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ISSN 1600-5368

Editors: W.T. A. Harrison, J. Simpson and

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Bis(2,3,5,6-tetra-2-pyridylpyrazine-3N 2,N 1,N 6)iron(II)

bis(dicyanamidate) 4.5-hydrate
L. Callejo, N. De la Pinta, G. Madariaga, M.L. Fidalgo and R. Cortes

Acta Cryst. (2010). E66, m249m250

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Acta Cryst. (2010). E66, m249m250

Callejo et al. [Fe(C24 H16 N6 )2 ](C2 N3 )2 4.5H2 O

metal-organic compounds
Acta Crystallographica Section E

Structure Reports
Online
ISSN 1600-5368

Bis(2,3,5,6-tetra-2-pyridylpyrazinej3N2,N1,N6)iron(II) bis(dicyanamidate)
4.5-hydrate
L. Callejo,a N. De la Pinta,a G. Madariaga,b* M.L. Fidalgoc
and R. Cortesc
a

Departamento de Qumica Inorganica, Facultad de Ciencia y Tecnologa,

Universidad del Pas Vasco, Apdo. 644, E-48080 Bilbao, Spain, bDepartamento de
Fsica de la Materia Condensada, Facultad de Ciencia y Tecnologa, Universidad del
Pas Vasco, Apdo. 644, E-48080 Bilbao, Spain, and cDepartamento de Qumica
Inorganica, Facultad de Farmacia, Universidad del Pas Vasco, Apdo. 450, E-01080
Vitoria, Spain
Correspondence e-mail: gotzon.madariaga@ehu.es
Received 13 December 2009; accepted 27 January 2010

;
Key indicators: single-crystal X-ray study; T = 293 K; mean (CC) = 0.004 A
disorder in solvent or counterion; R factor = 0.063; wR factor = 0.168; data-toparameter ratio = 20.4.

In the title compound, [Fe(C24H16N6)2][N(CN)2]24.5H2O, the

central iron(II) ion is hexacoordinated by six N atoms of two
tridentate 2,3,5,6-tetra-2-pyridylpyrazine (tppz) ligands. Two
dicyanamide anions [dca or N(CN)2] act as counter-ions, and
4.5 water molecules act as solvation agents. The structure
contains isolated cationic iron(II)tppz complexes and the
nal neutrality is obtained with the two dicyanamide anions.
One of the dicyanamide anions and a water molecule are
disordered with an occupancy ratio of 0.614 (8):0.386 (8). O
H  O, OH  N and CH  O hydrogen bonds involving
dca, water and tppz molecules are observed.

Experimental
Crystal data
[Fe(C24H16N6)2](C2N3)24.5H2O
Mr = 1045.88
Monoclinic, P21 =c

a = 13.9216 (7) A

b = 18.9271 (9) A

c = 19.1425 (9) A
 = 97.017 (4)

Data collection

For related structures including [M(II)(tppz)2]2+ cations, see:

Ruminski & Kiplinger (1990); Arana et al. (1992); Allis et al.
(2004); Burkholder & Zubieta (2004); Laine et al. (1995). For
the application of a [Co(II)(tppz)2]2+ complex as a homogeneous catalyst, see: Konigstein & Bauer (1994, 1997). For
dicyanamido (dca) anions, see: He et al. (2002). Some H-atom
positions were calculated using HYDROGEN (Nardelli,
1999).

