二(1-环戊烯基环戊二烯基)四羰基二钌(Ⅰ)的合成与晶体结构

Synthesis and Crystal Structure of Di(1-cyclopentenylcyclopentadienyl) Tetracarbonyl Diruthenium(Ⅰ)

由6,6-四亚甲基富烯与Ru3(CO)12在二甲苯中加热回流,合成了一个新的双核配合物(η5-C10H11)2Ru2(CO)2(μ-CO)2。通过元素分析、红外光谱、核磁共振氢谱对其结构进行了表征,用X射线单晶衍射法测定了配合物的结构,结果表明:晶体属于三斜晶系,P空间群,a=0.641 57(19)nm,b=0.761 3(2)nm,c=1.192 4(3)nm,α=89.973(4)°,β=87.143(4)°,γ=69.666(4)°,V=0.545 3(3)nm3,Dc=1.756 g·cm-3,μ=1.412 mm-1,F(000)=286,Z=1,R1=0.024 0,wR2=0.066 7。晶体结构表明6,6-四亚甲基富烯在反应过程中发生了双键的异构。

6,6-Tetramethylenefulvene reacted with Ru3（CO）12 in refluxing xylene to give the new dinuclear complex（η5-C10H11）2Ru2（CO）2（μ-CO）2.Its molecular structure was characterized by elemental analysis,IR,1H NMR.X-ray crystallography of the compound reveals that it belongs to triclinic system P1 space group,with a=0.641 57（19） nm,b=0.761 3（2） nm,c=1.192 4（3） nm,α=89.973（4）°,β=87.143（4）°,γ=69.666（4）°,V=0.545 3（3） nm3,Dc=1.756 g·cm-3,μ=1.412 mm-1,F（000）=286,Z=1,R1=0.024 0,wR2=0.066 7.Its crystal structure shows that the 6,6-tetramethylenefulvene undergoes double-bond isomerization in the reaction.