High-resolution synchrotron data collection for charge-density work at 100 and 20 K

Acta Crystallogr A. 2004 Sep;60(Pt 5):390-6. doi: 10.1107/S0108767304014825. Epub 2004 Aug 26.

Abstract

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 lambda approximately 0.5 A 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/sigma 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 C(60) fullerene are reported derived from a synchrotron data set of more than 350000 reflections.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Amino Acids / chemistry
  • Bridged-Ring Compounds / chemistry
  • Cold Temperature
  • Cyclohexanes / chemistry
  • Cyclopropanes / chemistry
  • Fullerenes / chemistry
  • Molecular Structure
  • Oligopeptides / chemistry
  • Organic Chemicals / chemistry*
  • Strychnine / chemistry
  • Synchrotrons / instrumentation*

Substances

  • Amino Acids
  • Bridged-Ring Compounds
  • Cyclohexanes
  • Cyclopropanes
  • Fullerenes
  • Oligopeptides
  • Organic Chemicals
  • Strychnine
  • fullerene C60