Tris(1,10-phenanthroline-κ2N,N′)iron(II) bis­(1,1,3,3-tetra­cyano-2-eth­oxy­propenide) hemihydrate

Setifi, Z.; Setifi, F.; Ng, S.W.; Oudahmane, A.; El-Ghozzi, M.; Avignant, D.

doi:10.1107/S1600536812048611

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 (C-C) = 0.004 Å
Disorder in main residue
R = 0.049
wR = 0.134
Data-to-parameter ratio = 16.4
Details

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

Zouaoui Setifi,^a,^b Fatima Setifi,^c,^b ^* Seik Weng Ng,^d,^e Abdelghani Oudahmane,^f,^g Malika El-Ghozzi ^f,^g and Daniel Avignant ^f,^g

^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-HN 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); Hwang & Ha (2006); Aparici Plaza et al. (2007); Zhou & Guo (2007). For a related structure, see: Cai & Zhan (2012). For further synthetic details, see: Middleton & Engelhardt (1958).

Experimental

Crystal data

[Fe(C₁₂H₈N₂)₃](C₉H₅N₄O)₂·0.5H₂O
M_r = 975.81
Triclinic, $[P \overline 1]$
a = 9.3497 (3) Å
b = 14.1736 (4) Å
c = 18.6086 (6) Å
= 94.462 (2)°
= 96.562 (1)°
= 101.129 (1)°
V = 2391.12 (13) Å³
Z = 2
Mo K radiation
= 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) T_min = 0.820, T_max = 0.946
38167 measured reflections
10845 independent reflections
6909 reflections with I > 2(I)
R_int = 0.043

Refinement

R[F² > 2(F²)] = 0.049
wR(F²) = 0.134
S = 1.02
10845 reflections
661 parameters
40 restraints
H-atom parameters constrained
_max = 0.36 e Å^-3
_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-HA	D-H	HA	DA	D-HA
O1w-H11N7	0.84	2.17	2.996 (5)	169
O1w-H12N8ⁱ	0.84	2.25	3.078 (5)	169
Symmetry code: (i) x+1, y, z.

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001) and Mercury (Macrae et al., 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

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

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