[Journal logo]

Volume 69 
Part 2 
Pages m79-m80  
February 2013  

Received 6 December 2012
Accepted 18 December 2012
Online 9 January 2013

Key indicators
Single-crystal X-ray study
T = 140 K
Mean [sigma](C-C) = 0.013 Å
Disorder in solvent or counterion
R = 0.084
wR = 0.228
Data-to-parameter ratio = 12.6
Details
Open access

(4'-Ethynyl-2,2':6',2''-terpyridine)(2,2':6',2''-terpyridine)ruthenium(II) bis(hexafluoridophosphate) acetonitrile disolvate

The title heteroleptic bis-terpyridine complex, [Ru(C15H11N3)(C17H11N3)](PF6)2·2CH3CN, crystallized from an acetonitrile solution as a salt containing two hexafluoridophosphate counter-ions and two acetonitrile solvent molecules. The RuII atom has a distorted octahedral geometry due to the restricted bite angle [157.7 (3)°] of the two mer-arranged N,N',N''-tridendate ligands, viz. 2,2':6',2''-terpyridine (tpy) and 4'-ethynyl-2,2':6',2''-terpyridine (tpy'), which are essentially perpendicular to each other, with a dihedral angle of 87.75 (12)° between their terpyridyl planes. The rod-like acetylene group lies in the same plane as its adjacent terpyridyl moiety, with a maximum deviation of only 0.071 (11) Å from coplanarity with the pyridine rings. The mean Ru-N bond length involving the outer N atoms trans to each other is 2.069 (6) Å at tpy and 2.070 (6) Å at tpy'. The Ru-N bond length involving the central N atom is 1.964 (6) Å at tpy and 1.967 (6) Å at tpy'. Two of the three counter anions were refined as half-occupied.

Related literature

For the crystal structure of a RuII-terpyridine complex containing the {Ru(tpy-C[triple bond]C)} fragment, see: Ruben et al. (2008[Ruben, M., Landa, A., Lörtscher, E., Riel, H., Mayor, M., Görls, H., Weber, H. B., Arnold, A. & Evers, F. (2008). Small, 4, 2229-2235.]). For a comparative discussion, see the Comment section in the Supplementary materials. For bond lengths and angles in related tpy complexes, see: Lashgari et al. (1999[Lashgari, K., Kritikos, M., Norrestam, R. & Norrby, T. (1999). Acta Cryst. C55, 64-67.]); Scudder et al. (2005[Scudder, M. L., Craig, D. C. & Goodwin, H. A. (2005). CrystEngComm, 7, 642-649.]). For the preparation of the starting materials, see: Benniston et al. (2005[Benniston, A. C., Harriman, A., Li, P. & Sams, C. A. (2005). J. Am. Chem. Soc. 127, 2553-2564.]); Grosshenny et al. (1997[Grosshenny, V., Romero, F. M. & Ziessel, R. (1997). J. Org. Chem. 62, 1491-1500.]); Sullivan et al. (1980[Sullivan, B. P., Calvert, J. M. & Meyer, T. J. (1980). Inorg. Chem. 19, 1404-1407.]); Ziessel et al. (2004[Ziessel, R., Grosshenny, V., Hissler, M. & Stroh, C. (2004). Inorg. Chem. 43, 4262-4271.]). For general properties of this complex and related systems, see: Grosshenny et al. (1996[Grosshenny, V., Harriman, A., Gisselbrecht, J.-P. & Ziessel, R. (1996). J. Am. Chem. Soc. 118, 10315-10316.]); Hammarström & Johansson (2010[Hammarström, L. & Johansson, O. (2010). Coord. Chem. Rev. 254, 2546-2559.]); Ruther et al. (2011[Ruther, R. E., Rigsby, M. L., Gerken, J. B., Hogendoorn, S. R., Landis, E. C., Stahl, S. S. & Hamers, R. J. (2011). J. Am. Chem. Soc. 133, 5692-5694.]); Ziessel et al. (2004[Ziessel, R., Grosshenny, V., Hissler, M. & Stroh, C. (2004). Inorg. Chem. 43, 4262-4271.]).

[Scheme 1]

Experimental

Crystal data
  • [Ru(C15H11N3)(C17H11N3)](PF6)2·2C2H3N

  • Mr = 963.67

  • Triclinic, [P \overline 1]

  • a = 8.704 (2) Å

  • b = 8.860 (2) Å

  • c = 27.277 (7) Å

  • [alpha] = 96.876 (4)°

  • [beta] = 95.619 (3)°

  • [gamma] = 93.023 (3)°

  • V = 2073.9 (10) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.55 mm-1

  • T = 140 K

  • 0.10 × 0.08 × 0.06 mm

Data collection
  • Bruker D8 with APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.947, Tmax = 0.968

  • 19870 measured reflections

  • 7496 independent reflections

  • 5137 reflections with I > 2[sigma](I)

  • Rint = 0.081

Refinement
  • R[F2 > 2[sigma](F2)] = 0.084

  • wR(F2) = 0.228

  • S = 1.25

  • 7496 reflections

  • 596 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.75 e Å-3

  • [Delta][rho]min = -0.94 e Å-3

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2007[Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SJ5287 ).


Acknowledgements

Support by the US Department of Energy through the Laboratory Directed Research and Development (LDRD) program at LANL is gratefully acknowledged.

References

Benniston, A. C., Harriman, A., Li, P. & Sams, C. A. (2005). J. Am. Chem. Soc. 127, 2553-2564.  [ISI] [CrossRef] [PubMed] [ChemPort]
Bruker (2007). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Grosshenny, V., Harriman, A., Gisselbrecht, J.-P. & Ziessel, R. (1996). J. Am. Chem. Soc. 118, 10315-10316.  [CrossRef] [ChemPort] [ISI]
Grosshenny, V., Romero, F. M. & Ziessel, R. (1997). J. Org. Chem. 62, 1491-1500.  [CrossRef] [ChemPort]
Hammarström, L. & Johansson, O. (2010). Coord. Chem. Rev. 254, 2546-2559.
Lashgari, K., Kritikos, M., Norrestam, R. & Norrby, T. (1999). Acta Cryst. C55, 64-67.  [CSD] [CrossRef] [details]
Ruben, M., Landa, A., Lörtscher, E., Riel, H., Mayor, M., Görls, H., Weber, H. B., Arnold, A. & Evers, F. (2008). Small, 4, 2229-2235.  [CSD] [CrossRef] [PubMed] [ChemPort]
Ruther, R. E., Rigsby, M. L., Gerken, J. B., Hogendoorn, S. R., Landis, E. C., Stahl, S. S. & Hamers, R. J. (2011). J. Am. Chem. Soc. 133, 5692-5694.  [ISI] [CrossRef] [ChemPort] [PubMed]
Scudder, M. L., Craig, D. C. & Goodwin, H. A. (2005). CrystEngComm, 7, 642-649.  [ISI] [CSD] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Sullivan, B. P., Calvert, J. M. & Meyer, T. J. (1980). Inorg. Chem. 19, 1404-1407.  [CrossRef] [ChemPort] [ISI]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]
Ziessel, R., Grosshenny, V., Hissler, M. & Stroh, C. (2004). Inorg. Chem. 43, 4262-4271.  [ISI] [CrossRef] [PubMed] [ChemPort]


Acta Cryst (2013). E69, m79-m80   [ doi:10.1107/S1600536812051227 ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.