【作者】 王一兵； 韩利民； 索全伶； 冶杰慧； 竺宁；

【Author】 Wang Yi-bing Han Li-min Suo Quan-ling Ye Jie-hui Zhu Ning(Chemical Engineering College, Inner Mongolia Polytechnic University, Hohhot 010062)

【机构】 内蒙古工业大学化工学院；

【摘要】 通过双炔配体Fc-C≡C-C≡C-Fc与簇合物Co2(CO)8在室温下反应,合成了两个具有μ2-η2-配位键的簇合物(Fc-C≡C-C≡C-Fc)[Co2(CO)6]n[Fc=C5H5FeC5H4,n=1(1),2(2)],并利用元素分析,IR,NMR,MS和X-ray单晶衍射的方法对配合物的组成和结构进行了表征。簇合物1的晶体属于正交晶系,空间群为P2(1)2(1)2(1)。晶胞参数:a=1.0644(3),b=1.1528(3),c=2.2328(6))nm,α=90°,β=90°,γ=90°,V=2.7397(14)nm3,Z=4,Dc=1.707g.cm-3,S=1.037,△ρmax=333 e.nm-3,△ρmax=-458 e.nm-3。最终偏离因子[I>2σ(I)]:R=0.0399,wR=0.0797,偏离因子(all data)R=0.0581,wR=0.0857,w=1/[σ2(Fo2)+(0.0408P)2+0.0000P],其中P=(Fo2+2Fc2)/3。簇合物2的晶体属于三斜晶系,空间群为PT。晶胞参数:a=0.90501(7),b=0.93096(8),c=1.18334(10)nm,α=81.821(2)°,β=88.098(2)°,γ=65.1440(10)°,V=0.89505(13)nm3,Z=1,Dc=1.837g.cm-3,S=1.004,△ρmax=1024 e.nm-3,△ρmin=-909e.nm-2。最终偏离因子[I>2σ(I)]:R=0.0491,wR=0.1279,偏离因子(all data)R=0.0528,wR=0.1308,w=1/[σ2(Fo2)+(0.0908P)2+0.0000P],其中P=-(Fo2+2Fc2)/3。更多还原

【Abstract】 The reaction of ferrocenylacetylide compounds with Co2(CO)8 in room temperature affords two complexes (Fc-C≡C-C≡C-Fc)[Co2(CO)6]n [Fc=C5H5FeC5H4, n=1(1), 2(2)] bearing ferrocenyl units with approximately tetrahedral (μ-alkyne)dicobalt moieties . The compounds were characterized by element analysis, IR, 1H(13C)NMR, MS and single-crystal X-ray diffraction analysis. The cluster I crystallizes in Orthorhombic, space group P2(1) 2(1) 2(1) with a=1.0644(3), b=1.1528(3), c=2.2328(6))nm, α=90°,β=90°,γ=90°, V= 2.7397(14) nm3, Z=4, Dc= 1 .707g.cm-3, S=1.037,Δρmax=333e.nm-3,Δρmin=-458 e.nm-3, final Rindices[I>2σ(Ⅰ)]: K= 0.0399, wR = 0.0797 , Rindices(all data) R= 0.0581, wR= 0.0857 ,w=1/[σ2(Fo2)+ (0.0408P)2+0.0000P],where P=(Fo2+2Fc2)/3. The cluster 2 crystallizes in Triclinic, space group P1 with a = 0.90501(7), b = 0.93096(8), c =1.18334 (10) nm,α= 81.821 (2)°,β= 88.098 (2)°,γ= 65.1440(10)°,V=0.89505(13)nm3,Z=1,Dc=1.837g.cm-3, S= 1.004,Δρmax=1024e.nm-3,Δρmin= -909e.nm-3. final R indices[I>2σ(Ⅰ)]: R=0.0491, wR = 0.1279, R indices(all data) R= 0.0528, wR= 0.1308,x1/[σ2(Fo2)+ (0.0908P)2+0.0000P], where P=(Fo2+2Fc2)/3.更多还原