[1]Ferrocenophanes, [1]Chromarenophanes, and [1]Vanadarenophanes with Aluminium and Gallium in Bridging Positions

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• 作者：Clinton L. Lund ; Jö ; rg A. Schachner ; J. Wilson Quail ; Jens M&uuml ; ller
• 刊名：Organometallics
• 出版年：2006
• 出版时间：November 20, 2006
• 年：2006
• 卷：25
• 期：24
• 页码：5817 - 5823
• 全文大小：127K
• 年卷期：v.25,no.24(November 20, 2006)
• ISSN：1520-6041

文摘

Aluminum- and gallium-bridged [1]ferrocenophanes (4a, 4b), [1]chromarenophanes (5a, 5b), and[1]vanadarenophanes (6a, 6b) were synthesized from the respective dilithiated sandwich compounds withelement dichlorides (Me₂Ntsi)ECl₂ [E = Al, Ga; Me₂Ntsi = C(SiMe₃)₂(SiMe₂NMe₂)] in moderate tohigh isolated yields (54-97%). The new intramolecularly stabilized aluminum compound (Me₂NCH₂tsi)AlCl₂ (2a) was synthesized, but was proven to be unreactive with respect to [Fe(LiC₅H₄)₂]·2/3TMEDA.The diamagnetic species 2a, 4a, 4b, 5a, and 5b were characterized by NMR spectroscopy (¹H, ¹³C,²⁷Al), CHN elemental analysis, and mass spectrometry, whereas the paramagnetic compounds 6a and 6bwere characterized by IR spectroscopy, CHN elemental analysis, and mass spectrometry. In addition, themolecular structures of compounds 2a, 4a, 4b, 5a, 5b, 6a, and 6b were determined by single-crystalX-ray analysis. All [1]cyclophanes are strained species, as revealed by the following tilt angles hars/alpha.gif" BORDER=0> [deg]:14.33(14) (4a), 15.83(19) (4b), 11.81(9) (5a), 13.24(13) (5b), 14.65(14) (6a), and 15.63(14) (6b).