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-κ2P,P′}hydrido(triphenyl­phosphane-κP)rhodium(I) diethyl ether tris­olvate

Selent, D.; Spannenberg, A.; Börner, A.

doi:10.1107/S1600536812049124

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 (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

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-²P,P'}hydrido(triphenylphosphane-P)rhodium(I) diethyl ether trisolvate

Detlef Selent,^a ^* Anke Spannenberg ^a and Armin Börner ^a

^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 Rh^I 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). 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, 2012). For the crystal structure of another diphosphite hydrido complex of rhodium(I), see: van Rooy et al. (1995, 1996). An octahedral Rh^III hydrido complex with both diphosphite and triphenylphosphane ligands adopting coordination sites in the same plane has been characterized structurally, see: Rubio et al. (2009).

Experimental

Crystal data

[RhH(C₇₄H₆₈O₈P₂)(C₁₈H₁₅P)(CO)]·3C₄H₁₀O
M_r = 1763.78
Triclinic, $[P \overline 1]$
a = 21.1611 (4) Å
b = 22.1298 (4) Å
c = 22.6020 (4) Å
= 112.345 (1)°
= 101.135 (1)°
= 96.757 (1)°
V = 9389.9 (3) Å³
Z = 4
Mo K radiation
= 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) T_min = 0.94, T_max = 1.00
388867 measured reflections
43155 independent reflections
32017 reflections with I > 2(I)
R_int = 0.073

Refinement

R[F² > 2(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
_max = 1.43 e Å^-3
_min = -0.99 e Å^-3

Data collection: APEX2 (Bruker, 2011); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); 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.
Rubio, M., Suárez, A., del Rio, D., Galindo, A., Álvarez, E. & Pizzano, A. (2009). Organometallics, 28, 547-560.
Selent, D., Franke, R., Kubis, C., Spannenberg, A., Baumann, W., Kreidler, B. & Börner, A. (2011). Organometallics, 30, 4509-4514.
Selent, D., Spannenberg, A. & Börner, A. (2012). Acta Cryst. E68, m488.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.

metal-organic compounds

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-2P,P'}hydrido(triphenylphosphane-P)rhodium(I) diethyl ether trisolvate