Tris[4-(dimethyl­amino)­pyridinium] hexa­kis­(thio­cyanato-κN)ferrate(III) monohydrate

Wöhlert, S.; Jess, I.; Näther, C.

doi:10.1107/S1600536812049574

Volume 69
Part 1
Page m33
January 2013

Received 13 November 2012
Accepted 3 December 2012
Online 8 December 2012

Key indicators
Single-crystal X-ray study
T = 180 K
Mean (C-C) = 0.005 Å
R = 0.042
wR = 0.104
Data-to-parameter ratio = 17.1
Details

Tris[4-(dimethylamino)pyridinium] hexakis(thiocyanato-N)ferrate(III) monohydrate

Susanne Wöhlert,^a ^* Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
Correspondence e-mail: swoehlert@ac.uni-kiel.de

In the title compound, (C₇H₁₁N₂)₃[Fe(NCS)₆]·H₂O, the Fe^III cation is coordinated by six terminal N-bonded thiocyanate anions into a discrete threefold negatively charged complex. Charge balance is achieved by three protonated 4-(dimethylamino)pyridine cations. The asymmetric unit consists of one Fe^III cation, six thiocyanate anions, three 4-(dimethylamino)pyridinium cations and one water molecule, all of them located in general positions.

Related literature

For general background to our work on the synthesis and characterization of coordination compounds based on transition metal thiocyanates and neutral N-donor co-ligands such as pyridine, see: Boeckmann & Näther (2011, 2012).

Experimental

Crystal data

(C₇H₁₁N₂)₃[Fe(NCS)₆]·H₂O
M_r = 791.88
Triclinic, $[P \overline 1]$
a = 11.5780 (7) Å
b = 11.7620 (7) Å
c = 16.5450 (11) Å
= 81.260 (7)°
= 71.550 (7)°
= 62.950 (6)°
V = 1903.4 (2) Å³
Z = 2
Mo K radiation
= 0.77 mm^-1
T = 180 K
0.13 × 0.08 × 0.06 mm

Data collection

Stoe IPDS-1 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) T_min = 0.808, T_max = 0.947
13617 measured reflections
7356 independent reflections
4936 reflections with I > 2(I)
R_int = 0.075

Refinement

R[F² > 2(F²)] = 0.042
wR(F²) = 0.104
S = 0.95
7356 reflections
431 parameters
H-atom parameters constrained
_max = 0.34 e Å^-3
_min = -0.50 e Å^-3

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2012); software used to prepare material for publication: XCIF in SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HP2051 ).

Acknowledgements

We gratefully acknowledge financial support by the State of Schleswig-Holstein and the Deutsche Forschungsgemeinschaft (project 720/3-1). We thank Professor Dr Wolfgang Bensch for access to his experimental facility.

References

Boeckmann, J. & Näther, C. (2011). Dalton Trans. 39, 11019-11026.
Boeckmann, J. & Näther, C. (2012). Polyhedron, 31 587-595.
Brandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.

metal-organic compounds