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Volume 69 
Part 1 
Pages m12-m13  
January 2013  

Received 16 November 2012
Accepted 26 November 2012
Online 5 December 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.004 Å
Disorder in main residue
R = 0.049
wR = 0.134
Data-to-parameter ratio = 16.4
Details
Open access

Tris(1,10-phenanthroline-[kappa]2N,N')iron(II) bis(1,1,3,3-tetracyano-2-ethoxypropenide) hemihydrate

aDépartement de Technologie, Faculté de Technologie, Université 20 Août 1955 de Skikda, 21000 Skikda, Algeria,bUnité de Recherche de Chimie de l'Environnement et Moléculaire Structurale (CHEMS), Université Mentouri Constantine, 25000 Constantine, Algeria,cLaboatoire de Chimie, Ingénierie Moléculaire et Nanostructures (LCIMN), Université Ferhat Abbas de Sétif, 19000 Sétif, Algeria,dDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia,eChemistry Department, King Abdulaziz University, PO Box 80203 Jeddah, Saudi Arabia,fClermont Université, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, BP 10448, 63000 Clermont-Ferrand, France, and gCNRS UMR 6296, ICCF, BP 80026, 63171 Aubière, France
Correspondence e-mail: fat_setifi@yahoo.fr

In the title hydrated molecular salt, [Fe(C12H8N2)3](C9H5N4O)2·0.5H2O, the water molecule site is half-occupied. The Fe-N bond lengths within the octahedral tris-chelate [Fe(phen)3]2+ ion (phen is 1,10-phenantroline) are indicative of a low-spin d6 electronic configuration for the metal ion. The C-N, C-C and C-O bond lengths in the polynitrile anions indicate extensive electronic delocalization. In the crystal, the components are linked through O-H...N hydrogen bonds, forming [100] chains, as well as through Coulombic interactions.

Related literature

For background to 1,10-phenanthroline as a chelating ligand, see: Hoshina et al. (2000[Hoshina, G., Ohba, S., Tsuchiya, N., Isobe, T. & Senna, M. (2000). Acta Cryst. C56, e191-e192.]); Hwang & Ha (2006[Hwang, I.-C. & Ha, K. (2006). Acta Cryst. E62, m376-m378.]); Aparici Plaza et al. (2007[Aparici Plaza, L., Baranowska, K. & Becker, B. (2007). Acta Cryst. E63, m1537-m1539.]); Zhou & Guo (2007[Zhou, D.-P. & Guo, G.-L. (2007). Acta Cryst. E63, m1122-m1124.]). For a related structure, see: Cai & Zhan (2012[Cai, Z.-M. & Zhan, S.-Z. (2012). Acta Cryst. E68, m956.]). For further synthetic details, see: Middleton & Engelhardt (1958[Middleton, W. J. & Engelhardt, V. A. (1958). J. Am. Chem. Soc. 80, 2788-2795.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe(C12H8N2)3](C9H5N4O)2·0.5H2O

  • Mr = 975.81

  • Triclinic, [P \overline 1]

  • a = 9.3497 (3) Å

  • b = 14.1736 (4) Å

  • c = 18.6086 (6) Å

  • [alpha] = 94.462 (2)°

  • [beta] = 96.562 (1)°

  • [gamma] = 101.129 (1)°

  • V = 2391.12 (13) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.38 mm-1

  • T = 293 K

  • 0.55 × 0.35 × 0.15 mm

Data collection
  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.820, Tmax = 0.946

  • 38167 measured reflections

  • 10845 independent reflections

  • 6909 reflections with I > 2[sigma](I)

  • Rint = 0.043

Refinement
  • R[F2 > 2[sigma](F2)] = 0.049

  • wR(F2) = 0.134

  • S = 1.02

  • 10845 reflections

  • 661 parameters

  • 40 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.36 e Å-3

  • [Delta][rho]min = -0.43 e Å-3

Table 1
Selected bond lengths (Å)

Fe1-N6 1.9563 (19)
Fe1-N5 1.9654 (18)
Fe1-N4 1.9686 (19)
Fe1-N1 1.9752 (18)
Fe1-N2 1.9819 (18)
Fe1-N3 1.9836 (18)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1w-H11...N7 0.84 2.17 2.996 (5) 169
O1w-H12...N8i 0.84 2.25 3.078 (5) 169
Symmetry code: (i) x+1, y, z.

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2 and SAINT. 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.]) and Mercury (Macrae et al., 2006[Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.]); 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: HB6994 ).


Acknowledgements

We are grateful for financial assistance from the DG-RSDT and ANDRU (Diretion Générale de la Recherche Scientifique et du Développement Technologique et l'Agence Nationale pour le Développement de la Recherche Universitaire, Algéria) through the PNR project. We also acknowledge the Ministry of Higher Education of Malaysia (grant No·UM.C/HIR/MOHE/SC/12) for supporting this study.

References

Aparici Plaza, L., Baranowska, K. & Becker, B. (2007). Acta Cryst. E63, m1537-m1539.  [CSD] [CrossRef] [details]
Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.  [CrossRef] [ChemPort]
Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Cai, Z.-M. & Zhan, S.-Z. (2012). Acta Cryst. E68, m956.  [CSD] [CrossRef] [details]
Hoshina, G., Ohba, S., Tsuchiya, N., Isobe, T. & Senna, M. (2000). Acta Cryst. C56, e191-e192.  [CSD] [CrossRef] [details]
Hwang, I.-C. & Ha, K. (2006). Acta Cryst. E62, m376-m378.  [CSD] [CrossRef] [details]
Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.  [ISI] [CrossRef] [ChemPort] [details]
Middleton, W. J. & Engelhardt, V. A. (1958). J. Am. Chem. Soc. 80, 2788-2795.  [CrossRef] [ChemPort] [ISI]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]
Zhou, D.-P. & Guo, G.-L. (2007). Acta Cryst. E63, m1122-m1124.  [CSD] [CrossRef] [details]


Acta Cryst (2013). E69, m12-m13   [ doi:10.1107/S1600536812048611 ]

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