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Volume 69 
Part 5 
Pages m296-m297  
May 2013  

Received 8 April 2013
Accepted 24 April 2013
Online 30 April 2013

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.002 Å
Disorder in solvent or counterion
R = 0.025
wR = 0.074
Data-to-parameter ratio = 16.1
Details
Open access

{2,2'-[N,N'-Bis(pyridin-2-ylmethyl)propane-1,3-diyldi(nitrilo)]diacetato}cobalt(III) hexafluoridophosphate acetonitrile 0.064-solvate

aDepartment of Chemistry, Illinois State University, Campus Box 4160, Normal, IL 61790-4160, USA, and bDepartment of Chemistry, Loyola University Chicago, Chicago, IL 60626, USA
Correspondence e-mail: mclauchlan@illinoisstate.edu

In the title compound, [Co(C19H22N4O4)]PF6·0.064CH3CN, commonly known as [Co(bppd)]PF6·0.064CH3CN, where bppd represents the historical ligand name N,N'-bis(2-pyridylmethyl)-1,3-diaminopropane-N,N'-diacetate, the CoIII atom is coordinated in a distorted octahedral geometry with an N4O2 donor atom set. The acetate O atoms, which exhibit monodentate coordination, are oriented in a trans configuration with respect to each other, whereas the pyridyl N atoms are coordinated in a cis configuration. The compound crystallizes with two crystallographically unique cations and two anions per asymmetric unit along with a disordered, partially occupied (occupancy = 0.128) acetonitrile solvent molecule. Crystals of the title complex were found to be twinned by pseudomerohedry with a 180° rotation around [10-1] and a refined contribution of 90.5 (3)% of the major twin component.

Related literature

For this and related ligands, see: Lacoste et al. (1965[Lacoste, R. G., Christoffers, G. V. & Martell, A. E. (1965). J. Am. Chem. Soc. 87, 2385-2388.]); Caravan et al. (1997[Caravan, P., Rettig, S. J. & Orvig, C. (1997). Inorg. Chem. 36, 1306-1315.]); Kanamori et al. (2001[Kanamori, K., Kyotoh, A., Fujimoto, K., Nagata, K., Suzuki, H. & Okamoto, K. (2001). Bull. Chem. Soc. Jpn, 74, 2113-2118.]); Kissel et al. (2013[Kissel, D. S., Bender, J., Arnold, W. R., McLauchlan, C. C. & Herlinger, A. W. (2013). Paper #985. Division of Inorganic Chemistry, Lanthanide and Actinide Session, 245th ACS National Meeting and Exposition, New Orleans, LA, April 7-11, 2013.]). For a structure with a derivative of this ligand, see: Sato et al. (2012[Sato, K., Ohnuki, T., Takahashi, H., Miyashita, Y., Nozaki, K. & Kanamori, K. (2012). Inorg. Chem. 51, 5026-2036.]). For a related CoIII-N,N'-bis(2-pyridylmethyl)-1,2-diaminoethane-N,N'-diacetate complex, [Co(bped)+], see: Caravan et al. (1997[Caravan, P., Rettig, S. J. & Orvig, C. (1997). Inorg. Chem. 36, 1306-1315.]). For literature on possible applications, see: Caravan et al. (1997[Caravan, P., Rettig, S. J. & Orvig, C. (1997). Inorg. Chem. 36, 1306-1315.]); Geraldes (1999[Geraldes, C. F. G. C. (1999). NMR Supramol. Chem. 526, 133-154.]); Jensen (2000[Jensen, M. P. (2000). J. Alloys Compd, 303-304, 137-145.]); Heitzmann et al. (2009[Heitzmann, M., Bravard, F., Gateau, C., Boubals, N., Berthon, C., Pecaut, J., Charbonnel, M. C. & Delangle, P. (2009). Inorg. Chem. 48, 246-256.]); Ogden et al. (2012[Ogden, M. D., Meier, G. P. & Nash, K. L. (2012). J. Solution Chem. 41, 1-16.]); Sato et al. (2012[Sato, K., Ohnuki, T., Takahashi, H., Miyashita, Y., Nozaki, K. & Kanamori, K. (2012). Inorg. Chem. 51, 5026-2036.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(C19H22N4O4)]PF6·0.064C2H3N

