P. Woidy, F. Kraus
ARTICLE
Further details of the crystal structure investigations may be obtained
from the Fachinformationszentrum Karlsruhe, 76344 Eggenstein-
Leopoldshafen, Germany (Fax: +49-7247-808-666; E-Mail:
posited data.html) on quoting the depository number CSD-426384.
Experimental Section
All work was carried out under exclusion of humidity and air in an
atmosphere of dried and purified argon (Westfalen AG) using vacuum
glass lines or a glove box (MBraun). Liquid ammonia (Westfalen AG)
was dried and stored over sodium (VWR) in a special high-vacuum
glass line. All reaction vessels were made of borosilicate glass and Supporting Information (see footnote on the first page of this article):
flame-dried three times before use. The purity of silver acetate Plots of the profile fitting of the powder X-ray pattern recorded from
(ChemPur, 99%) was checked by powder X-ray diffractometry and IR
spectroscopy and could be used without further purification.
compound 1 at room temperature and the thermogram. Table S1 con-
tains the assigned IR and Raman frequencies.
Preparation of [Ag(NH3)2]OAc (1): A reaction vessel was charged
with colorless AgOAc (110 mg, 0.659 mmol) and liquid ammonia
(10 mL) at –78 °C. This led to a clear and colorless solution and small
amounts of an undissolved colorless residue, which disappeared after
a few weeks of storage at –40 °C and finally needle-shaped colorless
crystals were obtained from this solution. Single crystals can also be
obtained by slow evaporation of ammonia within two days at –78 °C.
Suitable single-crystals were separated manually at –40 °C under per-
fluoroether oil (Galden PFPE, Solvey Solexis) and a nitrogen atmo-
sphere. Compound 1 can be prepared as a powder by simply dissolving
AgOAc in NH3(l) and removing the liquid NH3 at room temperature.
Acknowledgements
We thank M. Sc. M. Fichtl, TUM, for the thermogravimetric analyses
and Prof. A. Kornath, LMU, for allowing us to perform measurements
on his Raman spectrometer. F. K. would like to thank the Deutsche
Forschungsgemeinschaft for his Heisenberg fellowship. P. W. would
like to thank the Deutsche Forschungsgemeinschaft for financial sup-
port and the TUM Graduate School. We thank Prof. Dr. B. G. Müller,
Giessen, and Prof. R. Hoppe, Giessen, for the kind donation of many
chemicals and equipment.
Powder X-ray Diffractometry: Powder X-ray patterns were recorded
in flame-sealed Lindemann glass capillaries using a Stoe Stadi-P pow-
der diffractometer with germanium-monochromated Mo-Kα1 radiation
or germanium-monochromated Cu-Kα1 radiation and a Mythen 1 K
detector.[27] Evaluation of the powder patterns was carried out with the
software package of WinXPOW.[28] Profile fitting was done with
JANA 2006,[29] with an Rp of 3.17% and a wRp of 5.25% (see Sup-
porting Information).
References
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Thermogravimetric Analysis – Mass Spectroscopy: Thermogravi-
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equipped with a TASC 414/3 signal amplifier and a mass-selective
analyzer Pfeiffer Omnistar GSD 301 O in a steady argon stream (5.0,
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MiTeGen MicroLoop system. Evaluation of diffraction data was car-
ried out by using the CRYSALISRED[33] software. An empirical ab-
sorption correction was applied by using spherical harmonics within
SCALE3 ABSPACK.[33] The structure was solved using Direct Meth-
ods (SHELXS-97)[34] and refined against F2 (SHELXL-97).[35] Non-
hydrogen atoms were located by Difference Fourier synthesis and re-
fined anisotropically. Hydrogen atoms were located from the Differ-
ence Fourier synthesis and refined isotropically. The residual electron
density is located close to the silver atom.
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© 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Z. Anorg. Allg. Chem. 2013, 2643–2647