环状配合物Me_2Si［η~5－C_5H_4Fe（CO）_2］_2SnR_2的合

Syntheses and Structures of Cyclic Complexes Me_2Si[η￣5-C_5H_4Fe(CO)_2]_2SnR_2

通过ＳｎＣｌ_２对化合物Ｍｅ_２Ｓｉ［η~５－Ｃ_５Ｈ_４Ｆｅ（ＣＯ）］_２（μ－ＣＯ）_２（Ⅰ）中Ｆｅ－Ｆｅ键的插入反应以及Ⅰ被Ｎａ－Ｈｇ齐还原所生成的相应双铁负离子｛Ｍｅ_２Ｓｉ［η~５－Ｃ_５Ｈ_４Ｆｅ（ＣＯ）_２］_２｝^（２－）与ＳｎＲ_２Ｃｌ_２（Ｒ＝Ｍｅ，Ｐｈ）的亲核反应，合成了环状化合物Ｍｅ_２Ｓｉ［η~５－Ｃ_５Ｈ_４Ｆｅ（ＣＯ）_２］_２ＳｎＲ_２［Ｒ＝Ｃｌ（１），Ｍｅ（２），Ｐｈ（３）］。以元素分析、ＩＲ和~１ＨＮＭＲ谱表征了它们的结构，并用Ｘ射线衍射测定了配合物３的晶体结构。３为单斜晶系，空间群Ｐ２_１／ｎ，ａ＝１．０３８４（３）ｎｍ，ｂ＝１．６３８４（１）ｎｍ，ｃ＝１．５７６２（５）ｎｍ，β＝９７．９３（２）°，Ｖ＝２．６５６（２）ｎｍ~３，Ｚ＝４，Ｄｘ＝１．７１ｇ／ｍＬ。

The cyclic compounds of Me_2Si[η￣5-C_5H_4Fe(CO)_2]_2SnR_2[R=Cl(1),Me(2),Ph(3)] were synthesized via insertion of SnCl_2 to Fe-Fe bond of complex 1,Me_2Si[η￣5C_5H_4Fe(CO)]_2(μ-CO)_2 and the reactions of the related dianion{Me_2Si[η￣5-C_5H_4Fe(CO)_2]_2}￣(2-)with R_2SnCl_2(R=Me,PH).They were characterized by IR,￣1H NMR and elementary analysis. No expected product was isolated from the corresponding reactions of complex 2,(η￣5,η￣5C_5H_4SiMe_2OSiMe_2H_4)[Fe (CO)]_2(μ-CO)_2.The crystal structure of 3 was determined by X-ray diffraction. The crystals of 3 are monoclinic,space group P21/n with a=1. 0384(3)nm,b=1.6384(1) nm,c=1.5762(5) nm and β=97.93(2)°,V=2.656(2) nm￣3,Z=4,Dx =1.71g/mL.The final agreement factor,R=0.036.