Synthesis, spectral and electrochemical characteristics of asymmetrical iron(II) tris-dioximates

• Published in: Polyhedron 1998-01, Vol.17 (25), p.4315-4326
• Main Authors: Voloshin, Yan Z., Varzatskii, Oleg A., Palchik, Aleksei V., Polshin, Ernest V., Maletin, Yurii A., Strizhakova, Nataly G.
• Format: Article
• Language: English
• Subjects: cage compounds; electrochemistry; f>57 Fe Mössbauer spectra; X-ray structure
• ISSN: 0277-5387
• DOI: 10.1016/S0277-5387(98)00168-5

Meridianal- and axial-asymmetrical clathrochelate tris-dioximates of the FeD 2D′(BF) 2 and FeD 3(BX)(Y) types (where D,D′=dioximes dianions, X=C 6H 5, F; Y=BF, B n-C 4H 9, SnCl 3) have been prepared by a stepwise synthesis from a planar-square macrocyclic precursors in the first case and from a semiclathrochelate compounds immobilized on the sorbent surface in the second one. The composition and structure of the isolated compounds have been established from elemental analysis data, polynuclear NMR, 57 Fe Mössbauer and FAB mass spectra. The structure parameters of α-benzyldioximate FeBd 3(BF)(B n-C 4H 9) · C 6H 5CH 3 · 1 2–C 8H 16 (Fe–N distance – 1.89 Å, bite angle – 38.6°, polyhedron distortion angle – 17.9°) were determined by X-ray crystallography. The electrochemical properties of the obtained complexes and their dependence on the nature of a ligand have been determined by cyclic voltammetry.