cis-Dichlorido[2,3-dimethyl-3-(4,4,5,5-tetra­methyl-1,3,2λ5-dioxaphospho­lan-2-yl­oxy)butan-2-olato-κ2O,P]oxido(triphenyl­phosphane-κP)rhenium(V)

Skarżyńska, A.; Siczek, M.; Gniewek, A.

doi:10.1107/S1600536812015565

Volume 68
Part 5
Pages m605-m606
May 2012

Received 4 April 2012
Accepted 10 April 2012
Online 18 April 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.005 Å
R = 0.026
wR = 0.046
Data-to-parameter ratio = 23.3
Details

cis-Dichlorido[2,3-dimethyl-3-(4,4,5,5-tetramethyl-1,3,2⁵-dioxaphospholan-2-yloxy)butan-2-olato-²O,P]oxido(triphenylphosphane-P)rhenium(V)

Anna Skarzynska,^a Milosz Siczek ^a and Andrzej Gniewek ^a ^*

^aFaculty of Chemistry, University of Wroclaw, 14 F. Joliot-Curie, 50-383 Wroclaw, Poland
Correspondence e-mail: andrzej@netesa.com

The title compound, cis-[Re(C₁₂H₂₄O₄P)Cl₂O(C₁₈H₁₅P)], was prepared from the analogous trans isomer [Glowiak et al. (2000). Polyhedron, 19, 2667-2672] by a trans-cis isomerization reaction. The Re^V atom adopts a distorted octahedral coordination geometry. Besides being coordinated by the oxide and the butanolate O atoms, the Re^V atom is coordinated by a pair of chloride ligands and two P atoms in cis positions with respect to each other. In the crystal, adjacent molecules are linked by weak C-HCl interactions, forming a three-dimensional network.

Related literature

For related structures and further discussion, see: Glowiak et al. (1998, 2000); Rybak et al. (2005). For typical bond lengths in coordination complexes, see: Orpen et al. (1989). For hydrogen-bond interactions, see: Aullón et al. (1998); Desiraju & Steiner (1999); Fábry et al. (2004). For details of the temperature control unit used during the data collection, see: Cosier & Glazer (1986). For specifications of the analytical numeric absorption correction, see: Clark & Reid (1995).

Experimental

Crystal data

[Re(C₁₂H₂₄O₄P)Cl₂O(C₁₈H₁₅P)]
M_r = 798.65
Orthorhombic, P 2₁ 2₁ 2₁
a = 10.963 (3) Å
b = 16.328 (4) Å
c = 17.797 (5) Å
V = 3185.7 (15) Å³
Z = 4
Mo K radiation
= 4.12 mm^-1
T = 100 K
0.16 × 0.12 × 0.05 mm

Data collection

Oxford Diffraction Xcalibur PX diffractometer with a CCD detector
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Wroclaw, Poland.]$ ) T_min = 0.582, T_max = 0.808
15943 measured reflections
8614 independent reflections
6813 reflections with I > 2(I)
R_int = 0.036

Refinement

R[F² > 2(F²)] = 0.026
wR(F²) = 0.046
S = 0.87
8614 reflections
369 parameters
H-atom parameters constrained
_max = 1.21 e Å^-3
_min = -1.09 e Å^-3
Absolute structure: Flack (1983), 3463 Friedel pairs
Flack parameter: -0.015 (4)

Table 1
Selected bond lengths (Å)

Re1-O1	1.698 (2)
Re1-O2	1.877 (3)
Re1-P1	2.3659 (12)
Re1-P2	2.4883 (12)
Re1-Cl1	2.4461 (10)
Re1-Cl2	2.4339 (10)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C31-H31BCl2ⁱ	0.98	2.86	3.796 (4)	161
C42-H42BCl1ⁱⁱ	0.98	2.87	3.830 (4)	167
C51-H51BCl1ⁱⁱ	0.98	2.85	3.809 (4)	166
C65-H65Cl2ⁱⁱⁱ	0.95	2.91	3.514 (4)	123
Symmetry codes: (i) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (ii) $[-x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iii) $[-x+{\script{1\over 2}}, -y+1, z+{\script{1\over 2}}]$ .

Data collection: CrysAlis CCD (Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Wroclaw, Poland.]$ ); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Wroclaw, Poland.]$ ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2403 ).

Acknowledgements

This work was supported with European funds in the frame of the Human Capital Operational Programme, through project POKL.04.01.01-00-054/10-00 "Development of the potential and educational offer of the University of Wroclaw - the chance to enhance the competitiveness of the University".

References

Aullón, G., Bellamy, D., Brammer, L., Bruton, E. & Orpen, A. G. (1998). Chem. Commun. pp. 653-654.
Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.
Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst. 19, 105-107.
Desiraju, G. R. & Steiner, T. (1999). The Weak Hydrogen Bond in Structural Chemistry and Biology. New York: Oxford University Press.
Fábry, J., Krupková, R., Vanek, P., Dusek, M. & Nemec, I. (2004). Acta Cryst. E60, m924-m926.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Glowiak, T., Rybak, W. K. & Skarzynska, A. (1998). Polyhedron, 17, 3153-3160.
Glowiak, T., Rybak, W. K. & Skarzynska, A. (2000). Polyhedron, 19, 2667-2672.
Orpen, A. G., Brammer, L., Allen, F. H., Kennard, O., Watson, D. G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans. pp. S1-83.
Oxford Diffraction (2010). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Wroclaw, Poland.
Rybak, W. K., Skarzynska, A., Szterenberg, L., Ciunik, Z. & Glowiak, T. (2005). Eur. J. Inorg. Chem. pp. 4964-4975.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds

cis-Dichlorido[2,3-dimethyl-3-(4,4,5,5-tetramethyl-1,3,25-dioxaphospholan-2-yloxy)butan-2-olato-2O,P]oxido(triphenylphosphane-P)rhenium(V)