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研究生： 王期麟
Wang, Chi-Lin
論文名稱： 過渡金屬鎘二價苯甲酸鹽系列與多種有機含氮雜環的錯合物之晶體結構設計與性質研究
The Study on Crystal Structure Design and the Properties of Cadmium(II) Complexes with Benzoic Acid Series and Nitrogen heterocycles
指導教授： 許拱北
Shiu, Kom-Bei
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2011
畢業學年度： 99
語文別： 中文
論文頁數： 166
中文關鍵詞： 無機-有機配位高分子
外文關鍵詞： Hybrid Inorganic-Organic Coordination Polymer
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    • 五種pyrazole及imidazole衍生的雙芽配位基與CdO反應，得到12種錯合物，包括單核錯合物[Cd(o-O2CPhCH3)2(mim)]2 (1-2)，雙核錯合物[Cd(O2CPh)2(oim)]2 (2-2a)、[Cd(m-O2CPhCH3)2(oim)]2 (2-2b) 和[Cd(p-O2CPhCH3)2(oim)]2 (2-2c)、與聚合物[Cd(p-O2CPhCH3)2(pim)]n (1-1)、[Cd2(p-O2CPhCH3)4(mpz)2]n (2-1)、[Cd3(m-O2CPhCH3)6(mpz)2]n (3a)、[Cd3(o-O2CPhCH3)6(pim)2]n (3b)、[Cd5(O2CPh)10(mpz)2]n (5)、 [Cd4(m-O2CPhCH3)8(pim)4]n (2-3)、[Cd2(O2CCH2Ph)4(mim)2]n (2-4)和[Cd2(m-O2CPhCH3)4(ppz)]n (6)
    (mim = N1,N1’-m-phenylenedimethylene-bis(imidazole),
    oim = N1,N1’-o-phenylenedimethylene-bis(imidazole),
    pim = N1,N1’-p-phenylenedimethylene-bis(imidazole),
    mpz = N1,N1’-m-phenylenedimethylene-bis(pyrazole),
    ppz = N1,N1’-p-phenylenedimethylene-bis(pyrazole))。
    所有錯合物均藉由元素分析、粉末X-光繞射、固態NMR、UV-vis與IR光譜鑑定，除錯合物2-1, 5, 6外，其他錯合物的固態熱穩定都在340 oC以上，錯合物的發光性質來自於所用的配位基，每一個單晶構造也都進一步由X-光單晶繞射數據決定。

    Five nitrogen bidentates, derived from pyrazole and imidazole, reacted with CdO to form twelve Cd compounds, including: mononuclear complex of [Cd(o-O2CPhCH3)2(mim)]2(1-2); dinuclear complexes of [Cd(O2CPh)2(oim)]2(2-2a), [Cd(m-O2CPhCH3)2(oim)]2(2-2b), and [Cd(p-O2CPhCH3)2(oim)]2(2-2c); and polymers of [Cd(p-O2CPhCH3)2(pim)]n(1-1), [Cd2(p-O2CPhCH3)4(mpz)2]n(2-1), [Cd3(m-O2CPhCH3)6(mpz)2]n(3a), [Cd3(o-O2CPhCH3)6(pim)2]n(3b), [Cd5(O2CPh)10(mpz)2]n(5), [Cd4(m-O2CPhCH3)8(pim)4]n(2-3), [Cd2(O2CCH2Ph)4(mim)2]n(2-4) and [Cd2(m-O2CPhCH3)4(ppz)]n(6)
    (mim=N1,N1’-m-phenylenedimethylene-bis(imidazole),
    oim=N1,N1’-o-phenylenedimethylene-bis(imidazole),
    pim=N1,N1’-p-phenylenedimethylene-bis(imidazole),
    mpz=N1,N1’-m-phenylenedimethylene-bis(pyrazole),
    ppz=N1,N1’-p-phenylenedimethylene-bis(pyrazole))。
    All complexes were characterized by elemental analyses, powder X-ray diffraction, solid-state NMR, UV-VIS and IR spectra. Except complexes 2-1, 5 and 6, other complexes are thermally stable in the solid state above 340 oC. The photoluminescence property of the complexes comes from that of the used bidentates. Single-crystal structures of each complex were also determined by X-ray single-crystal diffraction data.

    摘要 1 Abstract 2 致謝 3 目錄 5 表目錄 8 附表目錄 9 圖目錄 10 附圖目錄 12 第一章 緒論 15 1-1 晶體工程 15 1-2 無機－有機配位高分子 17 1-3 文獻回顧 20 1-4 實驗動機 27 第二章 實驗部分 28 2-1 實驗儀器/軟體與實驗操作 28 2-2 實驗藥品 32 2-3 實驗合成 33 2-3-1有機ligand起始物合成 33 2-3-2金屬鹽類起始物合成 38 2-3-3鎘金屬錯合物[Cd(p-O2CPhCH3)2(pim)]n (1-1)的合成 39 2-3-4鎘金屬錯合物[Cd(o-O2CPhCH3)2(mim)]2 (1-2)的合成 39 2-3-5鎘金屬錯合物[Cd2(p-O2CPhCH3)4(mpz)2]n (2-1)的合成 40 2-3-6鎘金屬錯合物[Cd(O2CPh)2(oim)]2 (2-2a)的合成 40 2-3-7鎘金屬錯合物[Cd(m-O2CPhCH3)2(oim)]2 (2-2b)的合成 40 2-3-8鎘金屬錯合物[Cd(p-O2CPhCH3)2(oim)]2 (2-2c)的合成 41 2-3-9鎘金屬錯合物[Cd4(m-O2CPhCH3)8(pim)4]n (2-3)的合成 41 2-3-10鎘金屬錯合物[Cd2(O2CCH2Ph)4(mim)2]n (2-4)的合成 42 2-3-11鎘金屬錯合物[Cd3(m-O2CPhCH3)6(mpz)2]n (3a)的合成 42 2-3-12鎘金屬錯合物[Cd3(o-O2CPhCH3)6(pim)2]n (3b)的合成 42 2-3-13鎘金屬錯合物[Cd5(O2CPh)10(mpz)2]n (5)的合成 43 2-3-14鎘金屬錯合物[Cd2(m-O2CPhCH3)4(ppz)]n (6)的合成 43 第三章 結果與討論 44 3-1單晶結構 44 3-1-1錯合物(1-1) 44 3-1-2錯合物(2-1) 47 3-1-3錯合物(3a) 51 3-1-4錯合物(3b) 54 3-1-5錯合物(5) 57 3-1-6錯合物(1-2) 61 3-1-7錯合物(2-2a) 63 3-1-8錯合物(2-2b) 65 3-1-9錯合物(2-2c) 67 3-1-10錯合物(2-3) 70 3-1-11錯合物(2-4) 74 3-1-12錯合物(6) 77 3-2金屬中心Cd的幾何配位 80 3-3羧酸根的配位模式 82 3-4紫外光 – 可見光光譜與螢光放光光譜 84 3-5熱重量分析儀 85 第四章 結論 87 參考資料 89 附錄 93

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