[Journal logo]

Volume 64 
Part 1 
Page m1  
January 2008  

Received 6 November 2007
Accepted 21 November 2007
Online 6 December 2007


[Cited in]
[Download citation]

© International Union of Crystallography 2008

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.003 Å
R = 0.041
wR = 0.108
Data-to-parameter ratio = 19.1
Details

{Tris[2-(imidazol-2-ylmethylimino)ethyl]methylammonium}iron(II) tris(perchlorate) dihydrate

Greg A. Brewer,a Jerry P. Jasinskib* and Ray J. Butcherc

aDepartment of Chemistry, Catholic University, 620 Michigan Ave. NE, Washington, DC 20064, USA,bDepartment of Chemistry, Keene State College, 229 Main Street, Keene, NH 03435-2001, USA, and cDepartment of Chemistry, Howard University, 525 College Street NW, Washington DC 20059 USA
Correspondence e-mail: jjasinski@keene.edu

The title complex, [Fe(C19H27N10)](ClO4)3·2H2O, is a new polymorph of an iron(II) Schiff base complex of tris(2-aminoethyl)methylammonium with imidazole-2-carboxaldehyde. The octahedral FeII atom is bound to three facial imidazole N atoms with average Fe-Nimidazole and Fe-Nimine bond distances of 1.963 (5) and 1.951 (5) Å, respectively. The central N atom of the tripodal ligand is outside the bonding distance at 3.92 Å. The crystal packing is stabilized by the hydrogen-bonding interactions between the two water molecules (acceptor) and two of the three imidazole NH groups (donor). The third imidazole NH group (donor) forms a hydrogen bond to one of the three perchlorate counter-ions (acceptor).

Related literature

For the synthesis, see: Brewer et al. (2005[Brewer, C., Brewer, G., Patil, G., Sun, Y., Viragh, C. & Butcher, R. J. (2005). Inorg. Chim. Acta. 358, 3441-3448.]). For related structures, see: Brewer et al. (2006[Brewer, G., Olida, M. J., Schmiedekamp, A. M., Viragh, C. & Zavalij, P. (2006). Dalton Trans. pp. 5617-5629.], 2007[Brewer, G., Butcher, R. J., Viragh, C. & White, G. (2007). Dalton Trans. pp. 4132-4142.]).

[Scheme 1]

Experimental

Crystal data

  • [Fe(C19H27N10)](ClO4)3·2H2O

  • Mr = 785.74

  • Orthorhombic, P b c a

  • a = 13.9630 (18) Å

  • b = 11.7810 (15) Å

  • c = 37.182 (5) Å

  • V = 6116.4 (14) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 0.84 mm-1

  • T = 173 K

  • 0.54 × 0.45 × 0.12 mm
Data collection

  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.682, Tmax = 0.904

  • 65065 measured reflections

  • 8324 independent reflections

  • 6601 reflections with I > 2[sigma](I)

  • Rint = 0.054
Refinement

  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.108

  • S = 1.04

  • 8324 reflections

  • 436 parameters

  • 6 restraints

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

  • [Delta][rho]max = 0.76 e Å-3

  • [Delta][rho]min = -0.62 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1W-H1W2...O14i 0.807 (19) 2.29 (4) 2.938 (3) 138 (5)
O2W-H2W1...O14ii 0.820 (17) 2.26 (2) 2.987 (3) 148 (4)
O2W-H2W2...O22iii 0.821 (18) 2.07 (2) 2.861 (3) 160 (4)
N3A-H3AB...O2W 0.88 1.91 2.730 (3) 155
N3B-H3BB...O1W 0.88 1.95 2.752 (3) 152
N3C-H3CB...O14 0.88 2.05 2.907 (3) 163
Symmetry codes: (i) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z]; (ii) x, y+1, z; (iii) [-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z].

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2006[Bruker (2006). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990[Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997). SHELXL97. University of Göttingen, Germany.]); molecular graphics: SHELXTL (Bruker, 2000[Bruker (2000). SMART and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.]); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2214 ).

Acknowledgements

RJB acknowleges the Laboratory for the Structure of Matter at the Naval Research Laboratory for access to their diffractometers.

References

Brewer, C., Brewer, G., Patil, G., Sun, Y., Viragh, C. & Butcher, R. J. (2005). Inorg. Chim. Acta. 358, 3441-3448.  [CrossRef] [ChemPort]
Brewer, G., Butcher, R. J., Viragh, C. & White, G. (2007). Dalton Trans. pp. 4132-4142.  [CrossRef]
Brewer, G., Olida, M. J., Schmiedekamp, A. M., Viragh, C. & Zavalij, P. (2006). Dalton Trans. pp. 5617-5629.  [CrossRef]
Bruker (2000). SMART and SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2006). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473.  [CrossRef] [details]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (1997). SHELXL97. University of Göttingen, Germany.

Acta Cryst (2008). E64, m1  [ doi:10.1107/S1600536807061673 ]