Note
867
Experimental Part
All work was carried out under argon (4.8, Westfalen
AG) using standard Schlenk techniques. Liquid ammonia
(
3.8, Westfalen AG) was dried and stored over sodium
◦
metal at −78 C. FeF was prepared from the reaction of
3
◦
FeCl ·6H O with 100 % F gas at 300 C. A reaction ves-
3
2
2
sel was charged with 130 mg (1.15 mmol) of FeF and, af-
3
ter evacuation, with approximately 10 mL of liquid ammo-
◦
nia at −40 C. Colorless, needle-shaped crystals suitable for
the X-ray diffraction experiment were obtained. The crys-
tals are temperature-sensitive and decrepitate at temperatures
◦
above −20 C losing ammonia. All crystals were handled
in a perfluorinated ether under nitrogen atmosphere at tem-
◦
peratures below −50 C, and mounted on the diffractometer
using the MiTeGen MicroLoop system. The structure was
solved using Direct Methods and refined on F [11, 12].
All non-hydrogen atoms were localized by Fourier cycling
methods and refined anisotropically. The hydrogen atoms
were localized by Fourier cycling methods and refined iso-
tropically.
Fig. 4. The unit cell of the title compound at 150 K. Dis-
placement ellipsoids are shown at the 70 % probability level,
hydrogen atoms with arbitrary radii.
2
stability at low temperature, but decomposition occurs
on warming.
Further details of the crystal structure investigation
are available from the FachinformationszentrumKarls-
ruhe, D-76344 Eggenstein-Leopoldshafen (Germany),
Acknowledgements
F. K. would like to thank the Fonds der Chemischen Indus-
http://www.fiz-karlsruhe.de/icsd.html, on quoting the trie for his stipend and Solvay Fluor for a continuous supply
of elemental fluorine. Deutsche Forschungsgemeinschaft is
depository number CSD 423231 for the compound, the
names of the authors, and the citation of the paper.
acknowledged for financial support.
[
[
[
[
1] E. C. Franklin, C. A. Kraus, Am. Chem. J. 1898, 20,
20 – 853.
2] W. Biltz, E. Rahlfs, Z. Anorg. Allg. Chem. 1927, 166,
51 – 376.
3] G. F. H u¨ ttig, Z. Anorg. Allg. Chem. 1920, 114, 161 –
73.
[7] F. Kraus, S. A. Baer, M. B. Fichtl, Eur. J. Inorg. Chem.
2009, 441 – 447.
8
[8] F. Kraus, S. A. Baer, Chem. Eur. J. 2009, 15, 8269 –
8274.
3
[9] F. Kraus, M. B. Fichtl, S. A. Baer, Z. Naturforsch. 2009,
1
64b, 257 – 262.
4] R. Eßmann, G. Kreiner, A. Niemann, D. Rechenbach,
A. Schmieding, T. Sichla, U. Zachwieja, H. Jacobs, Z.
Anorg. Allg. Chem. 1996, 622, 1161 – 1166.
[10] W. Meng, F. Kraus, Eur. J. Inorg. Chem. 2008, 3068 –
3074.
[11] G. M. Sheldrick, SHELXS-97, University of G o¨ ttingen,
G o¨ ttingen (Germany), 1997. See also: G. M. Sheldrick,
Acta Crystallogr. 1990, A46, 467 – 473.
[12] G. M. Sheldrick, SHELXL-97, University of G o¨ ttingen,
G o¨ ttingen (Germany), 1997. See also: G. M. Sheldrick,
Acta Crystallogr. 2008, A64, 112 – 122.
[
5] S. A. Baer, F. Kraus, Z. Naturforsch. 2010, 65b, 1177 –
1184.
[
6] F. Kraus, S. A. Baer, Z. Anorg. Allg. Chem. 2010, 636,
414 – 422.
-
10.1515/znb-2011-0814
Downloaded from De Gruyter Online at 09/13/2016 12:25:32AM
via free access