高等学校化学学报 ›› 1997, Vol. 18 ›› Issue (8): 1246.

• 论文 • 上一篇    下一篇

Co3(CO)73-S)[μ,η2-SCNC (O)C (R1) (R2)N (COR3)]的合成和晶体结构

成庆民, 刘树堂, 胡襄, 刘启旺, 许莹   

  1. 内蒙古大学化学系, 呼和浩特 010021
  • 收稿日期:1996-06-20 出版日期:1997-08-24 发布日期:1997-08-24
  • 通讯作者: 刘树堂.
  • 作者简介:成庆民, 男, 26岁, 博士研究生.
  • 基金资助:

    国家自然科学基金;南京大学配位化学重点实验室资助

Synthesis and Crystalline Structure of Cluster Co3(CO)73-S)[μ,η2-SCNC (O)C (R1) (R2)N (COR3)]

CHENG Qing-Min, LIU Shu-Tang, HU Xiang, LIU Qi-Wang, XU Ying   

  1. Department of Chemistry, Inner Mongolia University Huhehaote 010021
  • Received:1996-06-20 Online:1997-08-24 Published:1997-08-24

摘要: Co2(CO8)分别与4种硫代乙内酰脲(这里有图片)<19970802-1246-1.gif>反应,得到4个新的含硫代乙内酰脲桥基双齿配位的三核钴羰基硫簇合物.用元素分析、IR、1HNMR和MS等手段表征了它们的结构,用X射线衍射测定了其中一个簇合物(这里有图片19970802-1246-2.gif)(IV)的晶体结构,晶体属三斜晶系,P1空间群,晶胞参数:a=0.8456(3)nm,b=1.1534(3)nm,c=1.1990(4)nm;a=107.36(3)°,β=108.44(5)°,γ=90.18(3)°;V=1.052(6)nm3,Z=2,F(000)=584,Dc=1.86g/cm3,μ=25.71cm-1,最终偏离因子R=0.046,Rw=0.058.

关键词: 钴羰基硫簇合物, 硫代乙内酰脲配体, 合成, 晶体结构

Abstract: Through the reaction of Co2(CO)8 with four thiohydantoins,(这里有图片19970802-1246-3.gif),four new sulfur-capped trinuclear cobalt carbonyl clusters (这里有图片19970802-1246-4.gif)[I: R1=R2=H;II: R1=H,R2=CH3, R3 =Ph; III: R1=R2=H, R3=CH3;IV: R1=R2=R3=CH3], were prepared and characterized by elementary analysis, IR, 1H NMRand MSspectroscopy. The crystal struc-ture of the cluster (这里有图片19970802-1246-5.gif)(IV ) was deter-mined by X-ray single crystal diffraction method.The crystal of the cluster is triclinic be-longing to space group P1 and the cell parameters are as follows:a=0.8456(3) nm,b=1.1534(3)nm, c=1.1990(4)nm;α=107.36(3)°, β=108.44 (5)°, γ=90.18(3)°;V=1.052(6)nm3,Z=2, F(00 0) =584, Dc=1.86g/cm3, μ=25.71cm-1,R=0.046,Rw=0.058. The molecule has revealed to have a pyrimidal Co3Sframework and contain a heterocyclic bridging bidentate ligand (这里有图片19970802-1246-6.gif)linked to the Co(1)and Co(2) atoms of the cluster by a cobalt-nitrogen and a cobalt-sulfur bond respectively.

Key words: Sulfo-trinuclear cobalt cluster, Thiohydantoino ligand, Synthesis, Crystal structure

中图分类号: 

TrendMD: