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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Synthesis, crystal and molecular structure of a twelve-membered N,N'-dilithium-cyclosiloxazane [Me_2SiOSiMe_2N(Li)SiMe _2O]_2 [Darstellung, Kristall- und Molekülstruktur eines Zw?lfgliedrigen N,N'-DiLithium-cyclosiloxazans [Me_2SiOSiMe_2N(Li)SiMe _2O]_2]
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Synthesis, crystal and molecular structure of a twelve-membered N,N'-dilithium-cyclosiloxazane [Me_2SiOSiMe_2N(Li)SiMe _2O]_2 [Darstellung, Kristall- und Molekülstruktur eines Zw?lfgliedrigen N,N'-DiLithium-cyclosiloxazans [Me_2SiOSiMe_2N(Li)SiMe _2O]_2]

机译：十二元N，N'-二锂-环硅氧氮烷[Me_2SiOSiMe_2N（Li）SiMe _2O] _2 [Darstellung，Kristall- undMolekülstruktureines Zw？lfgliedrigen N，N'-二锂-环硅氧氮烷[Me_2SiOSiMe_2 Li）SiMe _2O] _2]

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摘要

The twelve membered and eighteen membered cyclosiloxazanes [Me _2SiOSiMe_2N(H)SiMe_2O]_2 (3) and [Me_2SiOSiMe_2N (H)SiMe_2O]_3 (4) have been obtained as colourless liquids from the reaction, of 1,5- Dichlorohexamethyltrisiloxane with ammonia at -50°C without any solvent. For compound 3 and 4, the yield is 30% and 43%, respectively. The treatment of 3 with two equivalents of n-butyllithium in n-hexane leads in almost quantitative yield (93 %) to the dilithiumsilylamide [Me_2SiOSiMe _2N(Li)SiMe_2O]_2 (5). Compound 5 can be isolated at room temperature and recrystallized from benzene without any decomposition or contraction of the ring size. An X-ray structure determination on [Me _2SiOSiMe_2N(Li)SiMe_2O]_2 (5) reveals a waved, crown-like twelve membered. Si_6N_2O _4-cycle. Each of the two lithium ions is coordinated by two nitrogen and two oxygen atoms leading to a square pyramid, in which the metal occupies the apex. The two square-pyramidal coordination figures are located above and below the waved crown-like Si_6N_2O_4-ring sharing a common edge by the atoms N(1) and N(2). All. synthesised compounds have been characterised by spectroscopic methods. Because of the lower solubility of the dilithiumsilylamide 5, only a ~1H-NMR could be applied for further characterisation in solution.
机译：从1,5-二氯六甲基三硅氧烷与氨水的反应中获得了无色液体，得到了十二元和十八元环硅氧氮杂[Me _2SiOSiMe_2N（H）SiMe_2O] _2（3）和[Me_2SiOSiMe_2N（H）SiMe_2O] _3（4）。 -50°C，无任何溶剂。对于化合物3和4，产率分别为30％和43％。在正己烷中用两当量的正丁基锂处理3几乎可以定量（93％）生成二锂硅酰胺[Me_2SiOSiMe_2N（Li）SiMe_2O] _2（5）。化合物5可以在室温下分离并从苯中重结晶而没有任何环尺寸的分解或收缩。通过对[Me _2SiOSiMe_2N（Li）SiMe_2O] _2（5）的X射线结构测定，发现波形的冠状十二元。 Si_6N_2O _4-周期。两个锂离子中的每个均由两个氮和两个氧原子配位，形成一个方形金字塔，其中金属占据顶点。两个方锥坐标图位于波浪状的冠状Si_6N_2O_4-环的上方和下方，该环由原子N（1）和N（2）共享公共边缘。所有。合成的化合物已通过光谱方法表征。由于二锂甲硅烷基酰胺5的溶解度较低，因此只能将〜1H-NMR用于溶液中的进一步表征。

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