物理化学学报 >> 2000, Vol. 16 >> Issue (05): 426-430.doi: 10.3866/PKU.WHXB20000510

研究论文 上一篇    下一篇

51V NMR监测[VS4-Cun](n6)簇合物自兜反应过程

陈忠, 叶剑良, 蔡淑惠, 周兴旺, 万惠霖, 郑发鲲, 黄锦顺   

  1. 厦门大学化学系,物理系,固体表面物理化学国家重点实验室,厦门 361005|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:1999-08-09 修回日期:1999-11-03 发布日期:2000-05-15
  • 通讯作者: 陈忠 E-mail:chenz@jingxian.xmu.edu.cn

Probing Self-assembling Process of [VS4-Cun](n6) Clusters by 51V NMR

Chen Zhong, Ye Jian-Liang, Cai Shu-Hui, Zhou Xing-Wang, Wan Hui-Lin, Zheng Fa-Kun, Huang Jin-Shun   

  1. Department of Chemistry,Department of Physics,State Key Laboratory for Physical Chemistry of Solid Surface,Xiamen University,Xiamen 361005|Fujian Institute of Research on the Structure of Matter,the Chinese Academy of Sciences,State Key Laboratory of Structure Chemistry,Fuzhou 350002
  • Received:1999-08-09 Revised:1999-11-03 Published:2000-05-15
  • Contact: Chen Zhong E-mail:chenz@jingxian.xmu.edu.cn

摘要:

采用 51V NMR监测在核磁管内模拟 (NH4 ) 3VS4 /Et4NBr/CuBr/PPh3体系在CH2Cl2 中的反应过程 ,研究了反应条件如反应物不同配比对生成各种 [VS4-Cun](n≤ 6)簇合物的影响 ,提供了该反应体系在CH2Cl2 溶液中成簇过程的一些信息 .该方法不仅可用来研究反应机理 ,而且可用于指导一些条件难以确定 (溶剂、温度、酸碱度等 )的簇合物如低核数及更高核数V Cu S簇合物的合成.

关键词: 51V NMR, V-Cu-S簇合物, 自兜反应, 反应过程

Abstract:

51V NMR was used as a new pseudo in situ and nondestructive analytical tool to monitor and identify possible products of [VS4-Cun] (n≤6) clusters. The reaction of (NH 4) 3VS 4/Et 4NBr/CuBr/PPh 3 systems with various molar ratios in CH2Cl2 were mimicked in NMR tubes. The reaction conditions for the formation of the [VS 4-Cu n] clusters with different coordinate number of copper atoms n were studied. The results show the influence of the ratio among the reactants on the products and reveal the reaction mechanism in solution. This method not only provides some information about reaction mechanism, but also provides a guide in the synthesis of some clusters such as V-Cu-S clusters with less or more coordinate copper number whose reaction conditions (solvent, temperature, pH etc.) are difficult to be determined.

Key words: 51V NMR, V-Cu-S clusters, Self-assemble, Reaction process