Syntheses, Crystal Structures, NMR Spectroscopy, and Vibrational Spectroscopy of Sr(PO3F)·H2O and Sr(PO3F). Issue 7 (8th February 2016)

• Record Type: Journal Article
• Authors: Jantz, Stephan G.; van Wüllen, Leo; Fischer, Andreas; Libowitzky, Eugen; Baran, Enrique J.; Weil, Matthias; Höppe, Henning A.
• Is Part Of: European journal of inorganic chemistry. Issue 7(2016)
• Page Start: 1121
• Page End: 1128
• Publication Date: 2016-02-08
• Subjects: Main group elements -- Layered compounds -- Solid‐state structures -- Structure elucidation -- Topotactic reactions; Chemistry, Inorganic -- Periodicals; Organometallic chemistry -- Periodicals; Bioinorganic chemistry -- Periodicals; Solid state chemistry -- Periodicals; 546
• DOI: 10.1002/ejic.201501143
• Languages: English
• ISSNs: 1434-1948

Abstract

Abstract: Single crystals of Sr(PO3 F)· H2 O { P 21 / 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 [SrO8 ] polyhedra and PO3 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(PO3 F). The monazite‐type crystal structure of Sr(PO3 F) was elucidated from the X‐ray powder data by simulated annealing [ P 21 / 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, Rp = 0.010, Rwp = 0.015, RF = 0.030]. During dehydration, the structure of Sr(PO3 F)· H2 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. Abstract : The dehydration of Sr(PO3 F)· H2 O yields Sr(PO3 F) by a topotactic reaction. The crystal structures of both solids were elucidated by X‐ray diffraction methods, and the presence of P–F bonds was confirmed by magic‐angle spinning (MAS) NMR and IR spectroscopy.