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The first ribbed functionalized tris-dioximate clathrochelates with inherent hydroxyl substituents: Synthesis, spectra and X-ray structure
Authors:Aleksei B Burdukov  Mikhail A Vershinin  Ilya V Eltsov  Nataliya V Pervukhina  Yan Z Voloshin  
Affiliation:aNikolaev Institute of Inorganic Chemistry, Siberian Branch of the Russian Academy of Sciences, 630090 Novosibirsk, Russia;bNovosibirsk State University, 630090 Novosibirsk, Russia;cNesmeyanov Institute of Organoelement Compounds of the Russian Academy of Sciences, 119991 Moscow, Russia
Abstract:The controlled hydrolysis of the dichlorine-containing iron(II) clathrochelate FeBd2(Cl2Gm)(BF)2 precursor (where Bd2− and Cl2Gm2− are α-benzyldioxime and dichloroglyoxime dianions, respectively) afforded the hydroxy-containing clathrochelate derivatives with the hydroxyl substituent inherently bound to the ribbed chelate fragment of the macrobicyclic ligand. The triethylammonium and tetra-n-butylammonium salts of the clathrochelate FeBd2(OClGm)(BF)2] anion have been characterized using elemental analysis, MALDI-TOF mass spectrometry, IR, UV–Vis, 57Fe Mössbauer and 1H, 13C{1H}, 11B and 19F NMR spectroscopies, and X-ray crystallography. The X-ray structural data for this deprotonated anion showed strong delocalization of its negative charge into the clathrochelate framework.
Keywords:Macrocyclic complexes  Iron(II)  Clathrochelates  Ligand reactivity  X-ray crystallography
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