electronic reprint Sr 5 (V IV OF 5 ) 3 F(H 2 O) 3 refined from a non-merohedrally twinned crystal Armel Le Bail, Anne-Marie Mercier and Ina Dix

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1 ISSN Inorganic compounds Metal-organic compounds Organic compounds Acta Crystallographica Section E Structure Reports Online ISSN Editors: W.T. A. Harrison, J. Simpson and M. Weil Sr 5 (V IV OF 5 ) 3 F(H 2 O) 3 refined from a non-merohedrally twinned crystal Armel Le Bail, Anne-Marie Mercier and Ina Dix Acta Cryst. (2009). E65, i46 i47 This open-access article is distributed under the terms of the Creative Commons Attribution Licence which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited. Volume 61 Part 11 November 2005 Acta Crystallographica Section E Structure Reports Online Editors: W. Clegg and D. G. Watson Acta Crystallographica Section E: Structure Reports Online is the IUCr s highly popular open-access structural journal. It provides a simple and easily accessible publication mechanism for the growing number of inorganic, metal-organic and organic crystal structure determinations. The electronic submission, validation, refereeing and publication facilities of the journal ensure very rapid and high-quality publication, whilst key indicators and validation reports provide measures of structural reliability. In 2007, the journal published over 5000 structures. The average publication time is less than one month. journals.iucr.org International Union of Crystallography * Chester Crystallography Journals Online is available from journals.iucr.org Acta Cryst. (2009). E65, i46 i47 Le Bail et al. Sr 5 (VOF 5 ) 3 F(H 2 O) 3

2 inorganic compounds Acta Crystallographica Section E Structure Reports Online ISSN Sr 5 (V IV OF 5 ) 3 F(H 2 O) 3 refined from a non-merohedrally twinned crystal Armel Le Bail, a * Anne-Marie Mercier a and Ina Dix b a Laboratoire des Oxydes et Fluorures, CNRS UMR 6010, Université du Maine, Le Mans, France, and b Bruker AXS GmbH, Östliche Rheinbrückenstrasse 49, D Karlsruhe, Germany Correspondence armel.le_bail@univ-lemans.fr = mm 1 T = 298 K Data collection Bruker SMART APEX CCD areadetector diffractometer Absorption correction: multi-scan (TWINABS; Bruker, 2003) Refinement R[F 2 >2(F 2 )] = wr(f 2 ) = S = reflections 290 parameters 9 restraints mm T min = 0.065, T max = (expected range = ) 6596 measured reflections 6596 independent reflections 4299 reflections with I > 2(I) H atoms treated by a mixture of independent and constrained refinement max = 1.28 e Å 3 min = 1.11 e Å 3 Received 14 May 2009; accepted 20 May 2009 Key indicators: single-crystal X-ray study; T = 298 K; mean (V O) = Å; R factor = 0.038; wr factor = 0.083; data-to-parameter ratio = The title compound, pentastrontium tris[pentafluoridooxidovanadate(iv)] fluoride trihydrate, was obtained under hydrothermal conditions. Its crystal structure has been refined from intensity data of a non-merohedrally twinned crystal. Two domains in almost equal proportions are related by a 180 rotation along the reciprocal [101]* vector. The structure may be considered as a derivative of the fluorite structure type, adopted here by SrF 2. In the title compound, fluorite-like large rods are recognized, built up from a group of 16 Sr atoms of which 6 are substituted by V atoms, leading to [Sr 10 V 6 ] 1 units. These rods extend infinitely along the b axis and are interconnected by the three water molecules. Each of the water molecules is shared by two different Sr atoms belonging to two different rods. The rods are also interconnected by an independent F atom in a distorted triangular [FSr 3 ] coordination and by hydrogen-bonding interactions via donor water molecules. The acceptors are either F atoms or the O atoms of the vanadyl ion, VO 2+, that is part of the [VOF 5 ] isolated octahedron. Related literature For V IV in [VOF 5 ] coordination, see: Crosnier-Lopez et al. (1994). Sr 2 V III 2 F 10 H 2 O which was also synthesized during this study is isostructural with Sr 2 Fe 2 F 10 H 2 O (Le Meins et al., 1997). For a description of similar independent F atoms in the crystal structure of Sr 5 Zr 3 F 22, see: Le Bail (1996). For bondvalence analysis, see: Brown & Altermatt (1985); Brese & O Keeffe (1991). Experimental Crystal data Sr 5 (VOF 5 ) 3 F(H 2 O) 3 M r = Monoclinic, P2 1 =n a = (2) Å b = (15) Å c = (4) Å = (4) V = (6) Å 3 Z =4 Mo K radiation Table 1 Hydrogen-bond geometry (Å, ). D HA D H HA DA D HA O1 H11O4 i 0.88 (4) 2.48 (5) (6) 132 (5) O1 H11O5 i 0.88 (4) 2.44 (4) (6) 143 (5) O1 H12F4 ii (18) 1.96 (3) (5) 157 (5) O2 H21F (4) 2.03 (4) (5) 146 (5) O2 H22F (4) 2.18 (4) (5) 135 (4) O3 H31F (5) 2.07 (5) (5) 164 (5) O3 H32O6 iii 0.89 (4) 2.17 (4) (5) 135 (5) Symmetry codes: (i) x; y þ 1; z; (ii) x þ 1 2 ; y þ 1 2 ; z þ 1 2 ; (iii) x 1; y; z. Table 2 Valence-bond analysis of Sr 5 (V IV OF 5 ) 3 F(H 2 O) 3. V1 V2 V3 Sr1 Sr2 Sr3 Sr4 Sr5 expected F F F F F F F F F F ; ; F F F F F F O * 2 O * 2 O * 2 O O O expected Note: (*) adding a bond valence of 1.6 units, corresponding to the two H atoms linked to O1, O2 and O3, forming water molecules. The valence deficit observed on O4, O5 and O6, as well as on F4, F7, F13 and F16, is expected to be compensated by hydrogen bonding, since they behave as acceptors. Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: i46 Le Bail et al. doi: /s Acta Cryst. (2009). E65, i46 i47

3 inorganic compounds DIAMOND (Brandenburg, 1999) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: publcif (Westrip, 2009). Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2236). References Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Brese, N. E. & O Keeffe, M. (1991). Acta Cryst. B47, Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, Bruker (2003). APEX, SAINT and TWINABS. Bruker AXS Inc., Madison, Wisconsin, USA. Crosnier-Lopez, M. P., Duroy, H. & Fourquet, J. L. (1994). Z. Anorg. Allg. Chem. 620, Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Le Bail, A. (1996). Eur. J. Solid State Inorg. Chem. 33, Le Meins, J.-M., Hemon-Ribaud, A. & Courbion, G. (1997). Acta Cryst. C53, Sheldrick, G. M. (2008). Acta Cryst. A64, Westrip, S. P. (2009). publcif. In preparation. Acta Cryst. (2009). E65, i46 i47 Le Bail et al. Sr 5 (VOF 5 ) 3 F(H 2 O) 3 i47

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= mm 1 T = 298 K. Data collection. Refinement. R[F 2 >2(F 2 )] = wr(f 2 ) = S = reflections 290 parameters 9 restraints

= mm 1 T = 298 K. Data collection. Refinement. R[F 2 >2(F 2 )] = wr(f 2 ) = S = reflections 290 parameters 9 restraints inorganic compounds Acta Crystallographica Section E Structure Reports Online ISSN 1600-5368 Sr 5 (V IV OF 5 ) 3 F(H 2 O) 3 refined from a non-merohedrally twinned crystal Armel Le Bail, a * Anne-Marie

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