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2008 Zeitschrift für Kristallographie - New Crystal Structures  
H 18 NaO 12 PSSr, cubic, P2 1 3 (no. 198), a = 10.917(1) Å, V = 1301.1 Å 3 , Z = 4, R gt (F) = 0.041, wR ref (F 2 ) = 0.087, T = 223 K. Source of material Trisodium monothiophosphate, Na 3 [PO 3 S], was synthesized from aqueous solutions of NaOH and PSCl 3 according to [1] . A solution of sodium strontium monothiophosphate nonahydrate was obtained by adding SrCl 2 · 6H 2 O (1.50 g, 5.626 mmol) to a solution of Na 3 [PO 3 S] (1.01 g, 5.626 mmol) in 40 mL distilled water at 40°C. Slowly cooling
more » ... C. Slowly cooling at room temperature yielded cubeshaped colorless crystals of the title compound within some days. Experimental details The H atom parameters were refined freely except those which did not converge. The latter ones were fixed, positional parameters at the parameters found from Fourier difference maps and U iso at 0.05 Å 2 . Discussion The alkali metal oxothiophosphates were first reported by Berzelius in 1843 [2] . In 1885, Kubierschky has investigated the hydrolysis of P 4 S 10 in NaOH and prepared the oxothiophosphates Na 3 [PO 2 S 2 ]·11H 2 Oand Na 3 [POS 3 ]·11H 2 O[3]. Afew oxothiophosphates have been characterized in the last years [4] [5] [6] [7] [8] . The present work is a continuation of structural studies of thiophosphates [9,10]. The crystal structure of title compound is isotypic to those of NaMPO 4 · 9H 2 O (M = Ba, Sr) [11, 12] and consists of discrete [PO 3 S] tetrahedra, [SrO 9 ], [NaO 6 ] polyhedra, and water molecules, held together by hydrogen bonds of type O-H···O and O-H···S. Each Sr 2+ cation is ninefold coordinated by water O atoms with Sr-O distances of 2.592(4) Å -2.814(5) Å. Its coordination polyhedron can be described as tricapped trigonal prism. The Na + cation is sixfold coordinated by water oxygen atoms with Na-O distances of 2.455(5) Å -2.485(5) Å. One [NaO 6 ]and three[SrO 9 ]polyhedra are connected through common edges completing the three-dimensional framework structure ( figure, top). Equal lengths of the P-O bonds of the [PO 3 S] 3anion indicate an ideal C 3v symmetry. P-S (2.035(4) Å) and P-O (1.524(5) Å) bond lengths and S-P-O bond angle (109.0(2)°) are similar to those found in Na 3 [POS 3 ]·11H 2 O [4] and Na 3 [PO 3 S] · 12H 2 O [13]. Each thiophosphate S or O atom acts as an acceptor in three hydrogen bonds, linking water oxygen donors (figure, bottom). The hydrogen-bonding distances O-H···O range from 2.732(1) Å to 2.838(2) Å, the O-H···O angles from 152.0(1)°to 165.0(1)°and the hydrogen-bonding distance O-H···S is 3.317(1) Å and the O-H···S angle 146.9(1)°. These values are typical for hydrogen bonds and correspond to literature data of Na 3 [PO 2 S 2 ] ·
doi:10.1524/ncrs.2008.frontmatter1 fatcat:mutgqoaewnb6tohbi2brgopcji