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Volume 64 
Part 2 
Page m435  
February 2008  

Received 4 January 2008
Accepted 24 January 2008
Online 30 January 2008

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Key indicators
Single-crystal X-ray study
T = 130 K
Mean [sigma](C-C) = 0.012 Å
R = 0.040
wR = 0.040
Data-to-parameter ratio = 10.6
Details
Open access

Di-[mu]-hydroxido-[kappa]4O:O-[mu]-trifluoromethanesulfonato-[kappa]2O:O'-bis[(5,5'-dimethyl-2,2-bipyridine-[kappa]2N,N')([eta]5-pentamethylcyclopentadienyl)ytterbium(III)] tetraphenylborate 5,5'-dimethyl-2,2-bipyridine

Daniel Kazhdana*

aChemistry Department and Chemical Sciences Division of Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720, USA
Correspondence e-mail: kazhdan@berkeley.edu

The title compound, [Yb2(CF3O3S)(C10H15)2(OH)2(C12H12N2)2](C24H20B)·C12H12N2, crystallizes as a half-sandwich complex with a bridging trifluoromethanesulfonate as well as two bridging hydroxide groups. The bound bipyridine ligands have N-C-C-N torsion angles of 13.1 (9) and -12.1 (8)°. The structure also contains an uncoordinated 5,5'-dimethyl-2,2'-bipyridine molecule with an N-C-C-N torsion angle of 169.5 (7)°. The triply bridged Yb centers are 3.5990 (4) Å apart. The Yb-N bond lengths are in the range 2.389 (6)-2.424 (5) Å.

Related literature

For related literature, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]); van Albada et al. (2005[Albada, G. A. van, Mutikainen, I., Turpeinen, U. & Reedijk, J. (2005). Acta Cryst. E61, m1411-m1412.]); Schultz et al. (2002[Schultz, M., Boncella, J. M., Berg, D. J., Tilley, T. D. & Andersen, R. A. (2002). Organometallics, 21, 460-472.]).

[Scheme 1]

Experimental

Crystal data

  • [Yb2(CF3O3S)(C10H15)2(OH)2(C12H12N2)2](C24H20B)·C12H12N2

  • Mr = 1671.57

  • Triclinic, [P \overline 1]

  • a = 13.0458 (8) Å

  • b = 13.7179 (9) Å

  • c = 23.3306 (15) Å

  • [alpha] = 87.215 (1)°

  • [beta] = 86.669 (1)°

  • [gamma] = 68.161 (1)°

  • V = 3867.4 (4) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 2.49 mm-1

  • T = 130 (1) K

  • 0.15 × 0.13 × 0.08 mm
Data collection

  • Bruker APEX diffractometer

  • Absorption correction: multi-scan (using intensity measurements; Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.691, Tmax = 0.819

  • 20924 measured reflections

  • 15784 independent reflections

  • 9459 reflections with F2 > 3[sigma](F2)

  • Rint = 0.021
Refinement

  • R[F2 > 2[sigma](F2)] = 0.040

  • wR(F2) = 0.040

  • S = 1.39

  • 9459 reflections

  • 892 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.59 e Å-3

  • [Delta][rho]min = -2.03 e Å-3

Table 1
Selected geometric parameters (Å, °)

Cg1 and Cg2 are the centroids of the C1-C5 and C6-C10 rings, respectively.
Yb1-Yb2 3.5990 (4)
Yb1-O1 2.255 (4)
Yb1-O2 2.207 (4)
Yb1-O3 2.361 (4)
Yb1-N1 2.408 (5)
Yb1-N2 2.424 (5)
Yb1-Cg1 2.3750 (3)
Yb2-O1 2.295 (5)
Yb2-O2 2.214 (4)
Yb2-O4 2.332 (5)
Yb2-N3 2.408 (6)
Yb2-N4 2.389 (6)
Yb2-Cg2 2.3585 (3)
Yb1-O1-Yb2 104.5 (2)
Yb1-O2-Yb2 109.0 (2)

Data collection: SMART (Bruker, 2002[Bruker (2002). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2002[Bruker (2002). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.]); program(s) used to refine structure: TEXSAN (MSC/Rigaku, 1998[MSC/Rigaku (1998). TEXSAN. Version 1.10. MSC/Rigaku, The Woodlands, Texas, USA.]); molecular graphics: TEXSAN; software used to prepare material for publication: TEXSAN.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PV2065 ).

Acknowledgements

This work was supported by the Director, Office of Energy Research, Office of Basic Energy Sciences, Chemical Sciences Division, US Department of Energy, under contract No. DE-AC03-76SF0098. I thank Professor Richard A. Andersen (UC Berkeley) and Dr Fred Hollander (CHEXRAY, the UC Berkeley X-ray facility).

References

Albada, G. A. van, Mutikainen, I., Turpeinen, U. & Reedijk, J. (2005). Acta Cryst. E61, m1411-m1412.  [CSD] [CrossRef] [details]
Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [CrossRef] [details]
Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.  [CrossRef] [details]
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.  [CrossRef] [details]
Bruker (2002). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
MSC/Rigaku (1998). TEXSAN. Version 1.10. MSC/Rigaku, The Woodlands, Texas, USA.
Schultz, M., Boncella, J. M., Berg, D. J., Tilley, T. D. & Andersen, R. A. (2002). Organometallics, 21, 460-472.  [CrossRef] [ChemPort]

Acta Cryst (2008). E64, m435  [ doi:10.1107/S1600536808002791 ]

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