高等学校化学学报

高等学校化学学报 ›› 2001, Vol. 22 ›› Issue (S1): 85.

• 研究论文 • 上一篇    下一篇

不对称取代双(吡唑)甲烷VIB羰基金属化合物的合成及表征

王志宏, 杨智, 唐良富, 柴建方, 王积涛   

  1. 南开大学化学系, 天津 300071
  • 收稿日期:2001-07-17 出版日期:2001-12-31 发布日期:2001-12-31
  • 通讯作者: 唐良富(1970年出生),男,博士,副教授,从事金属有机化学研究.电话:022-23504446.e-mail:tanglf@eyou.com E-mail:tanglf@eyou.com
  • 基金资助:

    国家自然科学基金(批准号:29902002)及高等学校博士学科点专项科研基金资助课题.

Synthesis of Group 6 Metal Carbonyl Complexes Containing Asymmetric Substituted (3-phenylpyrazol-1-yl-5'-phenylpyrazol-1-yl) methane

WANG Zhi-Hong, YANG Zhi, TANG Liang-Fu, CHAI Jian-Fang, WANG Ji-Tao   

  1. Department of Chemistry, Nankai University, Tianjin 300071, China
  • Received:2001-07-17 Online:2001-12-31 Published:2001-12-31
  • Contact: tanglf@eyou.com E-mail:tanglf@eyou.com

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摘要：

3-苯基吡唑与二溴甲烷在相转移催化下反应,得到(3-苯基吡唑-5'-苯基吡唑)甲烷(1)和双(3-苯基吡唑)甲烷(2)的混合物.当该混合配体与M(CO)6(M=Cr,Mo,W)在光照下反应时,分离得到了不对称取代的(3-苯基吡唑-5'-苯基吡唑)甲烷四羰基铬(3),钼⑷和钨(5).用X-射线衍射测定了化合物5的晶体结构.结果表明,该晶体属于单斜晶系,P2(1)/n空间群,a=1.7976(7) rnn,b=1.3210(5) nm, c=1.8681(7) nm;β=98.293(8)°, V=4.390(3) nm3, Z=8,最终结构偏离因子[I>2σ(I)]=0.0516, Rw=0.0898, GOF=0.879.两个苯基分别处于两个吡唑的3位及5'位.

关键词: 多吡唑烷, VIB羰基化合物, 晶体结构

Abstract:

The reaction of 3(5)-phenylpyrazole with CH2Br2 under phase transfer catalysis yields (3-phenyl pyrazol-1-y1-5'-phenylpyrazo-1-yl)methane, CH2(3-PhPz-5'-PhPz) and bis(3-phenylpyrazo-1-yl)methane. Upon treating the isomeric mixture with M(CO)6 (M=Cr, Mo and W) under UV irradiation at room temperature, (3-phenylpyrazol-1-yl-5'-phenylpyrazo-1-yl)methane tetracarbonylchromium, molybdenum or tungsten complexes is isolated, respectively.The molecular structure of CH2(3-PhPz-5'-PhPz)W(CO)4 is determined by X-ray crystallography, which clearly shows that phenyl groups lie in the 3 and 51-positions of pyrazole rings. The compound crystallizes in the monotriclinic space group P2(1)/n, with a=1.7976(7) nm, b=1.3210(5) nm,c=1.8681(7) nm, β=98.293(8)°, V=4.390(3) nm3, Z=8, R=0.0516, Rw=0.0898.

Key words: Poly(pyrazo-1-yl)alkane, Group 6 metal carbonyl complex, X-ray structure

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