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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 [sigma](C-C) = 0.005 Å
R = 0.026
wR = 0.046
Data-to-parameter ratio = 23.3
Details
Open access

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

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[Glowiak, T., Rybak, W. K. & Skarzynska, A. (2000). Polyhedron, 19, 2667-2672.]). Polyhedron, 19, 2667-2672] by a trans-cis isomerization reaction. The ReV atom adopts a distorted octahedral coordination geometry. Besides being coordinated by the oxide and the butanolate O atoms, the ReV 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-H...Cl interactions, forming a three-dimensional network.

Related literature

For related structures and further discussion, see: Glowiak et al. (1998[Glowiak, T., Rybak, W. K. & Skarzynska, A. (1998). Polyhedron, 17, 3153-3160.], 2000[Glowiak, T., Rybak, W. K. & Skarzynska, A. (2000). Polyhedron, 19, 2667-2672.]); Rybak et al. (2005[Rybak, W. K., Skarzynska, A., Szterenberg, L., Ciunik, Z. & Glowiak, T. (2005). Eur. J. Inorg. Chem. pp. 4964-4975.]). For typical bond lengths in coordination complexes, see: Orpen et al. (1989[Orpen, A. G., Brammer, L., Allen, F. H., Kennard, O., Watson, D. G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans. pp. S1-83.]). For hydrogen-bond interactions, see: Aullón et al. (1998[Aullón, G., Bellamy, D., Brammer, L., Bruton, E. & Orpen, A. G. (1998). Chem. Commun. pp. 653-654.]); Desiraju & Steiner (1999[Desiraju, G. R. & Steiner, T. (1999). The Weak Hydrogen Bond in Structural Chemistry and Biology. New York: Oxford University Press.]); Fábry et al. (2004[Fábry, J., Krupková, R., Vanek, P., Dusek, M. & Nemec, I. (2004). Acta Cryst. E60, m924-m926.]). For details of the temperature control unit used during the data collection, see: Cosier & Glazer (1986[Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst. 19, 105-107.]). For specifications of the analytical numeric absorption correction, see: Clark & Reid (1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.]).

[Scheme 1]

Experimental

Crystal data
  • [Re(C12H24O4P)Cl2O(C18H15P)]

  • Mr = 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[alpha] radiation

  • [mu] = 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.]) Tmin = 0.582, Tmax = 0.808

  • 15943 measured reflections

  • 8614 independent reflections

  • 6813 reflections with I > 2[sigma](I)

  • Rint = 0.036

Refinement
  • R[F2 > 2[sigma](F2)] = 0.026

  • wR(F2) = 0.046

  • S = 0.87

  • 8614 reflections

  • 369 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.21 e Å-3

  • [Delta][rho]min = -1.09 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 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-H...A D-H H...A D...A D-H...A
C31-H31B...Cl2i 0.98 2.86 3.796 (4) 161
C42-H42B...Cl1ii 0.98 2.87 3.830 (4) 167
C51-H51B...Cl1ii 0.98 2.85 3.809 (4) 166
C65-H65...Cl2iii 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[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: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); 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.  [CrossRef] [details]
Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst. 19, 105-107.  [CrossRef] [ChemPort] [ISI] [details]
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.  [CSD] [CrossRef] [details]
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
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.  [CrossRef]
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.  [ISI] [CSD] [CrossRef]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2012). E68, m605-m606   [ doi:10.1107/S1600536812015565 ]

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