双(三甲硅基环戊二烯基羰基钼)配合物的合成和结构  

Synthesis and Structures of Bis(trimethylsilylcyclopentadienyl Carbonyl Molybdenum) Complexes

作　　者：邝代治 周秀中[2] 

机构地区：[1]衡阳师范专科学校化学系,衡阳421008 [2]南开大学化学系,天津300071

出　　处：《化学学报》1995年第3期243-247,共5页Acta Chimica Sinica

基　　金：南开大学元素有机化学所国家重点实验室资助的课题

摘　　要：通过三羰基(三甲硅基环戊二烯基)钼负离子盐[η-Me_3SiC_5H_4Mo(CO)_3]^-Li^-氧化偶联合成了Mo—Mo键双核化合物(1),在甲苯中回流制得含Mo≡Mo叁键化合物(2),乙炔对这Mo≡Mo键加成形成四面体形配合物(3),经元素分析,IR和~1H NMR 谱表征了标题化合物的结构,并用X射线衍射测定了配合物[η-Me_3SiC_5H_4Mo(CO)_3]_2(1)的晶体结构,1为单斜晶系,空间群为P2_1/C,晶体学数据:α=1.2826(2),b=0.8211(5),c=1.2902(1)nm,β=104.80(2)°,V=1.3138nm^3,Z=2,D_x=1.604g·Cm^(-3),μ=10.530cm^(-1),F(000)=636. 硅桥联双[三羰基(三甲硅基环戊二烯基)钼]负离子盐E[η-Me_3SiC_5H_3Mo(CO)_3]_2^(2-)Li_2^+,[E=SiMe_2,O(SiMe_2)_2]],也用类似方法合成化合物 4,5,也经元素分析,IR,~1H NMR表征.The Mo-Mo bond dinuclear compounds were synthesized via oxidative coupling tricarbonyl trimethyl silylcyclopentadienyl molybdenum anion salt and silylene-bridged bis (tricarbonyl trimethyl silylcyclopentadienyl molybdenum anion salt) E[η-Me3SiC5H3Mo(CO)3]22-Li2+, [E = SiMe2, O(SiMe2)2], respectively. Compound of containing molybdenum-molybdenum triple bond was also prepared by heating under reflux 1 in toluene. Acetylene add to the Mo ≡ Mo triple bond to give tetrahedron complex, structures of the title compounds were characterized by elemental analyses, IR and 1H NMR spectra, furthermore, the crystal structures of complex [η-Me3SiC5H4Mo(CO)3]2. 1 was determined by X-ray diffraction. The crystals of 1 are monoclinic, space group P21/ c, with a = 1.2826(2), b = 0.8211(5), c = 1.2902(1) nm, β=104.80(2)°, V = 1.3138nm3, Z = 2, Dx = 1.604g·cm-3,μ= 10.530cm-1, F(000) =636.

关 键 词：三甲硅基 环戊二烯 钼 氧化偶联 结构 配合物 

分 类 号：O627.63[理学—有机化学]