(IUCr) trans-Carbonylchloridobis(tri-p-tolylphosphine)rhodium(I) acetone solvate

Volume 64
Part 3
Pages m464-m465
March 2008

Received 14 December 2007
Accepted 31 January 2008
Online 8 February 2008

Key indicators
Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.006 Å
R = 0.048
wR = 0.115
Data-to-parameter ratio = 20.8
Details

trans-Carbonylchloridobis(tri-p-tolylphosphine)rhodium(I) acetone solvate

Fabio Lorenzini,^a ^* Brian O. Patrick ^a and Brian R. James ^a

^aDepartment of Chemistry, University of British Columbia, 2036 Main Mall, Vancouver, BC, Canada V6T 1Z1
Correspondence e-mail: brj@chem.ubc.ca

The title compound, [RhCl(C₂₁H₂₁P)₂(CO)]·C₃H₆O, was precipitated in trace yield from a reaction of RhCl(cod)(THP) with P(p-tol)₃ in a 1:1 acetone-d₆/CD₃OD solution under a hydrogen atmosphere [p-tol = p-tolyl, THP = tris(hydroxymethyl)phosphine, P(CH₂OH)₃, and cod = 1,5-cyclooctadiene]. The complex displays a square-planar geometry around the Rh^I atom. The complex molecules and the acetone molecules are linked into a chain along the a axis by intermolecular C-HCl and C-HO hydrogen bonds.

Related literature

For related literature, see: Beck et al. (1999, and references therein); Evans et al. (1990); Higham et al. (2004); Hoye et al. (1993); Lorenzini et al. (2007a,b, 2008a,b); Vallarino (1957).

Experimental

Crystal data

[RhCl(C₂₁H₂₁P)₂(CO)]·C₃H₆O
M_r = 833.14
Triclinic, $[P \overline 1]$
a = 10.784 (2) Å
b = 12.859 (3) Å
c = 17.086 (3) Å
= 70.852 (7)°
= 84.790 (7)°
= 71.012 (6)°
V = 2116.2 (7) Å³
Z = 2
Mo K radiation
= 0.58 mm^-1
T = 173 (2) K
0.25 × 0.10 × 0.07 mm

Data collection

Bruker X8 APEXII diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2003) T_min = 0.683, T_max = 0.960
31662 measured reflections
9909 independent reflections
6378 reflections with I > 2(I)
R_int = 0.063

Refinement

R[F² > 2(F²)] = 0.047
wR(F²) = 0.115
S = 1.00
9909 reflections
477 parameters
H-atom parameters constrained
_max = 0.48 e Å^-3
_min = -0.44 e Å^-3

Table 1
Selected geometric parameters (Å, °)

C43-Rh1	1.812 (4)
P1-Rh1	2.3449 (9)
P2-Rh1	2.3283 (9)
Cl1-Rh1	2.3822 (9)

C43-Rh1-P2	91.43 (10)
C43-Rh1-P1	90.55 (10)
P2-Rh1-P1	177.46 (3)
C43-Rh1-Cl1	178.12 (10)
P2-Rh1-Cl1	86.69 (3)
P1-Rh1-Cl1	91.33 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C10-H10O2ⁱ	0.95	2.38	3.302 (8)	163
C46-H46ACl1	0.98	2.81	3.773 (7)	168
Symmetry code: (i) x+1, y, z.

Data collection: APEX2 (Bruker, 2006); cell refinement: APEX2; data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CI2547 ).

Acknowledgements

We thank the Natural Sciences and Engineering Research Council of Canada for financial support via a Discovery Grant.

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.
Beck, C. M., Rathmill, S. E., Park, Y. J., Chen, J., Crabtree, R. H., Liable-Sands, L. M. & Rheingold, A. L. (1999). Organometallics, 18, 5311-5317.
Bruker (2003). SADABS. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2005). SAINT. Version 7.23. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2006). APEX2. Version 2.10. Bruker AXS Inc., Madison, Wisconsin, USA.
Evans, D., Osborn, J. A. & Wilkinson, G. (1990). Inorg. Synth. 28, 79-80.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Higham, L. J., Whittlesey, M. K. & Wood, P. T. (2004). J. Chem. Soc. Dalton Trans. pp. 4202-4208.
Hoye, P. A. T., Pringle, P. G., Smith, M. B. & Worboys, K. (1993). J. Chem. Soc. Dalton Trans. pp. 269-274.
Lorenzini, F., Patrick, B. O. & James, B. R. (2007a). J. Chem. Soc. Dalton Trans. pp. 3224-3226.
Lorenzini, F., Patrick, B. O. & James, B. R. (2007b). Inorg. Chem. 46, 8998-9002.
Lorenzini, F., Patrick, B. O. & James, B. R. (2008a). Inorg. Chim. Acta, doi: 10.1016/j.ica.2007.10.044.
Lorenzini, F., Patrick, B. O. & James, B. R. (2008b). Acta Cryst. E64, m179-m180.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Vallarino, L. (1957). J. Chem. Soc. pp. 2287-2292.

metal-organic compounds