(四甲基二硅撑)二(3-三甲硅基环戊二烯基)四羰基二铁及其相关化合物的合成及结构

1,2-二(三甲硅基环戊二烯基)四甲基二硅烷与Fe(CO)5在二甲苯中于105～110℃反应除分离到少量标题化合物(Me2SiSiMe2)η-(3-Me3SiC5H3Fe(CO)]2(μ-CO)2(5)外,主要是生成了脱Me3Si基的产物(Me2SiSiMe2)η-C5H4Fe(CO)]2(μ-CO)2(1)及1的热重排异构体Me2SiC5H4-Fe(CO)2]2(2).将5的二甲苯溶液加热回流18h,则转化为其异构体Me2Si(Me3SiC5H3)Fe(CO)2]2(6).脱硅基发生在由相应反应物制备5的过程中。且脱硅基是与反应物中(Me2SiSiMe2)桥的存在有关。5的晶体结构经X射线衍射测定属单斜晶系,P21/m空间群,晶体学数据:a=0.6780(1)nm,b=2.2303(9)nm,c=0.9988(1)nn,;β=98.96(1)°,V=1.4960nm3.Z=2,Dc=1.36g/cm3.

Synthesis and Structure of Tetramethyldisilandiyl Bis(3-trimethylsilylcyclopentadienyl)Tetracarbonyl Di-Iron and Its Related Compounds

Asmall amount of the title compound 5(5%)and a desilylated complex(Me2SiSiMe2)C5H4Fe(CO)]2(μ-CO)2(1)(3%)and its rearrangement isomerMe2SiC5H4Fe(CO)2]2(2)(16%) were obtained from the reaction of 1, 2-bis(3-trimethylsilylcyclopentadienyl)tetramethyldisilane with Fe (CO)5 at 105110℃.When a xylene solution of 5 was refluxed for 18h, compound Me2Si(3-Me3Si-C5H3)Fe(CO)2]2(6), as a rearrangement isomer of 5 was obtained in58% yield.It was proved that desilylation of Me3Sioccured in the process of preparing5 and desilylation is related to the(Me2SiSiMe2)-bridge of the reactant.The crystal structure of 5 was determined by X-ray diffraction, The crystal is monoclinic, space group P21/m with a=0.6780(1)nm, b=2.2303(9)nm, c=0.9988(1)nm, β=98.96(1)°, V=1.496 nm3, 2=2, Dc=1.36 g/cm3.The final deviation factor Ris0.044.