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三(三甲硅基)环戊二烯在一缩二乙二醇二甲醚或四氢呋喃中经n-BuLi处理后,随之与Mo(CO)_6加热,生成相应的环戊二烯基碳基钼负离子锂盐[η~5{(Me_3Si)_3C_5H_(5-n)}Mo~-(CO)_3]Li~+(n=2,3)(1),同时观察到有脱硅基现象发生.1与X(CH_2)_3X在一缩二乙二醇二甲醚中反应,无论X=I或Br,均生成标题化合物[η~5-(Me_3Si)_nC_5H_(5-n)]Mo(CO)_2(CH_2)_2CH_2[X=I:n=3(2),n=2(3);X=Br:n=3(4),n=2(5)].1与X(CH_2)_3X的反应如在THF中进行,则只有当X=I时才能生成环卡宾钼配合物.以元素分析,IR,~1H NMR和~(13)C NMR表征了2～5的结构,并用X射线衍射测定了4的晶体结构.晶体属单斜晶系,空间群为P2_1/n,晶胞参数a=1.2611(3),b=1.2434(2),c=1.7095(6)nm.β=91.07(2)°,V=2.680(2)nm~3, D_c=1.563g·cm~(-3),Z=4.最终偏差因子R=0.062,R_w=0.054.
Tris (trimethylsilyl) cyclopentadiene is treated with n-BuLi in diethylene glycol dimethyl ether or tetrahydrofuran, followed by heating with Mo (CO) 6 to give the corresponding cyclopentadienyl carbon group Molybdenum negative ion lithium salt [η ~ 5 {(Me_3Si) _3C_5H_ (5-n)} Mo ~ - (CO) _3] Li ~ + (n = 2,3) (1) .1 reacted with X (CH_2) _3X in diethylene glycol dimethyl ether to produce the title compound [η ~ 5- (Me_3Si) _nC_5H_ (5-n)] Mo ) 2 and X (CH_2) _2CH_2 [X = I: n = 3 (2), n = 2 (3); X = Br: n = 3 (4) and n = 2 (5) The reaction of 3X was carried out in THF, then cycloocarbene molybdenum complex could be formed only when X = I. The structure of 2 ~ 5 was characterized by elemental analysis, IR, ~ 1H NMR and ~ (13) C NMR and X The crystal structure of 4 was determined by X-ray diffraction. The crystal belongs to the monoclinic system with space group P2_1 / n. The cell parameters a = 1.2611 (3), b = 1.2434 (2), c = 1.7095 (6) 91.07 (2) °, V = 2.680 (2) nm ~ 3, D_c = 1.563g · cm ~ (-3) and Z = 4. The final deviation factor R = 0.062 and R_w = 0.054.