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Volume 69 
Part 1 
Page m14  
January 2013  

Received 26 October 2012
Accepted 29 November 2012
Online 5 December 2012

Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.004 Å
Some non-H atoms missing,
Disorder in solvent or counterion
R = 0.053
wR = 0.152
Data-to-parameter ratio = 23.1
Details
Open access

Carbonyl{3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-bis[(4,4,5,5-tetramethyl-1,3,2-dioxaphospholan-2-yl)oxy]biphenyl-[kappa]2P,P'}hydrido(triphenylphosphane-[kappa]P)rhodium(I) diethyl ether trisolvate

aLeibniz-Institut für Katalyse e. V. an der Universität Rostock, Albert-Einstein-Strasse 29a, 18059 Rostock, Germany
Correspondence e-mail: detlef.selent@catalysis.de

In the title compound, [RhH(C74H68O8P2)(C18H15P)(CO)]·3C4H10O, the CHP3 coordination set at the RhI ion is arranged in a distorted trigonal-bipyramidal geometry with the P atoms adopting equatorial coordination sites and the C atom of the carbonyl ligand as well as the H atom adopting the axial sites. The asymmetric unit contains two very similar molecules of the rhodium complex, two half-occupied diethyl ether molecules and further diethyl ether solvent molecules which could not be modelled successfully. Therefore contributions of the latter were removed from the diffraction data using the SQUEEZE procedure in PLATON [Spek (2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]). Acta Cryst. D65, 148-155].

Related literature

For the solid-state structure and for DFT calculations of the dicarbonyl precursor of the title compound, see: Selent et al. (2011[Selent, D., Franke, R., Kubis, C., Spannenberg, A., Baumann, W., Kreidler, B. & Börner, A. (2011). Organometallics, 30, 4509-4514.], 2012[Selent, D., Spannenberg, A. & Börner, A. (2012). Acta Cryst. E68, m488.]). For the crystal structure of another diphosphite hydrido complex of rhodium(I), see: van Rooy et al. (1995[Rooy, A. van, Kamer, P. C. J., van Leeuwen, P. W. N. M., Veldman, N. & Spek, A. L. (1995). J. Organomet. Chem. 494, C15-C18.], 1996[Rooy, A. van, Kamer, P. C. J., van Leeuwen, P. W. N. M., Goubitz, K., Fraanje, J., Veldman, N. & Spek, A. L. (1996). Organometallics, 15, 835-847.]). An octahedral RhIII hydrido complex with both diphosphite and triphenylphosphane ligands adopting coordination sites in the same plane has been characterized structurally, see: Rubio et al. (2009[Rubio, M., Suárez, A., del Rio, D., Galindo, A., Álvarez, E. & Pizzano, A. (2009). Organometallics, 28, 547-560.]).

[Scheme 1]

Experimental

Crystal data
  • [RhH(C74H68O8P2)(C18H15P)(CO)]·3C4H10O

  • Mr = 1763.78

  • Triclinic, [P \overline 1]

  • a = 21.1611 (4) Å

  • b = 22.1298 (4) Å

  • c = 22.6020 (4) Å

  • [alpha] = 112.345 (1)°

  • [beta] = 101.135 (1)°

  • [gamma] = 96.757 (1)°

  • V = 9389.9 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.29 mm-1

  • T = 150 K

  • 0.44 × 0.39 × 0.18 mm

Data collection
  • Bruker Kappa APEXII DUO diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.94, Tmax = 1.00

  • 388867 measured reflections

  • 43155 independent reflections

  • 32017 reflections with I > 2[sigma](I)

  • Rint = 0.073

Refinement
  • R[F2 > 2[sigma](F2)] = 0.053

  • wR(F2) = 0.152

  • S = 1.05

  • 43155 reflections

  • 1866 parameters

  • 55 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 1.43 e Å-3

  • [Delta][rho]min = -0.99 e Å-3

Data collection: APEX2 (Bruker, 2011[Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2697 ).


References

Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2009). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Rooy, A. van, Kamer, P. C. J., van Leeuwen, P. W. N. M., Goubitz, K., Fraanje, J., Veldman, N. & Spek, A. L. (1996). Organometallics, 15, 835-847.
Rooy, A. van, Kamer, P. C. J., van Leeuwen, P. W. N. M., Veldman, N. & Spek, A. L. (1995). J. Organomet. Chem. 494, C15-C18.  [CrossRef]
Rubio, M., Suárez, A., del Rio, D., Galindo, A., Álvarez, E. & Pizzano, A. (2009). Organometallics, 28, 547-560.  [CSD] [CrossRef] [ChemPort]
Selent, D., Franke, R., Kubis, C., Spannenberg, A., Baumann, W., Kreidler, B. & Börner, A. (2011). Organometallics, 30, 4509-4514.  [CSD] [CrossRef] [ChemPort]
Selent, D., Spannenberg, A. & Börner, A. (2012). Acta Cryst. E68, m488.  [CSD] [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [ISI] [CrossRef] [details]


Acta Cryst (2013). E69, m14  [ doi:10.1107/S1600536812049124 ]

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