(IUCr) Chloridotris[tris(4-fluorophenyl)phosphine]rhodium(I) methanol solvate

Volume 64
Part 4
Pages m512-m513
April 2008

Received 15 January 2008
Accepted 26 February 2008
Online 5 March 2008

Key indicators
Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.009 Å
Disorder in main residue
R = 0.034
wR = 0.075
Data-to-parameter ratio = 8.9
Details

Chloridotris[tris(4-fluorophenyl)phosphine]rhodium(I) methanol solvate

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

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

In the title compound, [RhCl{P(p-FC₆H₄)₃}₃]·CH₃OH, the Rh atom adopts a distorted square-planar geometry. Rh, Cl and one P atom lie on a mirror plane, as does the solvent molecule. There are two intermolecular hydrogen bonds, one between the methanol O atom and an aryl H atom (2.51 Å), and one between the Cl atom and the hydroxy H atom of methanol [2.34 (3) Å]. The complex precipitates in trace amounts from a reaction between RhCl(cod)(thp) [cod is 1,5-cyclooctadiene and thp is tris(hydroxymethyl)phosphine] and P(p-FC₆H₄)₃ under argon in CD₃OD. Two C₆H₄-F units are disordered over two positions; for one the site occupancy factors are ca. 0.53 and 0.47, for the other the values are ca. 0.64 and 0.36. The methyl H atoms of the solvent molecule are disordered across the mirror plane.

Related literature

For related literature, see: Beck et al. (1999) and references therein; Bennett & Donaldson (1977); Bennett et al. (1971); Evans et al. (1999); Higham et al. (2004); Hoye et al. (1993); Jones et al. (1980); Lorenzini et al. (2007a,b,c, 2008a,b); Montelatici et al. (1968); Young et al. (1965).

Experimental

Crystal data

[RhCl(C₁₈H₁₂F₃P)₃]·CH₄O
M_r = 1119.14
Monoclinic, C m
a = 10.831 (3) Å
b = 23.724 (7) Å
c = 9.845 (3) Å
= 108.213 (8)°
V = 2403.0 (12) Å³
Z = 2
Mo K radiation
= 0.59 mm^-1
T = 173.0 (1) K
0.30 × 0.15 × 0.03 mm

Data collection

Bruker X8 APEXII diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2003) T_min = 0.544, T_max = 0.983
10921 measured reflections
3312 independent reflections
3094 reflections with I > 2(I)
R_int = 0.048

Refinement

R[F² > 2(F²)] = 0.034
wR(F²) = 0.075
S = 1.03
3312 reflections
372 parameters
15 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.67 e Å^-3
_min = -0.47 e Å^-3
Absolute structure: Flack (1983), 812 Friedel pairs
Flack parameter: -0.03 (3)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C3-H3O1ⁱ	0.95	2.51	3.458 (9)	172
O1-H1OCl1ⁱⁱ	1.03 (5)	2.34 (5)	3.369 (9)	174 (11)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z-1.

Data collection: SAINT (Bruker, 2003); cell refinement: SAINT; data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (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: RK2075 ).

Acknowledgements

The authors 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.
Bennett, M. J. & Donaldson, P. B. (1977). Inorg. Chem. 16, 655-660.
Bennett, M. A., Robertson, G. B., Turney, T. W. & Whimp, P. O. (1971). J. Chem. Soc. D, pp. 762-764.
Bruker (2003). SADABS. and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Evans, P. A., Incarvito, C. D. & Rheingold, A. L. (1999). Private communication (deposition number: 115178). CCDC, Cambridge, England.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
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.
Jones, R. A., Real, F. M., Wilkinson, G., Galas, A. M. R., Hursthouse, M. B. & Malik, K. M. A. (1980). J. Chem. Soc. Dalton Trans. pp. 511-518.
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. (2007c). Inorg. Chim. Acta, doi:10.1016/j.ica.2007.10.044.
Lorenzini, F., Patrick, B. O. & James, B. R. (2008a). Acta Cryst. E64, m179-m180.
Lorenzini, F., Patrick, B. O. & James, B. R. (2008b). Acta Cryst. E64, m464-m465.
Montelatici, S., van der Ent, A., Osborn, J. A. & Wilkinson, G. (1968). J. Chem. Soc. A, pp. 1054-1058.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Young, J. F., Osborn, J. A., Jardine, F. H. & Wilkinson, G. (1965). Chem. Commun. pp. 131-132.

metal-organic compounds