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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 947-950 
    ISSN: 0009-2940
    Keywords: Heterosiloxanes ; Stibinosiloxanes ; Antimonites(III), silyl-, oxo- ; NMR, solid-state ; NMR; CPMAS ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of Sb(OSiMe3)3 with NaOSiMe3 in the molar ratio 1:2 in hexane at ambient temperature leads to the formation of Me3SiOSiMe3 and a crystalline complex of the formula Na4[Sb2O(OSiMe3)8] in ca. 35% yield. The composition of the product has been confirmed by elemental analysis and negative-ion CI mass spectrometry. The single crystal X-ray structure analysis (rhombohedral, space group R\documentclass{article}\pagestyle{empty}\begin{document}$\bar{3}$\end{document}c, Z=6) resulted in a disorder model for the complex with pseudo-cubic symmetry owing to virtually random distribution of sodium and antimony atoms over the vertices of an oxygen-centered octahedron with the eight silyloxy groups capping the faces. Low solubility in non-coordinating solvents prevented solution NMR studies, but solid-state NMR investigations using cross polarization and magic-angle spinning techniques (13C, 29Si) allowed the assignment of a point group C2v structure with the SbIII atoms in cis position relative to the oxo center of the complex.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Organoindium compound ; organothallium compound ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of Trimesitylthallium. A Comparison of the Trimesitylelement Compounds of Group 13The reaction of T1C13 with MesMgBr (Mes = 2,4,6-Me3C6H2) in THF at 0°C gives trimesitylthallium, TlMes3 (2). 2 has been characterized with NMR, IR and MS techniques as well as by an X-ray structure determination. 2 crystallizes isostructural to InMes3 (1a). The molecules of 2 are coordinated by the three mesityl substituents in a planar fashion. A new modification of InMes3 (1b) could be obtained by recrystallization of InMes3 from toluene/n-pentane in the space group C2/c. The literature known modification 1a and the new metallane 2 crystallize in the space group P21/n. The molecules in 1b possess C2-symmetry. The trimesitylelement compounds EMes3 (E = B, A1, Ga, In, T1) have been compared with each other.
    Notes: Die Reaktion von TlCl3 mit MesMgBr (Mes = 2,4,6-Me3C6H2) in THE bei 0°C liefert Trimesitylthallium, TlMes3 (2). 2 wurde mittels NMR- und IR-Spektroskopie bzw. Massenspektrometrie untersucht. Die Röntgenstrukturanalyse ergab ein isostrukturell zu InMes3 (1 a) kristallisierendes Molekül, dessen Tl-Zentrum planar von den drei Mesitylsubstituenten umgeben ist. Durch Kristallisation aus Toluol/n-Pentan konnte eine neue Modifikation des In-Mes3 (1 b) erhalten werden, die im Gegensatz zu 1 a und 2 (P21/n) in der Raumgruppe C2/c kristallisiert, wobei die Moleküle von 1 b C2-Symmetrie besitzen. Die Trimesitylelement-Verbindungen EMes3 (E = B, Al, Ga, In, Tl) werden miteinander verglichen.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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