TY - JOUR
T1 - High-resolution synchrotron data collection for charge-density work at 100 and 20 K
AU - Luger, Peter
AU - Messerschmidt, Marc
AU - Scheins, Stephan
AU - Wagner, Armin
PY - 2004/9/1
Y1 - 2004/9/1
N2 - For the measurement of very accurate high-resolution X-ray data for charge-density work, synchrotron beamlines provide a bright radiation source of outstanding properties. Most important are the very high primary intensity and the possibility of choosing hard radiation with λ ≈ 0.5 Å or even shorter. This together with area detection and a stable low-temperature device means that accurate and large data sets can be measured in a short time. A number of data collections are reported, which were carried out at the beamlines F1 and D3 of Hasylab (DESY, Hamburg) first at 100 K and later at 15-20 K, demonstrating the quality of the measured intensities. A low temperature of around 20 K was obtained at beamline D3 with a double-stage closed-cycle helium cryostat where the standard beryllium cylinder of the vacuum chamber was replaced by a 0.1 mm Kapton film. Comparison of different data sets measured for a strychnine crystal demonstrated how I/σ ratios favorably improve if synchrotron radiation at a low temperature of 15 K was used. Synchrotron-based studies on several biologically active compounds are briefly summarized and a synchrotron experiment of an otherwise not sufficiently diffracting crystal of a tetraphenyl barbaralane derivative is described in detail. Atomic volumes and charges of a highly substituted C60 fullerene are reported derived from a synchrotron data set of more than 350000 reflections.
AB - For the measurement of very accurate high-resolution X-ray data for charge-density work, synchrotron beamlines provide a bright radiation source of outstanding properties. Most important are the very high primary intensity and the possibility of choosing hard radiation with λ ≈ 0.5 Å or even shorter. This together with area detection and a stable low-temperature device means that accurate and large data sets can be measured in a short time. A number of data collections are reported, which were carried out at the beamlines F1 and D3 of Hasylab (DESY, Hamburg) first at 100 K and later at 15-20 K, demonstrating the quality of the measured intensities. A low temperature of around 20 K was obtained at beamline D3 with a double-stage closed-cycle helium cryostat where the standard beryllium cylinder of the vacuum chamber was replaced by a 0.1 mm Kapton film. Comparison of different data sets measured for a strychnine crystal demonstrated how I/σ ratios favorably improve if synchrotron radiation at a low temperature of 15 K was used. Synchrotron-based studies on several biologically active compounds are briefly summarized and a synchrotron experiment of an otherwise not sufficiently diffracting crystal of a tetraphenyl barbaralane derivative is described in detail. Atomic volumes and charges of a highly substituted C60 fullerene are reported derived from a synchrotron data set of more than 350000 reflections.
UR - http://www.scopus.com/inward/record.url?scp=19744371545&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=19744371545&partnerID=8YFLogxK
U2 - 10.1107/S0108767304014825
DO - 10.1107/S0108767304014825
M3 - Article
C2 - 15477676
AN - SCOPUS:19744371545
SN - 0108-7673
VL - 60
SP - 390
EP - 396
JO - Acta Crystallographica Section A: Foundations of Crystallography
JF - Acta Crystallographica Section A: Foundations of Crystallography
IS - 5
ER -