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A powder X-ray diffraction study of lead chloride oxalate Pb2Cl2(C2O4): ab initio structure determination and thermal behavior

Published online by Cambridge University Press:  06 March 2012

Chaouki Boudaren ,
Jean-Paul Auffrédic ,
Michèle Louër  and
Daniel Louër
Chaouki Boudaren
Affiliation:
Laboratoire de Chimie du Solide et Inorganique Moléculaire (UMR 6511 CNRS), Université de Rennes, Institut de Chimie, Avenue du Général Leclerc, 35042 Rennes, France
Jean-Paul Auffrédic
Affiliation:
Laboratoire de Chimie du Solide et Inorganique Moléculaire (UMR 6511 CNRS), Université de Rennes, Institut de Chimie, Avenue du Général Leclerc, 35042 Rennes, France
Michèle Louër
Affiliation:
Laboratoire de Chimie du Solide et Inorganique Moléculaire (UMR 6511 CNRS), Université de Rennes, Institut de Chimie, Avenue du Général Leclerc, 35042 Rennes, France
Daniel Louër*
Affiliation:
Laboratoire de Chimie du Solide et Inorganique Moléculaire (UMR 6511 CNRS), Université de Rennes, Institut de Chimie, Avenue du Général Leclerc, 35042 Rennes, France
*
b)Author to whom correspondence should be addressed; Tel.: (33) 2 23 23 62 48; Fax: (33) 2 99 38 34 87; electronic mail: [email protected]
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Abstract

Mixed lead chloride oxalate, Pb2Cl2(C2O4), has been obtained in a polycrystalline form in the course of a study on precursors of nanocrystalline PZT-type oxides. Its crystal structure has been solved ab initio from powder diffraction data collected using a monochromatic radiation from a conventional X-ray source. The symmetry is monoclinic, space group C2/m, the cell dimensions are a=5.9411(3) Å, b=5.8714(4) Å, c=9.4212(4) Å, β=95.232(4)° and Z=2. The structure consists of a stacking of complex double sheets, built from lead polyhedra, parallel to (001) and connected together through oxalate groups. The lead atom is nine-fold coordinated by four O atoms from one bidentate and two monodentate oxalate groups and five Cl atoms. The polyhedron can be described as a highly distorted square antiprism mono-capped by a Cl atom. The thermal behavior of lead chloride oxalate, in vacuum and in air, is carefully described from temperature-dependent powder diffraction and thermogravimetric measurements. It is shown that reaction pathways are complicated by the identification of various oxide chloride phases.

Type
Technical Articles
Information
Powder Diffraction , Volume 18 , Issue 3 , September 2003 , pp. 205 - 213
Copyright
Copyright © Cambridge University Press 2005

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