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首页> 外文期刊>Chemistry: A European journal >On the Reactivity of Silylated Ge-9 Clusters: Synthesis and Characterization of [ZnCp*(Ge-9{Si(SiMe3)(3)}(3))], [CuPiPr(3)(Ge-9{Si(SiMe3)(3)}(3))], and [(CuPiPr(3))(4){Ge-9(SiPh3)(2)}(2)]
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On the Reactivity of Silylated Ge-9 Clusters: Synthesis and Characterization of [ZnCp*(Ge-9{Si(SiMe3)(3)}(3))], [CuPiPr(3)(Ge-9{Si(SiMe3)(3)}(3))], and [(CuPiPr(3))(4){Ge-9(SiPh3)(2)}(2)]

机译：关于硅烷化的Ge-9团簇的反应性：[ZnCp *（Ge-9 {Si（SiMe3）（3）}（3））]，[CuPiPr（3）（Ge-9 {Si（SiMe3））的合成和表征（3）}（3））]和[（CuPiPr（3））（4）{Ge-9（SiPh3）（2）}（2）]和

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We report on the synthesis of new derivatives of silylated clusters of the type [Ge-9(SiR3)(3)](-) (R = SiMe3, Me = CH3; R = Ph, Ph = C6H5) as well as on their reactivity towards copper and zinc compounds. The silylated cluster compounds were synthesized by heterogeneous reactions starting from the Zintl phase K4Ge9. Reaction of K[Ge-9{Si(SiMe3)(3)}(3)] with ZnCl2 leads to the already known dimeric compound [Zn(Ge-9{Si(SiMe3)(3)}(3))(2)] (1), whereas upon the reaction with [ZnCp*(2)] the coordination of [ZnCp*](+) to the cluster takes place (Cp*= 1,2,3,4,5-pentamethylcyclopentadienyl) under the formation of [ZnCp*(Ge-9{Si(SiMe3)(3)}(3))] (2). A similar reaction leads to [CuPiPr(3)(Ge-9{Si(SiMe3)(3)}(3))] (3) from [CuPiPr3Cl] (iPr= isopropyl). Further we investigated the novel silylated cluster units [Ge-9(SiPh3)(3)](-) (4) and [Ge-9(SiPh3)(2)](-) (5), which could be identified by mass spectroscopy. Bis-and tris-silylated species can be synthesized by the respective stoichiometric reactions, and the products were characterized by ESI-MS and NMR experiments. These clusters show rather different reactivity. The reaction of the tris-silylated anion 4 with [CuPiPr(3)Cl] leads to [(CuPiPr(3)) 3Ge(9)(SiPh3)(2)](+) as shown from NMR experiments and to [(CuPiPr(3))(4){Ge-9(SiPh3)(2)}(2)] (6), which was characterized by single-crystal X-ray diffraction. Compound 6 shows a new type of coordination of the Cu atoms to the silylated Zintl clusters.
机译：我们报告了[Ge-9（SiR3）（3）]（-）（R = SiMe3，Me = CH3; R = Ph，Ph = C6H5）类型的甲硅烷基化簇的新衍生物的合成对铜和锌化合物有反应性。甲硅烷基化的簇状化合物是通过从Zintl相K4Ge9开始的异构反应合成的。 K [Ge-9 {Si（SiMe3）（3）}（3）]与ZnCl2的反应生成已知的二聚化合物[Zn（Ge-9 {Si（SiMe3）（3）}（3））（2 ）]（1），而在与[ZnCp *（2）]反应时，[ZnCp *]（+）与簇的配位发生（Cp * = 1,2,3,4,5-五甲基环戊二烯基） [ZnCp *（Ge-9 {Si（SiMe3）（3）}（3））]（2）的形成。类似的反应由[CuPiPr3Cl]（iPr =异丙基）生成[CuPiPr（3）（Ge-9 {Si（SiMe3）（3）}（3））]（3）。此外，我们研究了新型的甲硅烷基化簇单元[Ge-9（SiPh3）（3）]（-）（4）和[Ge-9（SiPh3）（2）]（-）（5），它们可以通过质量鉴定光谱学。可以通过各自的化学计量反应合成双-和三-甲硅烷基化的物种，并通过ESI-MS和NMR实验对产物进行表征。这些簇显示出相当不同的反应性。如NMR实验所示，三甲硅烷基化阴离子4与[CuPiPr（3）Cl]的反应生成[[CuPiPr（3））3Ge（9）（SiPh3）（2）]（+），并生成[[CuPiPr （3））（4）{Ge-9（SiPh3）（2）}（2）]（6），其特征在于单晶X射线衍射。化合物6显示了新型的Cu原子与甲硅烷基化的Zintl团簇的配位。

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