The first ribbed functionalized tris-dioximate clathrochelates with inherent hydroxyl substituents: Synthesis, spectra and X-ray structure

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.