1,1'-(四甲基二硅撑)双[环戊二烯基三羰基钼配合物]的合成及结构

1,2-二环戊二烯基四甲基二硅烷与正丁基锂作用生成(四甲基二硅撑)双[环戊二烯基负离子盐],后者随即与六羰基钼反应即形成1,1'-(四 甲基二硅撑)双[环戊二烯基三羰基钼负离子盐],分别与四种不同的卤化物反应,生成在钼原子上发生烃基化的产物与冰醋酸作用,随即分别与CCl~4及NBS反应,生成相应的钼氯化物和钼溴化物作用发生氧化偶联反应,生成Mo-Mo键断裂的钼碘化物,以元素分析、IR及^1HNMR表征了2-9的结构.并对5的单晶进行了X射线衍射分析.它的晶体属三斜晶系,PI空间群,晶体学数据:偏差因子R=0.043,R~W=0.055.

Synthesis and structure of 1,1-(tetramethyl disilandiyl)-bis (cyclopentadienyltricarbonyl molybdenum complex)

1,1'-(tetra-Me disilanediyl)-bis(cyclopentadienyllithium). Then the later reacted with hexacarbonylmolybdenym to generate the title compd, (Me2SiSiMe2)[CpMo(CO)3-Li+]2 (I). I reacted with four alkyl halides resp. to yield the alkylation products on Mo-atom, (Me2SiSiMe2) [CpMo(CO)3R]2(R = CH3, C2H5, PhCH2, CH2COOO2H5 (II)]. I was treated with HOAc and then reacted with CCl4 and NBS resp. to yield the corresponding molybdenum chloride and bromie. Oxidative coupling reaction was happened when the solution of I was treated with Fe2(SO4)3/H3+O and the dinuclear Mo-Mo complex (Me2SiSiMe2)[CpMo(CO)3]2 (III) was formed. III reacted with iodine in chloroform to produce the Mo-Mo bond cleaved product, (MeSiSiMe2)[CpMo(CO)3I]2. The crystal and mol. structure of II were determine by x-ray diffraction method.