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Volume 69 
Part 8 
Pages m462-m463  
August 2013  

Received 6 June 2013
Accepted 10 July 2013
Online 17 July 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.004 Å
Disorder in solvent or counterion
R = 0.050
wR = 0.129
Data-to-parameter ratio = 14.5
Details
Open access

Tetraethylammonium dicyanido(5,10,15,20-tetraphenylporphyrinato)ferrate(III) dichloromethane monosolvate

aDepartment of Chemistry, L.N. Gumilyov Eurasian National University, 5 Munaitpasov Str, 010008 Astana, Kazakhstan, and bDepartment of Chemistry and Biochemistry, Florida State University, 95 Chieftan Way, Tallahassee, FL 32306-4390, USA
Correspondence e-mail: shatruk@chem.fsu.edu

The title compound, (C8H20N)[Fe(C44H28N4)(CN)2]·CH2Cl2 or (Et4N)[Fe(TPP)(CN)2], was recrystallized from dichloromethane-diethyl ether. The compound crystallizes with the two unique halves of the FeIII porphyrinato complex, one tetraethylammonium cation and one interstitial dichloromethane molecule within the asymmetric unit. Both anionic FeIII complexes exhibit inversion symmetry. Both the cation and the solvent molecules show positional disorder. The cation is disordered over two sets of sites with an occupancy ratio of 0.710 (3):0.290 (3); the solvent molecule is disordered over three positions with a 0.584 (6):0.208 (3):0.202 (5) ratio. The crystal packing features columns of [Fe(TPP)(CN)2]- anions that propagate along [001]. The columns further pack into layers that are parallel to (011) and also include the Et4N+ cations. The interstitial CH2Cl2 molecules appear in the interlayer space. This complex may serve as a useful precursor for the assembly of multinuclear and extended CN-bridged complexes for the design of single-molecule and single-chain magnets, respectively.

Related literature

For transition metal ions bridged by cyanide, see: Corsi et al. (1999[Corsi, D. M., Murthy, N. N., Young, V. G. Jr & Karlin, K. D. (1999). Inorg. Chem. 38, 848-858.]); Dunbar & Heintz (1997[Dunbar, K. R. & Heintz, R. (1997). Prog. Inorg. Chem. 45, 283-391.]); Scott et al. (1994[Scott, M. J., Lee, S. C. & Holm, R. H. (1994). Inorg. Chem. 33, 4651-4662.]); Schelter et al. (2004[Schelter, E. J., Prosvirin, A. V., Reiff, W. M. & Dunbar, K. R. (2004). Angew. Chem. Int. Ed. 43, 4912-4915.], 2007[Schelter, E. J., Karadas, F., Avendano, C., Prosvirin, A. V., Wernsdorfer, W. & Dunbar, K. R. (2007). J. Am. Chem. Soc. 129, 8139-8149.]); Shatruk et al. (2009[Shatruk, M., Avendano, C. & Dunbar, K. R. (2009). Prog. Inorg. Chem. 56, 155-334.]). For similar porphyrin compounds, see: Li et al. (2009[Li, J., Noll, B. C., Schulz, C. E. & Scheidt, W. R. (2009). Angew. Chem. Int. Ed. 48, 5010-5013.]); Scheidt et al. (1980[Scheidt, W. R., Haller, K. J. & Hatano, K. (1980). J. Am. Chem. Soc. 102, 3017-3021.]).

[Scheme 1]

Experimental

Crystal data
  • (C8H20N)[Fe(C44H28N4)(CN)2]·CH2Cl2

  • Mr = 935.77

  • Triclinic, [P \overline 1]

  • a = 11.0069 (8) Å

  • b = 15.0344 (11) Å

  • c = 15.4350 (11) Å

  • [alpha] = 80.075 (1)°

  • [beta] = 77.527 (1)°

  • [gamma] = 83.077 (1)°

  • V = 2447.4 (3) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.46 mm-1

  • T = 173 K

  • 0.22 × 0.15 × 0.09 mm

Data collection
  • Bruker APEXII CCD area-detector diffractometer

  • Absorption correction: numerical (SADABS; Bruker, 2003[Bruker (2003). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.905, Tmax = 0.960

  • 19913 measured reflections

  • 9891 independent reflections

  • 7117 reflections with I > 2[sigma](I)

  • Rint = 0.034

Refinement
  • R[F2 > 2[sigma](F2)] = 0.050

  • wR(F2) = 0.129

  • S = 1.12

  • 9891 reflections

  • 682 parameters

  • 37 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.40 e Å-3

  • [Delta][rho]min = -0.43 e Å-3

Data collection: SMART (Bruker, 2003[Bruker (2003). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). SADABS, SAINT and SMART. 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: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PJ2003 ).


Acknowledgements

The National Science Foundation is gratefully acknowledged for the support of this research via grant CHE-0911109 to MS.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.  [CrossRef] [ChemPort]
Bruker (2003). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.
Corsi, D. M., Murthy, N. N., Young, V. G. Jr & Karlin, K. D. (1999). Inorg. Chem. 38, 848-858.  [Web of Science] [CrossRef] [PubMed] [ChemPort]
Dunbar, K. R. & Heintz, R. (1997). Prog. Inorg. Chem. 45, 283-391.  [CrossRef] [ChemPort]
Li, J., Noll, B. C., Schulz, C. E. & Scheidt, W. R. (2009). Angew. Chem. Int. Ed. 48, 5010-5013.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Scheidt, W. R., Haller, K. J. & Hatano, K. (1980). J. Am. Chem. Soc. 102, 3017-3021.  [CrossRef] [ChemPort] [Web of Science]
Schelter, E. J., Karadas, F., Avendano, C., Prosvirin, A. V., Wernsdorfer, W. & Dunbar, K. R. (2007). J. Am. Chem. Soc. 129, 8139-8149.  [Web of Science] [CSD] [CrossRef] [PubMed] [ChemPort]
Schelter, E. J., Prosvirin, A. V., Reiff, W. M. & Dunbar, K. R. (2004). Angew. Chem. Int. Ed. 43, 4912-4915.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Scott, M. J., Lee, S. C. & Holm, R. H. (1994). Inorg. Chem. 33, 4651-4662.  [CrossRef] [ChemPort] [Web of Science]
Shatruk, M., Avendano, C. & Dunbar, K. R. (2009). Prog. Inorg. Chem. 56, 155-334.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m462-m463   [ doi:10.1107/S1600536813019119 ]

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