Synthesis and Characterization of Alkali Metal Hypersilyl Borates

Thomas Lainer, Christoph Walkner, Nina M. Tasch, Roland C. Fischer, Ana Torvisco, Harald Stueger, Michael Haas
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Abstract

This study focuses on the synthesis of H‐ and MeO‐ functionalized alkali metal hypersilyl borates. Consequently, two distinct silanides were used as polysilane frameworks for our chemical manipulations. Tris(silyl)silanide (1) and tris(trimethoxysilyl)silanide (2) react in the same manner with the BH3 ⋅ SMe2 complex to obtain two new alkali metal hypersilyl borates [(R3Si)3SiBH3M (M=alkali metal; R=H, (3), R=MeO, (4 a–c))] in good to excellent yields. NMR spectroscopy for all compounds and single‐crystal X‐ray crystallography for 3 and 4 a, b enabled a clear structural characterization. Single crystal X‐ray analysis of 3 showed a dimeric structure, where two THF‐molecules and three hydrides from the BH3‐group contribute to the coordination sphere of the lithium atom. Interestingly, crystals suitable for X‐ray analysis of 4 a and 4 b showed a solvent‐free cluster formation, due to the coordination of the MeO groups. Both species form coordination polymers with different coordination modes depending on the nature of the alkali metal. Attempted hydride abstraction reactions of 3 and 4 with various reagents under the formation of the free boranes proceeded unselectively.
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碱金属超硅硼酸盐的合成与表征
本研究的重点是合成 H 原子和 Me 原子官能化的碱金属超硅硼酸盐。因此,我们使用了两种不同的硅烷作为多硅烷框架进行化学处理。三(硅烷基)硅烷化物 (1) 和三(三甲氧基硅烷基)硅烷化物 (2) 与 BH3 ⋅ SMe2 复合物以相同的方式发生反应,得到两种新的碱金属超硅硼酸盐 [(R3Si)3SiBH3M(M=碱金属;R=H,(3),R=MeO,(4 a-c))],收率良好至极佳。通过对所有化合物进行核磁共振光谱分析,以及对 3 和 4 a、b 进行单晶 X 射线晶体分析,可以清楚地确定其结构特征。3 的单晶 X 射线分析表明其具有二聚体结构,其中两个 THF 分子和三个来自 BH3 基团的氢化物构成了锂原子的配位层。有趣的是,适合对 4 a 和 4 b 进行 X 射线分析的晶体显示,由于 MeO 基团的配位,形成了无溶剂簇。根据碱金属的性质,这两种物质形成的配位聚合物具有不同的配位模式。在形成游离硼烷的条件下,尝试用各种试剂对 3 和 4 进行氢化物抽取反应,但反应无选择性地进行。
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