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研究生: 嚴佳宏
Yen, Chia-Hung
論文名稱: 含口比啶羧酸及口比啶雙羧酸之過渡金屬配位高分子的水熱合成及構造之研究
A Study on Hydrothermal Synthesis and Structures of Transition-Metal Coordination Polymers of Pyridine-carboxylic and -dicarboxylic Acid
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: 2005
畢業學年度: 93
語文別: 中文
論文頁數: 149
中文關鍵詞: 水熱法配位高分子
外文關鍵詞: Coordination Polymer, Hydrothermal Synthesis
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  • 過渡金屬化合物(CoCl2、Zn(NO3)2、Pb(NO3)2、Ni(OAc)2、Ni(NO3)2)與口比啶羧酸(3-pcH和4-pcH)或口比啶雙羧酸(2,3-pdcH2、2,4-pdcH2、2,5-pdcH2、2,6-pdcH2、3,4-pdcH2和3,5-pdcH2),在110~190℃,10~72小時狀況下,經水熱合成,得出
    零維:NCKU-1,[Co(4-pc)2(H2O)4]、
    NCKU-13,[Co(2,6-pdc)2‧Co(H2O)6‧2H2O]
    一維:NCKU-9,[Ni(2,3-pdc)(H2O)3]n、
    二維:NCKU-8,[Pb(2,3-pdc)]n、
    NCKU-16,[Co(3,5-pdc)(H2O)2]n、
    NCKU-18,
    [Cd(2,3-pdc)(H2O)(μ-2,3-pdc)2Ni(2,3-pdc)(H2O)]n
    三維:NCKU-6,[Cd2(2,3-pdc)2(H2O)(μ-2,3-pdc)2]n、
    NCKU-7,[Zn(2,3-pdc)(H2O)]n、
    NCKU-15,{[Co(3,4-pdc)(H2O)2].H2O}n;其中經氫鍵得出,NCKU-1與13(零維經分子間氫鍵形成三維);二維及三維的結構均有孔徑的形成;所有的化合物,均用元素分析,固態IR及UV-vis光譜鑑定,也得單晶X光繞射決定有關的構造;其中3-pcH為3-口比啶羧酸,4-pcH為4-口比啶羧酸,2,3-pdcH2為2,3-口比啶雙羧酸,2,4-pdcH2為2,4-口比啶雙羧酸,2,5-pdcH2為2,5-口比啶雙羧酸,2,6-pdcH2為2,6-口比啶雙羧酸,3,4-pdcH2為3,4-口比啶雙羧酸,3,5-pdcH2為3,5-口比啶雙羧酸。

    Transition-Metal compounds of CoCl2 , Zn(NO3)2, Pb(NO3)2, Ni(OAc)2, and Ni(NO3)2 reacted hydrothermally with pyridyl mono- or dicarboxylic acid of 3-pcH, 4-pcH, 2,3-pdcH2, 2,4-pdcH2, 2,5-pdcH2, 2,6-pdcH2, 3,4-pdcH2, and 3,5-pdcH2 in a autogenous stainless steel bomb under 110-190℃ to produce 0-, 1-, 2-, and 3-dimensional (0D, 1D, 2D, 3D) structures within 10-72 hours (3-pcH=3-pyridylcarboxylic acid,
    4-pcH=4-pyridylcarboxylic acid,
    2,3-pdcH2=pyridine-2,3-dicarboxylic acid,
    2,4-pdcH2=pyridine-2,4-dicarboxylic acid,
    2,5-pdcH2=pyridine-2,5-dicarboxylic acid,
    2,6-pdcH2=pyridine-2,6-dicarboxylic acid,
    3,4-pdcH2=pyridine-3,4-dicarboxylic acid,
    3,5-pdcH2=pyridine-3,5-dicarboxylic acid)
    0D:NCKU-1,[Co(4-pc)2(H2O)4]、
    NCKU-13,[Co(2,6-pdc)2‧2Co(H2O)6‧2H2O]
    1D:NCKU-9,[Ni(2,3-pdc)(H2O)3]n、
    2D:NCKU-8,[Pb(2,3-pdc)]n、
    NCKU-16,[Co(3,5-pdc)(H2O)2]n、
    NCKU-18,
    [Cd(2,3-pdc)(H2O)(μ-2,3-pdc)2Ni(2,3-pdc)(H2O)]n
    3D:NCKU-6,[Cd2(2,3-pdc)2(H2O)(μ-2,3-pdc)2]n、
    NCKU-7,[Zn(2,3-pdc)(H2O)]n、
    NCKU-15,{[Co(3,4-pdc)(H2O)2].H2O}n
    With consideration of hydrogen bonding interactions, NCKU-1and -13 can be converted into 3D structures. All the 2D and 3D structures contain cavities which were also measured. The new structures have been characterized by elemental analysis, solid-state IR and UV-vis spectral measurement, and single-crystal structures via X-ray diffraction data.

    中文摘要…………………………………………Ⅰ Abstract…………………………………………Ⅲ 圖目錄……………………………………………Ⅶ 表目錄……………………………………………Ⅷ 第一章緒論……………………………………..1 第二章實驗………………………………………13 2-1 藥品………………………………………13 2-2 儀器/軟體……………………………….14 2-3 實驗前處理………………………………14 2-4 高分子化合物合成………………………15 第三章實驗結果………………………………..22 第四章討論與結論………………………………38 參考文獻…………………………………………48 附錄一:各結構鍵長附表..................50 附錄二:相關實驗結果…………………….….58 附錄三:晶體常數表……………………………94 附錄四:UV-vis光譜圖……………………….114 附錄五:IR光譜圖…………………………….124 附錄六:已發表論文………………………….144

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