Reaction of SiCl2·dipp with K[Ge9{Si(SiMe3)3}3] - Synthesis and Characterization of [K(dipp)2][Ge9{Si(SiMe3)3}3]·tol and [dipp-H][Ge9{Si(SiMe3)3}3]·2acn [dipp = 1,3-Bis(2,6-Di
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- 作者：Christina Fischer ; Wilhelm Klein ; Laura-Alice Jantke ; Lorenz J. Schiegerl and Thomas F. Fä ; ssler
- 刊名：Zeitschrift f蹲 anorganische und allgemeine Chemie
- 出版年：2016
- 出版时间：November 2016
- 年：2016
- 卷：642
- 期：22
- 页码：1314-1319
- 全文大小：544K
- ISSN：1521-3749
文摘
From solutions of K[Ge9{Si(SiMe3)3}3] with 1,3-bis(2,6-diisopropylphenyl-)imidazol-2-ylidene (dipp) two new compounds were obtained. From toluene, single crystals of [K(dipp)2][Ge9{Si(SiMe3)3}3]·tol (1) (tol = toluene) were isolated and the crystal structure was determined [monoclinic, P21/c, a = 16.8386(3), b = 24.6597(5), c = 30.2988(6) Å, β = 101.813(2)°, V = 12314.7(4) Å3, Z = 4, 24192 independent reflections, R1 = 0.046, wR2 = 0.084]. The investigation of single crystals from acetonitrile solution revealed the formation of [dipp-H][Ge9{Si(SiMe3)3}3]·2acn (2) (acn = acetonitrile) [orthorhombic, P212121, a = 13.4484(4), b = 25.8775(7), c = 26.4390(9) Å, V = 9201.1(5) Å3, Z = 4, 18065 independent reflections, R1 = 0.031, wR2 = 0.052]. The two [Ge9{Si(SiMe3)3}3]– entities show the minimal and maximal distortion of the central tricapped prism that have been reported to date. All compounds were characterized by ESI-MS, NMR and Raman spectroscopy, and DFT calculations.