Resolution of Crystallographic Disorder by Coupled Single Crystal X-Ray Diffraction and Mossbauer Spectroscopy: Study of the (π-(1)-2-Thiollyl) Iron (II) System
In 1967, Hertier and co-workers  reported the synthesis of the anion, B10H10S2-, which was found to react with transltion metal halides to form complexes similar to those formed with cyclopentadienides and with B10H11C 2 2- . Their report  indicated however, that the spectra arid other physical data were insufficient to determine unambiguously whether the sulfur atom of the thiaborane was exo-cyclic or whether it was an integral part of the boron framework. Thus we decided to determine the crystal structure of the compound, [(CH3)4N]2 [Fe(B10H10S)2] for which suitable crystals for x-ray analysis could be obtained. In the process of refining the structural data it became evident that a crystallographic disorder occurs (vide infra) which is not readily resolved by structural analysis arguments alone, but which could be amenable to interpretation via a combination of crystallographic data and Mössbauer spectroscopy. This report is a summary of our combined efforts.
KeywordsSulfur Atom Quadrupole Splitting Boron Atom Mossbauer Spectrum Iron Foil
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