Di-μ-carbonyl-bis­[bis­(triphenyl­phos­phane)rhodium(0)](Rh—Rh) acetone disolvateCAS 47921–72–2, 48246–55–5.

Gueorguieva, P.G.; Laneman, S.A.; Stanley, G.G.; Fronczek, F.R.; Watkins, S.F.

doi:10.1107/S1600536812043528

Volume 68
Part 11
Pages m1408-m1409
November 2012

Received 1 October 2012
Accepted 19 October 2012
Online 27 October 2012

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.005 Å
Some non-H atoms missing,
R = 0.032
wR = 0.082
Data-to-parameter ratio = 18.2
Details

Di--carbonyl-bis[bis(triphenylphosphane)rhodium(0)](Rh-Rh) acetone disolvate¹

Petia G. Gueorguieva,^a ⁺ Scott A. Laneman,^a ⁺⁺ George G. Stanley,^a Frank R. Fronczek ^a ^* and Steven F. Watkins ^a

^aDepartment of Chemistry, Louisiana State University, Baton Rouge, LA 70803-1804, USA
Correspondence e-mail: ffroncz@lsu.edu

The dirhodium complex, [Rh₂(C₁₈H₁₅P)₄(CO)₂]·2(CH₃)₂CO, has crystallographic twofold symmetry and the Rh-Rh distance is 2.6266 (8) Å. The four atoms proximate to each Rh atom [Rh-P = 2.3222 (7) and 2.3283 (8) Å, and Rh-C = 1.961 (3) and 2.045 (3) Å] form a distorted tetrahedron with large deviations from the putative tetrahedral angles [r.m.s. deviation = 23 (1)°]. The six angles more closely approximate those of a trigonal bipyramid [r.m.s. deviation = 14 (1)°] with one missing equatorial ligand. The two bridging carbonyl ligands are much more linearly coordinated to one Rh [Rh-C [triple bond] O = 151.0 (2)°] than to the other [127.0 (2)°], and the two Rh₂CO planes form a dihedral angle of 45.43 (5)°. The two acetone solvent molecules are disordered, and their estimated scattering contribution was subtracted from the observed diffraction data using the SQUEEZE routine in PLATON [Spek (2009). Acta Cryst. D65, 148-155].

Related literature

For other dirhodium complex structures, see CCDC Refcode QAFHEM: Dzik et al. (2010), YOSMEZ: Okazaki et al. (2009), DEFJII: Douglas et al. (2005), TPCDRH10: Singh et al. (1973). For a description of the Cambridge Structural Database, see: Allen (2002). For the use of SQUEEZE, see: Spek (2009).

Experimental

Crystal data

[Rh₂(C₁₈H₁₅P)₄(CO)₂]·2C₃H₆O
M_r = 1427.16
Monoclinic, C 2/c
a = 23.535 (3) Å
b = 13.0758 (11) Å
c = 24.650 (2) Å
= 115.67 (2)°
V = 6837.1 (16) Å³
Z = 4
Mo K radiation
= 0.63 mm^-1
T = 298 K
0.38 × 0.38 × 0.23 mm

Data collection

Enraf-Nonius CAD-4 diffractometer
Absorption correction: scan (North et al., 1968) T_min = 0.797, T_max = 0.869
6874 measured reflections
6718 independent reflections
5170 reflections with I > 2(I)
R_int = 0.026
3 standard reflections every 3 reflections intensity decay: 4.0%

Refinement

R[F² > 2(F²)] = 0.032
wR(F²) = 0.082
S = 1.03
6718 reflections
370 parameters
H-atom parameters constrained
_max = 0.39 e Å^-3
_min = -0.27 e Å^-3

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) and SQUEEZE in PLATON (Spek, 2009); 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: LH5542 ).

Acknowledgements

The purchase of the diffractometer was made possible by a National Science Foundation chemical instrumentation grant, which we gratefully acknowledge. Improvements to the LSU X-ray Crystallography Facility were supported by grant No. LEQSF(1196-97)-ENH-TR-10, administered by the Louisiana Board of Regents.

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.
Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103.
Douglas, S., Lowe, J. P., Mahon, M. F., Warren, J. E. & Whittlesey, M. K. (2005). J. Organomet. Chem. 690, 5027-5035.
Dzik, W. I., Creusen, C., de Gelder, R., Peters, T. P. J., Smits, J. M. M. & de Bruin, B. (2010). Organometallics, 29, 1629-1641.
Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.
Okazaki, M., Hayashi, A., Fu, C. F., Liu, S. T. & Ozawa, F. (2009). Organometallics, 28, 902-908.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Singh, P., Dammann, C. B. & Hodgson, D. J. (1973). Inorg. Chem. 12, 1335-1339.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.