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Syntheses, Crystal Structures, NMR Spectroscopy, and Vibrational Spectroscopy of Sr(PO 3 F)·H 2 O and Sr(PO 3 F)
Author(s) -
Jantz Stephan G.,
van Wüllen Leo,
Fischer Andreas,
Libowitzky Eugen,
Baran Enrique J.,
Weil Matthias,
Höppe Henning A.
Publication year - 2016
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201501143
Subject(s) - chemistry , crystallography , crystal structure , spectroscopy , magic angle spinning , infrared spectroscopy , nuclear magnetic resonance spectroscopy , stereochemistry , physics , organic chemistry , quantum mechanics
Single crystals of Sr(PO 3 F) · H 2 O { P 2 1 / c , Z = 4, a = 7.4844(2) Å, b = 7.0793(2) Å, c = 8.4265(2) Å, β = 108.696(1)°, V = 422.91(2) Å 3 , 2391 F o 2 , 70 parameters, R 1 [ F 2 > 2σ( F 2 )] = 0.036; wR 2 ( F 2 all) = 0.049, S = 1.054} were grown from an aqueous solution by a metathesis reaction. The structure comprises [SrO 8 ] polyhedra and PO 3 F tetrahedra that form a layered arrangement parallel to (100). The topotactic dehydration of this phase proceeds between 80 and 140 °C to afford Sr(PO 3 F). The monazite‐type crystal structure of Sr(PO 3 F) was elucidated from the X‐ray powder data by simulated annealing [ P 2 1 / c , Z = 4, a = 6.71689(9) Å, b = 7.11774(11) Å, c = 8.66997(13) Å, β = 128.0063(7)°, V = 326.605(8) Å 3 , R p = 0.010, R wp = 0.015, R F = 0.030]. During dehydration, the structure of Sr(PO 3 F) · H 2 O collapses along [100] from a layered arrangement into a framework structure, accompanied by a change of the coordination number of the Sr 2+ ions from eight to nine. The magic‐angle spinning (MAS) NMR and vibrational spectroscopy data of both phases are discussed.