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Chapter 7 151
Single crystal XRD data for Ru-SBU were collected on an Oxford Supernova with Atlas
detector (Cu-Kα 1.54184 Å) by Dr. K. Freitag and M. Winter. The crystals were coated with
a perfluoropolyether, collected with a glass fiber loop under a microscope and mounted
in the nitrogen cold gas stream of the diffractometer. For the air-sensitive crystals, they
were transferred from a Schlenk tube in an argon stream onto a specimen holder with
perfluoro-polyalkylether before being picked up with the glass fiber loop. The structural
solution and refinement were done M. Winter and W. Zhang (with the assistance of, Dr. A.
Puls, and Dr. S. Henke) using the program suite Olex2 [298] with the executables SHELXS97
and SHELXL97. [299] For refinement the full-matrix least squares on F2 method was
employed. All non-hydrogen atoms were refined anisotropically while the hydrogen
atoms were calculated and refined with isotropic character.
7.1.2 FT-IR spectroscopy
Conventional FTIR spectra were collected by W. Zhang on a Bruker Alpha FTIR instrument
in the ATR geometry with a diamond ATR unit in the range 400–4000 cm -1 inside a
LABStar MB 10 compact MBraun glove-box (argon atmosphere).
Ultra High Vacuum (UHV) FT-IR measurements were performed using a novel UHV-FTIRS
apparatus (state‐of‐the‐art vacuum IR spectrometer (Bruker, VERTEX 80v) coupled to a
novel UHV system (Prevac)) [300] by our collaboration partners, M. Kauer and P. Guo (the
group of Dr. Y. Wang,) in the Laboratory of Industrial Chemistry (Prof. Dr. M. Muhler),
Ruhr‐University Bochum. The sample transfer to the instrument, data acquisition and
interpretation were carried out by M. Kauer and P. Guo. The discussion of the selected
data and the experimental/synthetic work documented in the thesis were done by W.
Zhang. The powder samples were first pressed into a stainless steel grid (0.5 x 0.5 cm)
covered by gold and then mounted on a sample holder, which was specially designed for
the FTIR transmission measurements under UHV conditions. The grid was cleaned by
heating up to 850 K to remove all contaminants formed on it during preparation. The base
pressure in the measurement chamber was 5 x 10 -11 mbar. The optical path inside the IR
spectrometer and the space between the spectrometer and UHV chamber were also
evacuated to avoid atmospheric moisture adsorption resulting in a high sensitivity and
stability. The MOF samples were cleaned in the UHV chamber by heating to 500 K in order
to remove the contaminants involved during synthesis and all the adsorbed species such