  • Mr = 576.80

  • Monoclinic, P 21 /n

  • a = 21.8891 (7) Å

  • b = 10.2350 (3) Å

  • c = 21.9242 (7) Å

  • [beta] = 112.802 (2)°

  • V = 4527.9 (2) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 0.91 mm-1

  • T = 100 K

  • 0.46 × 0.23 × 0.16 mm

Data collection
  • Bruker APEXII diffractometer equipped with a CCD detector

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.680, Tmax = 0.871

  • 98080 measured reflections

  • 10379 independent reflections

  • 9851 reflections with I > 2[sigma](I)

  • Rint = 0.028

Refinement
  • R[F2 > 2[sigma](F2)] = 0.025

  • wR(F2) = 0.074

  • S = 1.28

  • 10379 reflections

  • 645 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.64 e Å-3

  • [Delta][rho]min = -0.48 e Å-3

Table 1
Selected bond lengths (Å)

Co1-O1 1.8828 (11)
Co1-O3 1.8899 (11)
Co1-N1 1.9484 (13)
Co1-N2 1.9625 (12)
Co1-N3 1.9397 (13)
Co1-N4 1.9641 (13)
Co2-O5 1.8875 (10)
Co2-O7 1.8830 (11)
Co2-N5 1.9403 (13)
Co2-N6 1.9654 (12)
Co2-N7 1.9575 (12)
Co2-N8 1.9645 (12)

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: enCIFer (Allen et al., 2004[Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2736 ).


Acknowledgements

This work was supported by Illinois State University, Loyola University Chicago, and the National Science Foundation (US, CHE-0645081). CCM also acknowledges the National Science Foundation for the purchase of the Bruker APEXII (CHE-10-39689). DSK wishes to thank Loyola University Chicago and the Schmitt Foundation for fifth year fellowship support. The authors also thank Dr M. Zeller (Youngstown State University) for helpful discussions.

References

Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338.  [ISI] [CrossRef] [ChemPort] [details]
Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Caravan, P., Rettig, S. J. & Orvig, C. (1997). Inorg. Chem. 36, 1306-1315.  [CrossRef] [PubMed] [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Geraldes, C. F. G. C. (1999). NMR Supramol. Chem. 526, 133-154.  [CrossRef] [ChemPort]
Heitzmann, M., Bravard, F., Gateau, C., Boubals, N., Berthon, C., Pecaut, J., Charbonnel, M. C. & Delangle, P. (2009). Inorg. Chem. 48, 246-256.  [CrossRef] [PubMed] [ChemPort]
Jensen, M. P. (2000). J. Alloys Compd, 303-304, 137-145.  [CrossRef] [ChemPort]
Kanamori, K., Kyotoh, A., Fujimoto, K., Nagata, K., Suzuki, H. & Okamoto, K. (2001). Bull. Chem. Soc. Jpn, 74, 2113-2118.  [CrossRef] [ChemPort]
Kissel, D. S., Bender, J., Arnold, W. R., McLauchlan, C. C. & Herlinger, A. W. (2013). Paper #985. Division of Inorganic Chemistry, Lanthanide and Actinide Session, 245th ACS National Meeting and Exposition, New Orleans, LA, April 7-11, 2013.
Lacoste, R. G., Christoffers, G. V. & Martell, A. E. (1965). J. Am. Chem. Soc. 87, 2385-2388.  [CrossRef] [ChemPort]
Ogden, M. D., Meier, G. P. & Nash, K. L. (2012). J. Solution Chem. 41, 1-16.  [CrossRef] [ChemPort]
Sato, K., Ohnuki, T., Takahashi, H., Miyashita, Y., Nozaki, K. & Kanamori, K. (2012). Inorg. Chem. 51, 5026-2036.  [CrossRef] [ChemPort] [PubMed]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]


Acta Cryst (2013). E69, m296-m297   [ doi:10.1107/S1600536813011136 ]

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