Trimethyl­sulfonium 1-amino-6-fluoro-2,3,4,5,7,8,9,10,11,12-decaiodo-1-carba-closo-dodeca­borate

Finze, M.; Reiss, G.J.

doi:10.1107/S1600536812004424

Volume 68
Part 3
Page o640
March 2012

Received 26 January 2012
Accepted 2 February 2012
Online 10 February 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (B-B) = 0.008 Å
R = 0.024
wR = 0.052
Data-to-parameter ratio = 20.8
Details

Trimethylsulfonium 1-amino-6-fluoro-2,3,4,5,7,8,9,10,11,12-decaiodo-1-carba-closo-dodecaborate

Maik Finze ^a ^* and Guido J. Reiss ^b

^aInstitut für Anorganische Chemie, Julius-Maximilians-Universität Würzburg, Am Hubland, D-97074 Würzburg, Germany, and ^bInstitut für Anorganische Chemie und Strukturchemie, Lehrstuhl II: Material- und Strukturforschung, Heinrich-Heine-Universität Düsseldorf, Universitätsstrasse 1, D-40225 Düsseldorf, Germany
Correspondence e-mail: maik.finze@uni-wuerzburg.de

In the asymmetric unit of the title salt, C₃H₉S⁺·CH₂B₁₁FI₁₀N^- or (CH₃)₃S[1-H₂N-6-F-closo-1-CB₁₁I₁₀], both ions lie in general positions. The anion is perfectly ordered and so the positions of the C-NH₂ vertex and the fluorine substituent are clearly assigned. The relatively short C-N bond length may be interpreted in terms of a very electron deficient {closo-1-CB₁₁} cluster.

Related literature

For a general overview on monocarba-closo-dodecaborates, see: Körbe et al. (2006). For the synthesis and properties of 1-aminomonocarba-closo-dodecaboron clusters, see: Jelínek et al. (1986); Srivastava et al. (1996); Finze (2007, 2009); Finze et al. (2007); Finze & Sprenger (2010). For studies on the proton affinity of halogenated {closo-1-CB₁₁} clusters, see: Himmelspach et al. (2011, 2012). For the formation of (CH₃)₃S⁺ from dimethyl sulfoxide, see: Nifontova & Lavrentiev (1993); Forrester et al. (1995); Park et al. (2005). For the structure of (CH₃)₃SBr, see: Svensson & Kloo (1996).

Experimental

Crystal data

C₃H₉S⁺·CH₂B₁₁FI₁₀N^-
M_r = 1512.11
Monoclinic, P 2₁ /n
a = 10.0672 (1) Å
b = 16.7057 (2) Å
c = 17.5574 (2) Å
= 93.175 (1)°
V = 2948.26 (6) Å³
Z = 4
Mo K radiation
= 10.59 mm^-1
T = 100 K
0.79 × 0.28 × 0.20 mm

Data collection

Oxford Diffraction Xcalibur Eos diffractometer
Absorption correction: analytical [CrysAlis PRO (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, Oxfordshire, England.]$ ), based on expressions derived by Clark & Reid (1995)] T_min = 0.040, T_max = 0.204
30584 measured reflections
5482 independent reflections
5282 reflections with I > 2(I)
R_int = 0.029

Refinement

R[F² > 2(F²)] = 0.024
wR(F²) = 0.052
S = 1.31
5482 reflections
264 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 1.06 e Å^-3
_min = -0.61 e Å^-3

Data collection: CrysAlis PRO (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, Oxfordshire, England.]$ ); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2011); software used to prepare material for publication: publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RU2027 ).

Acknowledgements

The financial support of the Deutsche Forschungsgemeinschaft (FI 1628/2-1) is gratefully acknowledged.

References

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organic compounds