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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 [sigma](C-C) = 0.005 Å
Some non-H atoms missing,
R = 0.032
wR = 0.082
Data-to-parameter ratio = 18.2
Details
Open access

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

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[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]). Acta Cryst. D65, 148-155].

Related literature

For other dirhodium complex structures, see CCDC Refcode QAFHEM: Dzik et al. (2010[Dzik, W. I., Creusen, C., de Gelder, R., Peters, T. P. J., Smits, J. M. M. & de Bruin, B. (2010). Organometallics, 29, 1629-1641.]), YOSMEZ: Okazaki et al. (2009[Okazaki, M., Hayashi, A., Fu, C. F., Liu, S. T. & Ozawa, F. (2009). Organometallics, 28, 902-908.]), DEFJII: Douglas et al. (2005[Douglas, S., Lowe, J. P., Mahon, M. F., Warren, J. E. & Whittlesey, M. K. (2005). J. Organomet. Chem. 690, 5027-5035.]), TPCDRH10: Singh et al. (1973[Singh, P., Dammann, C. B. & Hodgson, D. J. (1973). Inorg. Chem. 12, 1335-1339.]). For a description of the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]). For the use of SQUEEZE, see: Spek (2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).

[Scheme 1]

Experimental

Crystal data
  • [Rh2(C18H15P)4(CO)2]·2C3H6O

  • Mr = 1427.16

  • Monoclinic, C 2/c

  • a = 23.535 (3) Å

  • b = 13.0758 (11) Å

  • c = 24.650 (2) Å

  • [beta] = 115.67 (2)°

  • V = 6837.1 (16) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.63 mm-1

  • T = 298 K

  • 0.38 × 0.38 × 0.23 mm

Data collection
  • Enraf-Nonius CAD-4 diffractometer

  • Absorption correction: [psi] scan (North et al., 1968[North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.]) Tmin = 0.797, Tmax = 0.869

  • 6874 measured reflections

  • 6718 independent reflections

  • 5170 reflections with I > 2[sigma](I)

  • Rint = 0.026

  • 3 standard reflections every 3 reflections intensity decay: 4.0%

Refinement
  • R[F2 > 2[sigma](F2)] = 0.032

  • wR(F2) = 0.082

  • S = 1.03

  • 6718 reflections

  • 370 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.39 e Å-3

  • [Delta][rho]min = -0.27 e Å-3

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994[Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.]); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995[Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.]); program(s) used to solve structure: SIR2002 (Burla et al., 2003[Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and SQUEEZE in PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).


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.  [ISI] [CrossRef] [details]
Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103.  [CrossRef] [details]
Douglas, S., Lowe, J. P., Mahon, M. F., Warren, J. E. & Whittlesey, M. K. (2005). J. Organomet. Chem. 690, 5027-5035.  [CSD] [CrossRef] [ChemPort]
Dzik, W. I., Creusen, C., de Gelder, R., Peters, T. P. J., Smits, J. M. M. & de Bruin, B. (2010). Organometallics, 29, 1629-1641.  [CSD] [CrossRef] [ChemPort]
Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
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.  [CrossRef] [details]
Okazaki, M., Hayashi, A., Fu, C. F., Liu, S. T. & Ozawa, F. (2009). Organometallics, 28, 902-908.  [CSD] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Singh, P., Dammann, C. B. & Hodgson, D. J. (1973). Inorg. Chem. 12, 1335-1339.  [CrossRef] [ChemPort] [ISI]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [ISI] [CrossRef] [details]


Acta Cryst (2012). E68, m1408-m1409   [ doi:10.1107/S1600536812043528 ]

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