化学学报 ›› 1996, Vol. 54 ›› Issue (12): 1209-1213. 上一篇    下一篇

研究论文

(1,1,2,2-四甲基二硅桥连)双(四甲基环戊二烯基)四羰基二铁与碘的反应

徐善生;钟秀斌;周秀中   

  1. 南开大学;化学系元素有机化学国家重点实验室
  • 出版日期:1996-12-15 发布日期:1996-12-15

Reaction of (1,1,2,2-tetramethyl disilanylene) bis(tetramethyl- cyclopentadienyl)-tetracarbonyl di-iron with iodine

XU SHANSHENG;ZHONG XIUBIN;ZHOU XIUZHONG   

  • Online:1996-12-15 Published:1996-12-15

标题化合物(Me~2SiSiMe~2)[η^5-(C~5Me~4)Fe(CO)]~2(μ-CO)~2 (1)与碘在苯中反应, 生成碘插入Fe-Fe键的碘正离子桥连二铁化合物(Me~2SiSiMe~2)[η^5-(C~5Me~4)Fe(CO~2)]~2I~n^+·I~n^-(n=3, 3: n=5, 4)。如反应在氯仿中进行, 则只能分离到Fe-Fe键断裂的双铁碘化物(Me~2SiSiMe~2)[η^5-(C~5Me~4)Fe(CO)~2I]2, (2)。将4溶于Me~2SO/Me~2CO中, 则其分子内的I~5^-与Fe-I^+-Fe两部分相互作用, 也生成碘桥断裂的产物。以元素分析、IR、^1H NMR谱表征了2-4的分子结构, 并经X射线衍射测定了2的晶体及分子结构。

关键词: 晶体结构测定, 碘化物, 羰基化合物, 铁化合物, 碘, 环戊二烯基, 国家教委高等学校博士学科点专项科研基金

The reaction of the title compound (Me~2SiSiMe~2)[η^5-(C~5Me~4)Fe(CO)~2]~2(μ-CO)~2 (1) with iodine in benzene yielded the iodo-bridged complex (Me~2SiSiMe~2)[η^5-(C~5Me~4)Fe-(CO~2)]~2I^+·I~n^-(n=3, 3; n=5, 4). If the reaction was proceeded in chloroform, only the Fe-Fe bond cleaved iron iodide (Me~2SiSiMe~2)[η^5-(C~5Me~4)Fe(CO~2)~2I]~2 (2) was isolated. When 4 was dissolved in Me~2SO-Me~2CO, the two parts of I~5^- and Fe-I^+-Fe reacted each other to form the iodo-bridge cleaved product 2. The structures of 2-4 were characterized by elemental analysis, IR and ^1H NMR spectra. The crystal structure of 2 was determined by X-ray crystallography. The crystal is monoclinic, space group P 2~1/n, with a= 0.7656(2), b=1.6068(4), c=1.3030(6)nm; β=95.11(3)^0, V=1.597(2)nm^3, Z=2, D~c=1.735g·cm^-^3, μ=29.24cm^-^1, F(000)=820. The final deviation factor R is 0.037.

Key words: CRYSTAL STRUCTURE DETERMINATION, IODIDE, CARBONYL COMPOUNDS, IRON COMPOUNDS, IODINE, CYCLOPENTADIENYL GROUP

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