One-Step Preparation of Dimethyl Sulfide Substituted Icosahedral Boranes: The Crystal and Molecular Structures of 1,7-(SMe2)2B12H10, 1,12-(SMe2)<

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• 作者：Ewan J. M. Hamilton ; Glenn T. Jordan IV ; Edward A. Meyers ; and Sheldon G. Shore
• 刊名：Inorganic Chemistry
• 出版年：1996
• 出版时间：August 28, 1996
• 年：1996
• 卷：35
• 期：18
• 页码：5335 - 5341
• 全文大小：335K
• 年卷期：v.35,no.18(August 28, 1996)
• ISSN：1520-510X

文摘

1,7-(SMe₂)₂B₁₂H₁₀,1,12-(SMe₂)₂B₁₂H₁₀,and[SMe₃][B₁₂H₁₁(SMe₂)]were prepared and isolated from the self-condensation reaction of BH₃·SMe₂ in theabsence of a solvent. At 150 G SRC="/images/entities/deg.gif">C the reaction yields, primarily,twoisomers:1,7-(SMe₂)₂B₁₂H₁₀, themajor component, and1,12-(SMe₂)₂B₁₂H₁₀the minor component, that are separatedby thin layer chromatography. Single-crystal X-ray structuredeterminations were performed for both isomers,confirming the structures inferred from ¹H,¹¹B, and¹¹B{¹H}-¹¹B{¹H}(COSY) NMR spectra. Crystal data for1,7-(SMe₂)₂B₁₂H₁₀:trigonal P3₂21, a =12.901(10) &Aring;, b = 12.901(10) &Aring;, c= 23.73(2) &Aring;, ges/gifchars/gamma.gif" BORDER=0 > = 120ges/entities/deg.gif">, Z = 9.Crystal data for1,12-(SMe₂)₂B₁₂H₁₀:orthorhombic Pbca, a = 10.101(2) &Aring;,b = 11.220(2) &Aring;, c = 13.464(2)&Aring;,Z = 4. At 60 ges/entities/deg.gif">C, the self-condensation ofBH₃·SMe₂ is very slow, but yields[SMe₃][B₁₂H₁₁(SMe₂)]as themajor product. Multinuclear and 2-dimensional NMR spectra are infull accord with the structure determined byX-ray methods. Crystal data for[SMe₃][B₁₂H₁₁(SMe₂)]·MeCN:monoclinic P2₁, a = 8.904(10)&Aring;, b = 9.08(2)&Aring;, c = 12.39(3)&Aring;, ges/gifchars/beta2.gif" BORDER=0 ALIGN="middle"> = 93.82ges/entities/deg.gif">, Z= 2.