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Resolution of Crystallographic Disorder by Coupled Single Crystal X-Ray Diffraction and Mossbauer Spectroscopy: Study of the (π-(1)-2-Thiollyl) Iron (II) System

  • Betty R. Davis
  • Ivan Bernal
  • John Buttone
  • Mary L. Good

Abstract

In 1967, Hertier and co-workers [1] 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 [1] 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.

Keywords

Sulfur Atom Quadrupole Splitting Boron Atom Mossbauer Spectrum Iron Foil 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

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References

  1. 1.
    W. R. Hertier, F. Klanberg and E. L. Muetterties, Inorg. Chem. 6, 1696 (1967).CrossRefGoogle Scholar
  2. 2.
    B. R. Davis and I. Bemal, J. Cryst. Mol. Struct., in press.Google Scholar
  3. 3.
    T. Birchall and I. Drummond, Inorg. Chem. 10, 399 (1971).CrossRefGoogle Scholar
  4. 4.
    G. K. Wertheim and R. H. Herber, J. Chem. Physics 38, 2106 (1963).CrossRefGoogle Scholar
  5. 5.
    M. F. Hawthorne and G. B. Dunks, Science 178, 462 (1972) and references therein.CrossRefGoogle Scholar
  6. 6.
    R. L. Collins, J. Chem. Physics, 42, 1072 (1965).CrossRefGoogle Scholar
  7. 7.
    J. P. Dahl and C. F. Ballhausen, Mat. Fys. Medd. Dan. Vid. Selsk. 33, No. 5 (1961).Google Scholar
  8. 8.
    D. St. Clair, A. Zalkin, and D. H. Templeton, J. Am. Chem. Soc., 92, 1173 (1970).CrossRefGoogle Scholar
  9. 9.
    A. V. Lesikar, J. Chem. Phys., 40, 2746 (1964).CrossRefGoogle Scholar

Copyright information

© New England Nuclear Corporation 1973

Authors and Affiliations

  • Betty R. Davis
    • 1
    • 2
  • Ivan Bernal
    • 1
    • 2
  • John Buttone
    • 1
    • 2
  • Mary L. Good
    • 1
    • 2
  1. 1.Brookhaven National LaboratoryUpton, Long IslandUSA
  2. 2.Louisiana State University in New OrleansLakefront, New OrleansUSA

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