗部分 49
I、試劑 49
II、儀器設備 50
III、化合物的製備 52
三、結果與討論 54
I、合成與鑑定部份 54
II、光物理部分 55
III、化合物之電化學性質 56
四、結論 61
五、參考文獻 62
目 錄
參、銠(III)金屬與2,2''-二?啶酮錯合物的合成、
光物理及電化學性質的探討 74
一、緒論 74
二、實驗部分 76
I、藥品及儀器 76
II、合成部分 76
三、結果與討論 78
四、結論 83
五、參考文獻 84
肆、含2-苯基酮?啶之混配基型銥(III)錯合物的合成、
光物理及電化學性質的探討 103
一、緒論 103
二、實驗部分 105
I、藥品及儀器 105
II、錯合物的製備 105
三、結果與討論 106
I、錯合物的合成及鑑定 106
II、紫外-可見光吸收光譜與激發極化光譜 108
III、放光及放光極化光譜 110
IV、電化學 112
四、結論 114
五、參考文獻 116
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