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作 者:叶剑良[1] 郑发鲲[2] 陈忠[1] 谢鸿琛 陈志伟[1] 黄培强[1]
机构地区:[1]厦门大学化学系 [2]中国科学院福建物质结构研究所结构化学国家重点实验室,福州350002
出 处:《波谱学杂志》2001年第4期315-320,共6页Chinese Journal of Magnetic Resonance
基 金:国家自然科学基金重点资助项目 (No.2 9832 0 2 0 ) ;福建省自然科学基金资助项目 (No .C991 0 0 0 1 )
摘 要:在核磁管内模拟反应体系 (NH4) 3VS4/Et4NBr/CuBr/PPh3在CH2 Cl2 溶液中生成[VS4 Cun](n =3 6 )簇合物的过程 .利用 51 VNMR技术对反应过程进行准原位的实时监测 ,研究 [VS4 Cun](n =3 6 )簇合物的成簇条件和机理以及配体对成簇过程的影响 .本文还详细讨论了反应溶液中不同浓度的PPh3对 [VS4 Cu4]簇合物的51 VNMR化学位移的影响 .The reaction system (NH 4) 3VS 4/Et 4NBr/CuBr/PPh 3 in CH 2Cl 2 for self-assembling of [VS 4-Cu n ] ( n from 3 to 6) clusters was simulated in NMR tube. After the relationship between the 51V NMR chemical shifts and the number of copper atoms in this family cluster was established theoretically and experimentally, 51V NMR was used as a pseudo in situ and real-time method to monitor and identify possible products during the reaction process. The reaction conditions and mechanism about the formation of [VS 4-Cu n ] clusters were investigated by changing the molar ratios of the reactants. The results showed that the concentration of PPh 3 has obvious influence on the 51V chemical shift, and their mechanism is discussed in detail.
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