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Crystals 2018, 8(1), 51; https://doi.org/10.3390/cryst8010051

Determination of the Correct Composition of “Hydrous Lead(II) Oxotellurate(IV)” as PbTeO3, Crystallizing as a New Polymorph

1
Institute for Chemical Technologies and Analytics, Division of Structural Chemistry, TU Wien, Getreidemarkt 9/164-SC, A-1060 Vienna, Austria
2
NETZSCH-Gerätebau GmbH, Wittelsbacherstraße 42, D-95100 Selb, Germany
3
Institute for Mineralogy and Crystallography, Faculty of Geosciences, Geography and Astronomy, Althanstr. 14, A-1090 Vienna, Austria
*
Author to whom correspondence should be addressed.
Received: 21 December 2017 / Revised: 16 January 2018 / Accepted: 17 January 2018 / Published: 19 January 2018
(This article belongs to the Special Issue Synthesis and Structural Investigations of Polymorphic Compounds)
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Abstract

In previous studies, it has been reported that the crystalline product precipitated from the reaction of aqueous solutions of lead(II) salts with sodium oxotellurate(IV) is hydrous lead(II) oxotellurate(IV); however, there have been conflicting specifications of the water content, and the crystal structure of the product is yet undetermined. During the present study, it was shown that the precipitated material does not contain any structural water and in fact represents the third modification (denoted as γ-) of PbTeO3, as revealed by thermal analysis, vibrational spectroscopy, single crystal and powder X-ray diffraction. This modification crystallizes in the space group P 1 ¯ with five formula units in the asymmetric unit, comprising off-centred coordination polyhedra around the PbII cations (coordination numbers: 5–7 with Pb-O distances ranging from 2.3–3.0 Å), and trigonal-pyramidal TeO32− units. The thermal behaviour and structural phase transitions of PbTeO3 were investigated by means of temperature-dependent X-ray powder diffraction and complementary thermal analysis measurements. In addition, the crystal structure of β-PbTeO3 was redetermined, and a comparison was made between the three known polymorphs of PbTeO3. View Full-Text
Keywords: structure determination; lead(II) oxotellurate(IV); polymorphism; thermal behaviour; thermal analysis; vibrational spectroscopy structure determination; lead(II) oxotellurate(IV); polymorphism; thermal behaviour; thermal analysis; vibrational spectroscopy
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).

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Weil, M.; Shirkhanlou, M.; Füglein, E.; Libowitzky, E. Determination of the Correct Composition of “Hydrous Lead(II) Oxotellurate(IV)” as PbTeO3, Crystallizing as a New Polymorph. Crystals 2018, 8, 51.

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