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Ζ. Kristallogr. NCS 216 (2001)© by Oldenbourg Wissenschaftsverlag, München
Refinement of the crystal structure of diammonium hexafluoro- stannate(IV), (NH^SnFi
G . Meyer* and N. Böhmer
Universität zu Köln, Institut für Anorganische Chemie, Greinstraße 6. D-50939 Köln, Germany Received July 14, 2000, CSD-No. 409509
Abstract
FeHgNiSn, trigonal, P3ml (No. 164), a = 6.081(1) Ä, c = 4.865(1) A, V = 155.8 A3, Ζ = 1 , ^ , ( ^ = 0.029, wRKf(F2) = 0.068, Τ = 293 Κ.
Source of material
Colorless single crystals of ( N H ^ S n F ö were obtained during the reaction of the Zintl phase KSn with NH4F in a sealed copper ampoule at 623 K.
Discussion
The crystal structure of ( N R t h S n F ö was originally determined by Davidovich and Kaidalova (1971) [ 1 ] via Rietveld refinement.
T h e structure is n o w d e t e r m i n e d f r o m single crystal data.
( N H 4 h S n F 6 c r y s t a l l i z e s i s o t y p i c to ( N H ^ G e F ö [2] and (NH4)2PbFö [3]. T h e crystal structure contains isolated [SnF6]2~ octahedra (</(Sn—F) = 1.955(4) A) and N H4 + ions.
Table 1. Data collection and handling.
Crystal: colorless, irregular.
size 0.1 χ 0.1 χ 0.1 mm Wavelength: Mo Ka radiation (0.71073 A)
μ: 41.48 cm-1
Diffractometer, scan mode: Stoe-IPDS, φ
29ma*: 49.84°
W/ltOmeasurcd, N(hkl)miqm: 1120,123 Criterion for /0bs, N(hkl)g,: /obs > 2 af/0bsA 122 N(param) refined: 17
Programs: SHELXS-97 [4], SHELXL-97 [5], DIAMOND [6]
Table 2. Atomic coordinates and displacement parameters (in A2).
Atom Site X Ζ V\so
H(l) 61 -0.275(8) 2x 0.49(2) 0.05(3)
H(2) 2d 2/3 1/3 0.10(6) 0.1(1)
Table 3. Atomic coordinates and displacement parameters (in A2).
Atom Site U11 U22 I/33 f/12 Uii Un
Sn F Ν
Ια 6ι 2d
0 0 0 0.0158(5) U11 0.1545(4) 2x 0.2228(9) 0.043(2) 0.027(2) 2/3 1/3 0.315(3) 0.024(3) Un
0.0234(6) t/n/2 0.044(2) 0.014(1) 0.042(6) i/n/2
0 -0.0069(9)
0
0 2Um 0
Acknowledgment. We are grateful to the Deutsche Forschungsgemeinschaft, Bonn, for financial support.
References
1. Davidovich, R. L.; Kaidalova, Τ. Α.: Ammonium Hexafluorostannate and Hexafluoroplumbate. Russ. J. Inorg. Chem.16 (1971) 1354.
2. Hoard, J. L.; Vincent, W. B.: Structures of Complex Fluorides. Potassium Hexafluorogermanate and Ammonium Hexafluorogermanate. J. Am.
Chem. Soc. 61 (1939) 2849-2852.
3. Reusch, U.: In situ-Beobachtungen von Reaktionen des Ammoniaks mit Ammonium-Fluoro-Komplexen des Zinns und Bleis. Dissertation.
Universität Tübingen, Germany 1999.
4. Sheldrick, G. M.: SHELXS-97-2, Program for the Solution of Crystal Structures. University of Göttingen, Germany 1997.
5. Sheldrick, G. M.: SHELXL-97-2, Program for Crystal Structure Refine- ment. University of Göttingen, Germany 1997.
6. Brandenburg, K.: Diamond (Version 2.1a). Crystal Impact GbR, Ger- many 1996-1999.
* Correspondence author (e-mail: gerd.meyer@uni-koeln.de)
