| 桥联8-氨基喹啉衍生物及其锆配合物的合成及结构 |
| Synthesis and Structures of Symmetric Bridged 8-Aminoquinolinyl Derivatives and Their Zirconium Complexes |
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| 摘要: 以8-氨基喹啉和8-氨基喹哪啶为原料，通过锂化再与二甲基二氯硅烷反应，分别得到对称的桥联配体Me2Si[NH（C9H6N）]2 （1a），Me2Si[NCH3（C9H5N）]2 （1b）。1a和1b分别与2倍物质的量的正丁基锂反应，然后与ZrCl4作用得到2种配位模式不同的硅桥联取代8-氨基喹啉锆配合物Zr{Me2Si[N（C9H6N）]2}2 （2）和Zr{Me2Si[NCH3（C9H5N）]2}Cl2 （3）。化合物1~3通过1H NMR、13C NMR和元素分析进行表征，2和3通过X-射线单晶衍射确定其晶体结构。结果表明配合物2的中心Zr原子与8个N原子配位，属于变形十二面体结构，单晶属于三斜晶系；配合物3的中心Zr原子与4个N原子和2个Cl原子配位，属于变形八面体，单晶属于正交晶系。 |
| 关键词: 8-氨基喹啉 桥联 锆配合物 合成 晶体结构 |
| 基金项目: 国家自然科学基金（No.20942009，21072120）；山西省科技攻关计划（No.20110321055）；山西省回国留学人员科研资助项目（No.2013010）。 |
| Abstract: Treatment of 8-aminoquinoline and 8-aminoquinadine with n-BuLi in Et2O followed by reacting with dimethyl dichlorosilane, give symmetrical bridged quinolinyl ligands Me2Si[NH(C9H6N)]2 (1a) and Me2Si[NCH3(C9H5N)]2 (1b) successfully. Reaction of quinolinyl ligands 1a and 1b with n-BuLi in THF, separately, then reacting with ZrCl4 in situ afford two kinds of multidentate complexes Zr{Me2Si[N(C9H6N)]2}2 (2) and Zr{Me2Si[NCH3(C9H5N)]2}Cl2 (3). All the compounds have been confirmed and characterized by 1H NMR, 13C NMR and elemental analysis. Complexes 2 and 3 were characterized by single-crystal X-ray diffraction analysis. A distorted dodecahedron of N8 atoms has been found for the zirconium(Ⅳ) center of complex 2, and the crystal of complex 2 belongs to triclinic space group. Complex 3 is a distorted octahedron for the zirconium(Ⅳ) center and belongs to orthorhombic space group. CCDC: 958191, 2; 999854, 3. |
| Keywords: 8-aminoquinoline bridged Zr complex synthesis crystal structure |
| 投稿时间：2014-05-01 修订日期：2014-05-17 |
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| 王鹏,李中元,冯颖,薛小燕,陈霞.桥联8-氨基喹啉衍生物及其锆配合物的合成及结构[J].无机化学学报,2014,30(10):2360-2366. |
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