[Journal logo]

Volume 69 
Part 10 
Pages m549-m550  
October 2013  

Received 3 September 2013
Accepted 11 September 2013
Online 21 September 2013

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.006 Å
R = 0.057
wR = 0.114
Data-to-parameter ratio = 17.2
Details
Open access

Tris[4-(dimethylamino)pyridine][tris(pyrazol-1-yl)methane]ruthenium(II) bis(hexafluoridophosphate) diethyl ether monosolvate

aSchool of Chemistry, University of Manchester, Manchester M13 9PL, UK
Correspondence e-mail: b.coe@manchester.ac.uk

In the title compound, [Ru(C10H10N6)(C7H10N2)3](PF6)2·C4H10O, the RuII cation is coordinated by one tris(1-pyrazolyl)methane (Tpm) and three dimethylaminopyridine (dmap) ligands in a slightly distorted octahedral geometry. The asymmetric unit consists of one complex cation, two hexafluoridophosphate anions and one diethyl ether solvent molecule in general positions. Although quite a large number of ruthenium complexes of the facially coordinating tridentate Tpm ligand have been structurally characterized, this is only the second one containing three pyridyl co-ligands. The average Ru-N(Tpm) distance is 2.059 (12) Å, while the average Ru-N(dmap) [dmap = 4-(dimethylamino)pyridine] distance is somewhat longer at 2.108 (13) Å. The orientation of the dmap ligands varies greatly, with dihedral angles between the pyridyl and opposite pyrazolyl rings of 14.3 (2), 23.2 (2) and 61.2 (2)°.

Related literature

For background to the synthesis, see: Llobet et al. (1988[Llobet, A., Doppelt, P. & Meyer, T. J. (1988). Inorg. Chem. 27, 514-520.]); Calvert et al. (1983[Calvert, J. M., Schmehl, R. H., Sullivan, B. P., Facci, J. S., Meyer, T. J. & Murray, R. W. (1983). Inorg. Chem. 22, 2151-2162.]). For examples of other structures of ruthenium complexes of the Tpm ligand, see: Llobet et al. (1989[Llobet, A., Curry, M. E., Evans, H. T. & Meyer, T. J. (1989). Inorg. Chem. 28, 3131-3137.]); Wilson & Nelson (2003[Wilson, D. C. & Nelson, J. H. (2003). J. Organomet. Chem. 682, 272-289.]); Katz et al. (2005[Katz, N. E., Romero, I., Llobet, A., Parella, T. & Benet-Buchholz, J. (2005). Eur. J. Inorg. Chem. pp. 272-277.]); Iengo et al. (2005[Iengo, E., Zangrando, E., Baiutti, E., Munini, F. & Alessio, E. (2005). Eur. J. Inorg. Chem. pp. 1019-1031.]); Foxon et al. (2007[Foxon, S. P., Metcalfe, C., Adams, H., Webb, M. & Thomas, J. A. (2007). Inorg. Chem. 46, 409-416.]); Kuzu et al. (2009[Kuzu, I., Nied, D. & Breher, F. (2009). Eur. J. Inorg. Chem. pp. 872-879.]); Waywell et al. (2010[Waywell, P., Gonzalez, V., Gill, M. R., Adams, H., Meijer, A. J. H. M., Williamson, M. P. & Thomas, J. A. (2010). Chem. Eur. J. 16, 2407-2417.]); Zagermann et al. (2011[Zagermann, J., Klein, K., Merz, K., Molon, M. & Metzler-Nolte, N. (2011). Eur. J. Inorg. Chem. pp. 4212-4219.]); De et al. (2011[De, P., Mondal, T. K., Mobin, S. M. & Lahiri, G. K. (2011). Inorg. Chim. Acta, 372, 250-258.]); Agarwala et al. (2011[Agarwala, H., Das, D., Mobin, S. M., Mondal, T. K. & Lahiri, G. K. (2011). Inorg. Chim. Acta, 374, 216-225.], 2013[Agarwala, H., Ehret, F., Chowdhury, A. D., Maji, S., Mobin, S. M., Kaim, W. & Lahiri, G. K. (2013). Dalton Trans. 42, 3721-3734.]); Serrano et al. (2011[Serrano, I., López, M. I., Ferrer, I., Poater, A., Parella, T., Fontrodona, X., Solà, M., Llobet, A., Rodríguez, M. & Romero, I. (2011). Inorg. Chem. 50, 6044-6054.]); Cadranel et al. (2012[Cadranel, A., Alborés, P., Yamazaki, S., Kleiman, V. D. & Baraldo, L. M. (2012). Dalton Trans. 41, 5343-5350.]). For examples of other structures of ruthenium complexes of the dmap ligand, see: Bonnet et al. (2003[Bonnet, S., Collin, J.-P., Gruber, N., Sauvage, J.-P. & Schofield, E. R. (2003). Dalton Trans. pp. 4654-4662.]); Rossi et al. (2008[Rossi, M. B., Piro, O. E., Castellano, E. E., Alborés, P. & Baraldo, L. M. (2008). Inorg. Chem. 47, 2416-2427.], 2010[Rossi, M. B., Abboud, K. A., Alborés, P. & Baraldo, L. M. (2010). Eur. J. Inorg. Chem. pp. 5613-5616.]); Mutoh et al. (2010[Mutoh, Y., Kozono, N., Araki, M., Tsuchida, N., Takano, K. & Ishii, Y. (2010). Organometallics, 29, 519-522.]); Dunbar et al. (2011[Dunbar, M. A., Balof, S. L., Roberts, A. N., Valente, E. J. & Schanz, H.-J. (2011). Organometallics, 30, 199-203.]). For the closest related structure, see: Laurent et al. (1999[Laurent, F., Plantalech, E., Donnadieu, B., Jiménez, A., Hernández, F., Martínez-Ripoll, M., Biner, M. & Llobet, A. (1999). Polyhedron, 18, 3321-3331.]).

