Low-temperature redetermination of tribenzyl­chloridotin(IV)

Ng, S.W.

doi:10.1107/S160053680900289X

Volume 65
Part 2
Page m238
February 2009

Received 20 January 2009
Accepted 23 January 2009
Online 28 January 2009

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.005 Å
R = 0.026
wR = 0.074
Data-to-parameter ratio = 19.7
Details

Low-temperature redetermination of tribenzylchloridotin(IV)

Seik Weng Ng ^a ^*

^aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Correspondence e-mail: seikweng@um.edu.my

Compared to the previous studies [Ng (1997). Acta Cryst. C53, 56-58; Yin et al. (2005). Huaxue Shiji, 27, 295-296], the redetermined structure of the title compound, [Sn(C₇H₇)₃Cl], exhibits a doubled c unit-cell parameter. There are two molecules in the asymmetric unit, with both Sn and both Cl atoms having 3 site symmetry. The Sn atoms have distorted SnClC₃ tetrahedral geometries and the molecules interact by way of short SnCl bridges [SnCl = 3.418 (2) and 3.475 (2) Å], thereby forming chains propagating in c.

Related literature

For the room-temperature structure of the title compound described in the R3 space group but with the unique c axis half as long, see: Ng (1997); Yin et al. (2005). For the direct synthesis of the title compound from metallic tin and benzyl chloride, see: Sisido et al. (1961).

Experimental

Crystal data

[Sn(C₇H₇)₃Cl]
M_r = 427.52
Trigonal, R 3
a = 16.7985 (2) Å
c = 11.6875 (2) Å
V = 2856.23 (6) Å³
Z = 6
Mo K radiation
= 1.48 mm^-1
T = 100 (2) K
0.40 × 0.08 × 0.06 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.589, T_max = 0.917
9077 measured reflections
2737 independent reflections
2431 reflections with I > 2(I)
R_int = 0.014

Refinement

R[F² > 2(F²)] = 0.026
wR(F²) = 0.074
S = 1.07
2737 reflections
139 parameters
1 restraint
H-atom parameters constrained
_max = 0.53 e Å^-3
_min = -0.25 e Å^-3
Absolute structure: Flack (1983), 1372 Friedel pairs
Flack parameter: -0.01 (4)

Table 1
Selected bond lengths (Å)

Sn1-C1	2.146 (3)
Sn1-Cl1	2.392 (2)
Sn2-C8	2.143 (3)
Sn2-Cl2	2.403 (2)

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); 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: HB2901 ).

Acknowledgements

The author thanks the University of Malaya for supporting this study.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Ng, S. W. (1997). Acta Cryst. C53, 56-58.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Sisido, K., Takeda, Y. & Kinugawa, Z. (1961). J. Am. Chem. Soc. 83, 538-541.
Westrip, S. P. (2009). publCIF. In preparation.
Yin, H.-D., Li, K.-Z. & Hong, M. (2005). Huaxue Shiji, 27, 295-296, 310.

metal-organic compounds