15912 independent reections

8433 reections with I > 2(I)
Rint = 0.051

Oxford Diffraction Xcalibur 2

diffractometer
51234 measured reections

Renement
R[F 2 > 2(F 2)] = 0.063
wR(F 2) = 0.168
S = 1.02
15912 reections
779 parameters
135 restraints

H atoms treated by a mixture of

independent and constrained
renement
3

max = 0.86 e A
3

min = 0.34 e A

Table 1

,  ).
Hydrogen-bond geometry (A
DH  A
O1WH11W  N13
O1WH12W  N12i
O2WH21W  N15
O2WH22W  O1W
O3WH31W  N10
O3WH32W  O5WAii
O3WH32W  O4W
O3WH32W  O4W ii
O4WH41W  O5WA
O5WAH52A  N16A
O5WBH51B  N6
O5WBH52B  N16B
C8H8  O4W iii
i

Related literature

3
V = 5006.2 (4) A
Z=4
Mo K radiation
 = 0.37 mm1
T = 293 K
0.1  0.1  0.01 mm

DH

H  A

D  A

DH  A

0.84
0.86
0.85
0.86
0.86
0.86
0.86
0.86
0.85
0.85
0.85
0.86
0.93

2.17
1.98
2.16
1.96
2.32
2.29
2.11
2.41
1.95
2.19
2.52
2.22
2.45

2.862 (5)
2.830 (4)
2.903 (6)
2.785 (4)
2.909 (10)
2.87 (2)
2.46 (3)
3.24 (3)
2.72 (4)
2.92 (2)
3.188 (8)
3.057 (18)
3.349 (16)

139
173
146
160
126
126
104
162
153
143
136
164
162

(2)
(2)
(3)
(3)
(11)
(12)
(12)
(12)
(7)
(4)
(11)
(8)

(3)
(2)
(4)
(3)
(13)
(15)
(18)
(12)
(9)
(4)
(12)
(7)

(3)
(3)
(3)
(4)
(11)
(15)
(13)
(15)
(17)
(7)
(13)
(10)

Symmetry codes: (i) x; y 12; z 12; (ii) x 1; y; z 1; (iii) x; y 12; z  12.

Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell

renement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS86
(Sheldrick, 2008); program(s) used to rene structure: SHELXL97
(Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2006);
software used to prepare material for publication: WinGX (Farrugia,
1999).

Acta Cryst. (2010). E66, m249m250

doi:10.1107/S1600536810003363

electronic reprint

Callejo et al.

m249

metal-organic compounds
This work was supported by the Universidad del PasVasco
(UPV 00169.12513956/2004), the Ministerio de Ciencia y
Tecnologa (CTQ200505778-PPQ) and the Basque Government (project IT-28207). LC thanks the UPV/EHU for her
doctoral fellowship. NdelaP thanks the UPV/EHU for nancial support from Convocatoria para la concesion de ayudas
de especializacion para investigadores doctores en la UPV/
EHU (2008).
Supplementary data and gures for this paper are available from the
IUCr electronic archives (Reference: ZL2260).

References
Allis, D. G., Burkholder, E. & Zubieta, J. (2004). Polyhedron, 23, 11451152.

m250

Callejo et al.

[Fe(C24H16N6)2](C2N3)24.5H2O

Arana, C., Yan, S., Keshavarz, K. M., Potes, K. T. & Abruna, H. D. (1992).
Inorg. Chem. 31, 36803682.
Burkholder, E. & Zubieta, J. (2004). Inorg. Chim. Acta, 357, 12291235.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837838.
He, Y., Kou, H.-Z., Zhou, B. C., Xiong, M., Wang, R.-J. & Li, Y. (2002). Acta
Cryst. E58, m389m391.
Konigstein, C. & Bauer, R. (1994). Hydrogen Energy Progress X (Proc. 10th
World Hydrogen Energy Conf.), Vol. 2, edited by D. L. Block & T. N.
Veziroglu, pp. 717725. Coral Gables: International Association for
Hydrogen Energy.
Konigstein, C. & Bauer, R. (1997). Int. J. Hydrogen Ener. 22, 471474.
Laine, P., Gourdon, A. & Launay, J. P. (1995). Inorg. Chem. 34, 51565165.
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, 453457.
Nardelli, M. (1999). J. Appl. Cryst. 32, 563571.
Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, England.
Ruminski, R. R. & Kiplinger, J. L. (1990). Inorg. Chem. 29, 45814584.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112122.

electronic reprint

Acta Cryst. (2010). E66, m249m250


 
  

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