双(η~5-环戊二烯基三羰基铬)汞的新合成方法及其单晶、分子结构

A New Synthetic method of Bis(η5-Cyclopentadienylchromium Tricarbonyl) Mercury and Its Single Crystal Molecular Structure

n^5-环戊二烯基三羰基铬钠与甲基氯化汞在二缩乙二醇二甲醚中室温反应12h,得产率为58％的双(n^5-环戊二烯基三羰基铬)汞.经碳氢分析、IR、~1H NMR、MS及单晶X光衍射技术证实.晶体属空间群P2_1/c..晶胞参数:α=8.023(2),6=20.843(9),c=10.331(2);β=96.00(3)°; Z=4.Cr—Hg平均键长为2.655.汞与2个铬原子近于共线.每个铬原子可看作是处于以环戊二烯基为底的五角锥和以3个羰基、1个汞原子为底的四角锥的公共顶点上。

Reaction of η5- cyclopentadienylchromium tricarbonyl sodium with methylmercuric chloride in diglyme at room temperature for 12 h gave bis(η5-cyclopentadienylchromium tricarbonyl) mercury [η5-C5H5Cr(CO)3]2Hg in 58% yield. Its structure was fully confirmed by combustion analysis, IR, 1H NMR, MS and X-ray diffraction methods. The crystal belongs to monoclinic space group P21/c. Cell parameters are a = 8. 023 (2) A, b=20. 843(9) A , c=10. 331 (2) A ; β=96. 00(3)°, V = 1718. 2 A3; Z=4. The average Cr-Hg bond length is 2. 655A. Mercury atom is approximately co-linear with two chromium atoms (△Cr(1)HgCr(2) = 171. 12°). Each chromium atom can be viewed as being on the common apex of the pentagonal pyramid constructed from cyclopentadienyl pentagon bottom and the square-based pyramid with the bottom of three carbonyls and one mercury atom.