波谱学杂志 ›› 2001, Vol. 18 ›› Issue (4): 315-320.

• 研究论文 • 上一篇    下一篇

[VS4-Cun] (n=3-6) 簇合物成簇反应的51V NMR研究

叶剑良1,  郑发鲲3,  陈忠1,2*, 谢鸿琛1,  陈志伟1,  黄培强1*   

  1. 1.厦门大学化学系; 2.厦门大学物理系, 固体表面物理化学国家重点实验室, 厦门  361005; 3.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
  • 收稿日期:2001-06-22 修回日期:2001-07-23 出版日期:2001-12-05 发布日期:2001-12-05
  • 作者简介:叶剑良(1971-),男,在职博士生.*通讯联系人.
  • 基金资助:

    国家自然科学基金重点资助项目(No.29832020),福建省自然科学基金资助项目(No.C9910001).

51V NMR STUDIES ON THE REACTION OF [VS4Cun](n=3-6) CLUSTERS

YE Jian-Liang1,  ZHENG Fa-Kun3,  CHEN Zhong1,2*, XIE Hong-Chen1, CHEN Zhi-Wei1, HUANG Pei-Qiang1*   

  1. 1.Department of Chemistry; 2.Department of Physics, Xiamen University, State Key Laboratory for Physical Chemistry of Solid Surface, Xiamen  361005; 3.Fujian Institute of Research on the Structure of Matter, The Chinese Academy  of Sciences, State Key Laboratory of Structure Chemistry, Fuzhou 350002
  • Received:2001-06-22 Revised:2001-07-23 Online:2001-12-05 Published:2001-12-05
  • About author:*Correspondence author
  • Supported by:

    国家自然科学基金重点资助项目(No.29832020),福建省自然科学基金资助项目(No.C9910001).

摘要:

在核磁管内模拟反应体系(NH4)3VS4/Et4NBr/CuBr/PPh3在CH2Cl2溶液中生成 [VS4-Cun](n=3-6)簇合物的过程. 利用51V NMR技术对反应过程进行准原位的实时监测,研究[VS4Cun](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51V NMR化学位移的影响.

关键词: 51V NMR, V-Cu-S 簇合物, 成簇机理,  , 动态过程

Abstract:

 The reaction system (NH4)3VS4/Et4Br/CuBr/PPh3 in CH2Cl2 for self -assembling of  [VS4-Cun](n from 3 to 6) clusters was simulated in NMR tube. Aft er the  relationship between the \{\}\+\{51\}V NMR chemical shifts and the number of copper atoms in this family cluster was established theoretically and experime ntally, 51}V NMR was used as a pseudo -in situ- and real-time method to monitor and identify possible prod ucts during the reaction process. The reaction conditions and mechanism about th e formation of [VS4-Cun] clusters were investigated by changing the m olar ratios of the reactants. The results showed that the concentration of PPh3 has obvious influence on the 51V chemical shift, and their mechanism is discussed in detail.

Key words: 51V NMR, Reaction mechanism, V-Cu-S heterometallic cluster, Dynamic process

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