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Crystal structure of antimony oxalate hydroxide, Sb(C2O4)OH

Published online by Cambridge University Press:  29 February 2012

James A. Kaduk ,
Mark A. Toft  and
Joseph T. Golab
James A. Kaduk*
Affiliation:
INEOS Technologies, P.O. Box 3011, MC F-9, Naperville, Illinois 60566
Mark A. Toft
Affiliation:
INEOS Technologies, P.O. Box 3011, MC F-9, Naperville, Illinois 60566
Joseph T. Golab
Affiliation:
INEOS Technologies, P.O. Box 3011, MC F-9, Naperville, Illinois 60566
*
Electronic mail: kaduk@polycrystallography.com
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Abstract

The crystal structure of Sb(C2O4)OH has been solved by charge flipping in combination with difference Fourier techniques using laboratory X-ray powder data exhibiting significant preferred orientation and refined by the Rietveld method. The compound crystallizes in Pnma with a=5.827 13(3), b=11.294 48 (10), c=6.313 77(3) Å, V=415.537(5) Å3, and Z=4. The crystal structure contains pentagonal pyramidal Sb3+ cations, which are bridged by hydroxyl groups to form zigzag chains along the a axis. Each oxalate anion chelates to two Sb in approximately the ab plane, linking the chains into a three-dimensional framework. The H of the hydroxyl group is probably disordered in order to form stronger more-linear hydrogen bonds. The highest energy occupied molecular orbitals are the Sb3+ lone pairs. The structure is chemically reasonable compared to other antimony oxalates and to Bi(C2O4)OH.

Keywords

Antimonyoxalatehydroxidecrystal structureRietveld refinementcharge flipping

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Type
Technical Articles
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Powder Diffraction , Volume 25 , Issue 1 , March 2010 , pp. 19 - 24
Copyright
Copyright © Cambridge University Press 2010

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