Bis[4-(dimethyl­amino)­pyridinium] bis­[4-(dimethyl­amino)­pyridine-κN1]tetra­kis­(thio­cyanato-κN)manganate(II)

Wöhlert, S.; Jess, I.; Näther, C.

doi:10.1107/S1600536812047678

Volume 68
Part 12
Page m1528
December 2012

Received 15 November 2012
Accepted 20 November 2012
Online 24 November 2012

Key indicators
Single-crystal X-ray study
T = 180 K
Mean (C-C) = 0.003 Å
R = 0.044
wR = 0.121
Data-to-parameter ratio = 20.8
Details

Bis[4-(dimethylamino)pyridinium] bis[4-(dimethylamino)pyridine-N¹]tetrakis(thiocyanato-N)manganate(II)

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 crystal structure of the title compound, (C₇H₁₁N₂)₂[Mn(NCS)₄(C₇H₁₀N₂)₂], the manganese(II) cations are coordinated by four N-bonded thiocyanate anions and two N-bonded 4-(dimethylamino)pyridine ligands into discrete complex dianions. For charge balance, two 4-(dimethylamino)pyridine counter cations are present, which do not coordinate to the metal cation. The asymmetric unit consists of one manganese(II) cation, four thiocyanate anions and two 4-(dimethylamino)pyridine ligands, as well as two protonated 4-(dimethylamino)pyridinium cations. The discrete complex anions are connected to the non-coordinating pyridinium cations by weak N-HS hydrogen-bonding interactions.

Related literature

For general background, see: Boeckmann & Näther (2011, 2012).

Experimental

Crystal data

(C₇H₁₁N₂)₂[Mn(NCS)₄(C₇H₁₀N₂)₂]
M_r = 777.96
Triclinic, $[P \overline 1]$
a = 11.7307 (8) Å
b = 11.9010 (9) Å
c = 15.4224 (12) Å
= 102.520 (9)°
= 96.794 (9)°
= 107.400 (8)°
V = 1966.6 (3) Å³
Z = 2
Mo K radiation
= 0.59 mm^-1
T = 180 K
0.18 × 0.11 × 0.05 mm

Data collection

Stoe IPDS-1 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) T_min = 0.873, T_max = 0.968
24452 measured reflections
9338 independent reflections
6752 reflections with I > 2(I)
R_int = 0.041

Refinement

R[F² > 2(F²)] = 0.044
wR(F²) = 0.121
S = 1.02
9338 reflections
450 parameters
H-atom parameters constrained
_max = 0.80 e Å^-3
_min = -0.72 e Å^-3

Table 1
Selected bond lengths (Å)

Mn1-N1	2.1928 (17)
Mn1-N2	2.2014 (19)
Mn1-N3	2.2468 (19)
Mn1-N4	2.2535 (18)
Mn1-N20	2.2561 (16)
Mn1-N10	2.2659 (16)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N30-H30S4	0.88	2.36	3.217 (2)	165
N40-H40AS3ⁱ	0.88	2.35	3.213 (3)	166
Symmetry code: (i) x+1, y+1, z+1.

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: VM2182 ).

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

Bis[4-(dimethylamino)pyridinium] bis[4-(dimethylamino)pyridine-N1]tetrakis(thiocyanato-N)manganate(II)