Template synthesis, structure and spectra of the semiclathrochelate and clathrochelate 1,4-pentadienylboron-capped iron(II) oximehydrazonates

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• 作者：Yan Z. Voloshin ; Irina G. Makarenko ; Sergey Y. Erdyakov ; Semen V. Svidlov ; Anna V. Vologzhanina ; Ekaterina G. Lebed ; Anatolii V. Ignatenko ; Mikhail E. Gurskii ; Yurii N. Bubnov
• 关键词：Macrocycle ; Clathrochelate ; Iron(II) ; Allylboration ; Organoboranes ; X-ray crystallography
• 刊名：Inorganica Chimica Acta
• 出版年：2010
• 出版时间：15 January 2010
• 年：2010
• 卷：363
• 期：2
• 页码：395-403
• 全文大小：967 K

文摘

The direct template condensation of diacetylmonooxime hydrazone with the 1,4-pentadienylboronates as Lewis acids on an iron(II) ion matrix led to the 1,4-pentadienylboron-capped semiclathrochelate iron(II) oximehydrazonates. The H⁺-ion-catalyzed macrocyclization of these precursors with an excess of triethyl orthoformate resulted in macrobicyclic complexes with a single apical 1,4-pentadienyl substituent. The complexes obtained were characterized using elemental analysis, MALDI-TOF mass spectrometry, IR, UV–Vis, ¹H, ¹¹B{¹H} and ¹³C{¹H} NMR, ⁵⁷Fe Mössbauer spectroscopies, and X-ray crystallography. The X-ray diffraction and NMR data for complexes obtained showed the syn,syn,syn-orientation of all ethoxy substituents in 1,3,5-triazacyclohexane capping fragment in relation to a clathrochelate framework.