[Scheme 1]

Experimental

Crystal data
  • [Ru(C10H10N6)(C7H10N2)3](PF6)2·C4H10O

  • Mr = 1045.88

  • Triclinic, [P \overline 1]

  • a = 12.1005 (9) Å

  • b = 12.5711 (9) Å

  • c = 15.7032 (11) Å

  • [alpha] = 80.047 (1)°

  • [beta] = 75.377 (1)°

  • [gamma] = 71.449 (1)°

  • V = 2180.1 (3) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.53 mm-1

  • T = 100 K

  • 0.30 × 0.10 × 0.03 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • 19049 measured reflections

  • 9932 independent reflections

  • 7805 reflections with I > 2[sigma](I)

  • Rint = 0.051

Refinement
  • R[F2 > 2[sigma](F2)] = 0.057

  • wR(F2) = 0.114

  • S = 0.95

  • 9932 reflections

  • 576 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.03 e Å-3

  • [Delta][rho]min = -0.98 e Å-3

Table 1
Selected bond lengths (Å)

N1-Ru1 2.122 (3)
N3-Ru1 2.097 (3)
N5-Ru1 2.104 (3)
N8-Ru1 2.071 (3)
N10-Ru1 2.048 (3)
N12-Ru1 2.059 (3)

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2003[Bruker (2003). SMART and SAINT-Plus. 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: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NC2317 ).


Acknowledgements

The authors would like to thank the EPSRC for funding (grant EP/G02099).

