Syntheses, Crystal Structures, NMR Spectroscopy, and Vibrational Spectroscopy of Sr(PO₃F)•H₂O and Sr(PO₃F)

Author(s)

Stephan G. Jantz, Leo van Wüllen, Andreas Fischer, Eugen Libowitzky, Enrique J. Baran, Matthias Weil, Henning A. Höppe

Abstract

Single crystals of Sr(PO3F)-·H2O {P21/c, Z = 4, a = 7.4844(2) Å, b = 7.0793(2) Å, c = 8.4265(2) Å, ß = 108.696(1)-°, V = 422.91(2) Å3, 2391 Fo2, 70 parameters, R1[F2 > 2s(F2)-] = 0.036; wR2(F2 all) = 0.049, S = 1.054} were grown from an aq. soln. by a metathesis reaction. The structure comprises [SrO8] polyhedra and PO3F tetrahedra that form a layered arrangement parallel to (100)-. The topotactic dehydration of this phase proceeds between 80 and 140 °C to afford Sr(PO3F)-. The monazite--type crystal structure of Sr(PO3F) was elucidated from the X--ray powder data by simulated annealing [P21/c, Z = 4, a = 6.71689(9) Å, b = 7.11774(11) Å, c = 8.66997(13) Å, ß = 128.0063(7)-°, V = 326.605(8) Å3, Rp = 0.010, Rwp = 0.015, RF = 0.030]-. During dehydration, the structure of Sr(PO3F)-·H2O collapses along [100] from a layered arrangement into a framework structure, accompanied by a change of the coordination no. of the Sr2+ ions from eight to nine. The magic--angle spinning (MAS) NMR and vibrational spectroscopy data of both phases are discussed.

Organisation(s)

Department of Mineralogy and Crystallography

External organisation(s)

Universität Augsburg, Universidad Nacional de La Plata, Technische Universität Wien

Journal

European Journal of Inorganic Chemistry

Volume

2016

Pages

1121-1128

No. of pages

8

ISSN

1434-1948

DOI

https://doi.org/10.1002/ejic.201501143

Publication date

02-2016

Peer reviewed

Yes

Austrian Fields of Science 2012

104026 Spectroscopy, 104011 Materials chemistry, 105113 Crystallography, 104024 X-ray structural analysis

Keywords

Portal url

https://ucrisportal.univie.ac.at/en/publications/syntheses-crystal-structures-nmr-spectroscopy-and-vibrational-spectroscopy-of-srpo3fh2o-and-srpo3f(c852806f-3969-45e4-a70b-0b899b488dd1).html