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Solving the Crystal Structure of Cd5(OH)8(NO3)2·2H2O from Powder Diffraction Data. A Comparison with Single Crystal Data

Published online by Cambridge University Press:  10 January 2013

Patricia Bénard ,
Michèle Louër  and
Daniel Louër
Patricia Bénard
Affiliation:
Laboratoire de cristallochimie (URA 254), Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France
Michèle Louër
Affiliation:
Laboratoire de cristallochimie (URA 254), Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France
Daniel Louër
Affiliation:
Laboratoire de cristallochimie (URA 254), Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France
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Abstract

A comparison between the results of ab initio structure determination from X-ray powder diffraction data of a new cadmium hydroxide nitrate, Cd5(OH)8 (NO3)2·2H2O (SG C2/m), and those obtained from single crystal data is presented. The powder diffraction pattern has been analysed by an indexing method and fitting techniques. A total of 119 unambiguously indexed reflections has been extracted and used in subsequent treatment. The power of powder techniques to index the pattern and to find the structure model by normal Patterson and Fourier methods is clearly shown. The refinement of approximate coordinates has been carried out by the Rietveld method (444 reflections). The comparison of results with those obtained from single crystal data (2218 reflections) shows that the precision of positional parameter values is lower by a factor of 10, on average, in the powder study. These results are discussed in terms of crystallographic parameters (number of reflections used, number of parameters to refine, contrast between atoms) and, also, in terms of sample dependent properties (preferred orientation effect, impurity). Finally, the crystal structure has been derived from powder data with a precision probably sufficient for most purposes.

Type
Research Article
Information
Powder Diffraction , Volume 6 , Issue 1 , March 1991 , pp. 10 - 15
Copyright
Copyright © Cambridge University Press 1991

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