Ultra-low-temperature X-ray data collection with a newly developed 0.1 mm Kapton-film cylinder for a closed-cycle helium cryostat

被引:21
作者
Meserschmidt, M
Meyer, M
Luger, P
机构
[1] Free Univ Berlin, Inst Chem Crystallog, D-14195 Berlin, Germany
[2] Oxford Diffract Ltd, Abingdon OX14 1RL, Oxon, England
关键词
D O I
10.1107/S0021889803019411
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
A 0.1 mm Kapton- film vacuum chamber was constructed to be mounted on the cold head of a closed- cycle helium cryostat. The use of Kapton instead of beryllium results in a low and practically non- structured background, which is thus tolerable on the area- detection frames of modern CCD detectors. The Kapton chamber is only fixed at the upper and lower holders of the cryostat and its counterweight, and is stabilized by spanning with fine pitch threads, holding constant the necessary vacuum of 10(-6) mbar for at least several days. Low costs and non- toxicity are further advantages of this material; moreover, the sample remains visible even after cooling. Data collections on strychnine single crystals at 15 K showed improved I/sigma ratios of high- order reflections compared with 100 K data, most favourably when synchrotron primary radiation was used.
引用
收藏
页码:1452 / 1454
页数:3
相关论文
共 5 条
[1]  
Burnett M.N., 1996, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations
[2]   Topological analysis of experimental electron densities. 3. Potassium hydrogen(+)-tartrate at 15 K [J].
Koritsanszky, T ;
Zobel, D ;
Luger, P .
JOURNAL OF PHYSICAL CHEMISTRY A, 2000, 104 (07) :1549-1556
[3]   STRUCTURAL STUDY OF THE STRYCHNINE MOLECULE IN CRYSTALS OF THE FREE BASE AND OF THE NITRIC-ACID COMPLEX [J].
MOSTAD, A .
ACTA CHEMICA SCANDINAVICA SERIES B-ORGANIC CHEMISTRY AND BIOCHEMISTRY, 1985, 39 (09) :705-716
[4]   The search for homoaromatic semibullvalenes. 6. X-ray structure and charge density studies of 1,5-dimethyl-2,4,6,8-semibullvalenetetracarboxylic dianhydride in the temperature range 123-15 K [J].
Williams, RV ;
Gadgil, VR ;
Luger, P ;
Koritsanszky, T ;
Weber, M .
JOURNAL OF ORGANIC CHEMISTRY, 1999, 64 (04) :1180-1190
[5]   CHARGE-DENSITY STUDIES ON SMALL ORGANIC-MOLECULES AROUND 20-K - OXALIC-ACID DIHYDRATE AT 15-K AND ACETAMIDE AT 23-K [J].
ZOBEL, D ;
LUGER, P ;
DREISSIG, W ;
KORITSANSZKY, T .
ACTA CRYSTALLOGRAPHICA SECTION B-STRUCTURAL SCIENCE CRYSTAL ENGINEERING AND MATERIALS, 1992, 48 :837-848