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Iron(III) complexes of 5,11,17,23-tetra-tert-butyl-24-hydroxy-26,27,28-tris(diethylcarbamoylmethoxy)calix[4]arene (II) and 5,11,17,23,29,35-hexa-tert-butyl-36,39-dihydroxy-37,38,40,41-tetrakis(diethylcarbamoylmethoxy)calix[6]arene (IV) have been synthesised, and a single crystal structure determination has been carried out on [Fe(II  − H)](FeCl4)2; the iron in the complex cation is bound to all seven O atoms of the calixarene with the shortest Fe–O distance to the phenolate O atom. The voltammetric properties of these complexes and the previously described Fe(III) complex of 5,11,17,23-tetra-tert-butyl-25,27-dihydroxy-26,28-bis(diethylcarbamoylmethoxy)calix[4]arene (I) have been studied. The results suggest that the complexes of I and II undergo a reduction which is metal-centred, and an oxidation which is ligand-centred.

Syntheses, structural studies and solution properties of iron complexes of some amide-substituted calixarenes