环戊烯配位的羰基钌簇合物Ru_3(CO)_9(C_5H_6)的合成及晶体结构

Synthesis and Crystal Structure of Substituted Decacarbonyltriruthenium by Cyclopentene Cluster Ru_3(CO)_9(C_5H_6)

本文合成了以环戊烯配位的羰基钌簇合物Ru_3(CO)_9(C_5H_6),用IR,~1H NMR,^(13)C NMR和元素分析等方法对此簇合物进行了结构表征,配体环戊烯的双键被打开并且分别配位于金属钌原子所组成的平面上和下,X射线进一步肯定了以上结论,簇合物为单斜晶系,空间群为P2_1/a,α=1.6498(8),b=1.3221(5),c=1.7330(6)nm,β=91.54(3)°,V=3.779(3)nm^3,Z=8,μ=23.5cm^(-1),D_c=2.18g/cm^3,F(000)=2352,最终偏差因子R=0.0754,R_w=0.0710.

Thermolysis of Ru3(CO)12 and cyclopentene in octane followed by TLC has given the title cluster compounds,which have been charaterized by IR, 1H NMR,13C NMR and elementary analysis. An X- ray diffraction of the product has unequivocally established its structure. The cluster crystallizes in monoclinic space group P21 /a , a = 1.6498 ( 8 ), b = 1. 3221 ( 5 ), c = 1. 7330(6)nm,β=91.54(3)°,V = 3779(3)nm3, Z = 8,u = 23.5cm-1,Dc = 2.18g/cm3,F(000)=2352and R = 0.0754,Rw = 0.0710 based on 3199 independent reflections with I≥3.5σ(I).