Tris[2-(deuteriomethyl­sulfan­yl)­phen­yl]­phosphine deuteriochloro­form 0.125-solvate

Wong, R.C.S.; Ooi, M.L.; Sakurai, H.; Ng, S.W.

doi:10.1107/S1600536808010817

Volume 64
Part 5
Page o898
May 2008

Received 28 February 2008
Accepted 18 April 2008
Online 23 April 2008

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.006 Å
Some non-H atoms missing,
Disorder in main residue
R = 0.062
wR = 0.194
Data-to-parameter ratio = 18.0
Details

Tris[2-(deuteriomethylsulfanyl)phenyl]phosphine deuteriochloroform 0.125-solvate

Richard Chee Seng Wong,^a Mei Lee Ooi,^a Hidehiro Sakurai ^b and Seik Weng Ng ^a ^*

^aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and ^bResearch Center for Molecular Nanoscience, Institute for Molecular Science, Myodaiji, Okazaki 444-8787, Japan
Correspondence e-mail: seikweng@um.edu.my

The title deuterated tripodal phosphine, C₂₁H₁₂D₉PS₃·0.125CDCl₃, crystallizes as two independent molecules, one of which lies on a general position and the other about a threefold rotation axis, and as a deuteriochloroform solvate. The solvent molecule is disordered about a site of symmetry 3, so that the ratio of phosphine to solvent is 8:1. The P atom adopts a pyramidal coordination geometry.

Related literature

For the synthesis and crystal structure of tris[(2-methylsulfanyl)phenyl]phosphine, see: Meek et al. (1976); Uttecht et al. (2005).

Experimental

Crystal data

C₂₁H₁₂D₉PS₃·0.125CDCl₃
M_r = 424.63
Hexagonal, $[R \overline 3]$
a = 23.090 (1) Å
c = 25.144 (1) Å
V = 11610 (1) Å³
Z = 24
Mo K radiation
= 0.52 mm^-1
T = 100 (2) K
0.20 × 0.15 × 0.10 mm

Data collection

Bruker SMART APEX diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.925, T_max = 1.000 (expected range = 0.878-0.949)
36814 measured reflections
5929 independent reflections
4200 reflections with I > 2(I)
R_int = 0.089

Refinement

R[F² > 2(F²)] = 0.062
wR(F²) = 0.194
S = 1.18
5929 reflections
329 parameters
12 restraints
H-atom parameters constrained
_max = 1.14 e Å^-3
_min = -0.49 e Å^-3

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, 2008).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2251 ).

Acknowledgements

We thank the ScienceFund MOSTI (03-01-03-SF0209) for funding the study, and the University of Malaya for the purchase of the diffractometer.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Meek, D. W., Dyer, G. & Workman, M. O. (1976). Inorg. Synth. 16, 168-174.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Uttecht, J.-G., Tuczek, F. & Näther, C. (2005). Acta Cryst. E61, o2916-o2917.
Westrip, S. P. (2008). publCIF. In preparation.

organic compounds