References

Agarwala, H., Das, D., Mobin, S. M., Mondal, T. K. & Lahiri, G. K. (2011). Inorg. Chim. Acta, 374, 216-225.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Agarwala, H., Ehret, F., Chowdhury, A. D., Maji, S., Mobin, S. M., Kaim, W. & Lahiri, G. K. (2013). Dalton Trans. 42, 3721-3734.  [CSD] [CrossRef] [ChemPort] [PubMed]
Bonnet, S., Collin, J.-P., Gruber, N., Sauvage, J.-P. & Schofield, E. R. (2003). Dalton Trans. pp. 4654-4662.  [CSD] [CrossRef]
Bruker (2003). SMART and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Cadranel, A., Alborés, P., Yamazaki, S., Kleiman, V. D. & Baraldo, L. M. (2012). Dalton Trans. 41, 5343-5350.  [CSD] [CrossRef] [ChemPort] [PubMed]
Calvert, J. M., Schmehl, R. H., Sullivan, B. P., Facci, J. S., Meyer, T. J. & Murray, R. W. (1983). Inorg. Chem. 22, 2151-2162.  [CrossRef] [ChemPort] [Web of Science]
De, P., Mondal, T. K., Mobin, S. M. & Lahiri, G. K. (2011). Inorg. Chim. Acta, 372, 250-258.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Dunbar, M. A., Balof, S. L., Roberts, A. N., Valente, E. J. & Schanz, H.-J. (2011). Organometallics, 30, 199-203.  [CSD] [CrossRef] [ChemPort]
Foxon, S. P., Metcalfe, C., Adams, H., Webb, M. & Thomas, J. A. (2007). Inorg. Chem. 46, 409-416.  [Web of Science] [CSD] [CrossRef] [PubMed] [ChemPort]
Iengo, E., Zangrando, E., Baiutti, E., Munini, F. & Alessio, E. (2005). Eur. J. Inorg. Chem. pp. 1019-1031.  [Web of Science] [CSD] [CrossRef]
Katz, N. E., Romero, I., Llobet, A., Parella, T. & Benet-Buchholz, J. (2005). Eur. J. Inorg. Chem. pp. 272-277.  [CSD] [CrossRef]
Kuzu, I., Nied, D. & Breher, F. (2009). Eur. J. Inorg. Chem. pp. 872-879.  [Web of Science] [CSD] [CrossRef]
Laurent, F., Plantalech, E., Donnadieu, B., Jiménez, A., Hernández, F., Martínez-Ripoll, M., Biner, M. & Llobet, A. (1999). Polyhedron, 18, 3321-3331.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Llobet, A., Curry, M. E., Evans, H. T. & Meyer, T. J. (1989). Inorg. Chem. 28, 3131-3137.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Llobet, A., Doppelt, P. & Meyer, T. J. (1988). Inorg. Chem. 27, 514-520.  [CrossRef] [ChemPort] [Web of Science]
Mutoh, Y., Kozono, N., Araki, M., Tsuchida, N., Takano, K. & Ishii, Y. (2010). Organometallics, 29, 519-522.  [CSD] [CrossRef] [ChemPort]
Rossi, M. B., Abboud, K. A., Alborés, P. & Baraldo, L. M. (2010). Eur. J. Inorg. Chem. pp. 5613-5616.  [Web of Science] [CSD] [CrossRef]
Rossi, M. B., Piro, O. E., Castellano, E. E., Alborés, P. & Baraldo, L. M. (2008). Inorg. Chem. 47, 2416-2427.  [Web of Science] [CSD] [CrossRef] [PubMed] [ChemPort]
Serrano, I., López, M. I., Ferrer, I., Poater, A., Parella, T., Fontrodona, X., Solà, M., Llobet, A., Rodríguez, M. & Romero, I. (2011). Inorg. Chem. 50, 6044-6054.  [Web of Science] [CSD] [CrossRef] [ChemPort] [PubMed]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Waywell, P., Gonzalez, V., Gill, M. R., Adams, H., Meijer, A. J. H. M., Williamson, M. P. & Thomas, J. A. (2010). Chem. Eur. J. 16, 2407-2417.  [CrossRef] [ChemPort] [PubMed]
Wilson, D. C. & Nelson, J. H. (2003). J. Organomet. Chem. 682, 272-289.  [CSD] [CrossRef] [ChemPort]
Zagermann, J., Klein, K., Merz, K., Molon, M. & Metzler-Nolte, N. (2011). Eur. J. Inorg. Chem. pp. 4212-4219.  [Web of Science] [CSD] [CrossRef]


Acta Cryst (2013). E69, m549-m550   [ doi:10.1107/S1600536813025245 ]

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.