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Volume 69 
Part 12 
Page m657  
December 2013  

Received 1 November 2013
Accepted 6 November 2013
Online 13 November 2013

Key indicators
Single-crystal X-ray study
T = 200 K
Mean [sigma](C-C) = 0.005 Å
R = 0.030
wR = 0.066
Data-to-parameter ratio = 18.0
Details
Open access

Bis(acetyl­acetonato-[kappa]2O,O')(pyridine-[kappa]N)(thio­cyanato-[kappa]N)manganese(III): a redetermination using data from a single crystal

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

In the crystal structure of the title compound, [Mn(C5H7O2)2(NCS)(C5H5N)], the Mn3+ cation is coordin­ated by two acetyl­acetonate anions, one terminal thio­cyanate anion and one pyridine ligand within a slightly distorted octa­hedron. The asymmetric unit consists of half a complex mol­ecule with the Mn3+ cation, the thio­cyanate anion and the pyridine ligand located on a mirror plane. The acetyl­acetonate anion is in a general position. The title compound was previously described [Stults et al. (1975[Stults, B. R., Marianelli, R. S. & Day, V. W. (1975). Inorg. Chem. 14, 722-730.]). Inorg. Chem. 14, 722-730] but could only be obtained as a powder. Suitable crystals have now been obtained for a high-precision single-crystal structure determination.

Related literature

For the preparation of the title compound in the form of a powder, see: Stults et al. (1975[Stults, B. R., Marianelli, R. S. & Day, V. W. (1975). Inorg. Chem. 14, 722-730.]).

[Scheme 1]

Experimental

Crystal data
  • [Mn(C5H7O2)2(NCS)(C5H5N)]

  • Mr = 390.33

  • Orthorhombic, C m c 21

  • a = 13.8803 (6) Å

  • b = 8.3195 (5) Å

  • c = 15.9035 (7) Å

  • V = 1836.49 (16) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.85 mm-1

  • T = 200 K

  • 0.17 × 0.14 × 0.09 mm

Data collection
  • STOE IPDS-2 diffractometer

  • Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]) Tmin = 0.802, Tmax = 0.883

  • 6523 measured reflections

  • 2267 independent reflections

  • 2090 reflections with I > 2[sigma](I)

  • Rint = 0.028

Refinement
  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.066

  • S = 1.04

  • 2267 reflections

  • 126 parameters

  • 1 restraint

  • H-atom parameters constrained

  • [Delta][rho]max = 0.22 e Å-3

  • [Delta][rho]min = -0.18 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1086 Friedel pairs

  • Absolute structure parameter: 0.015 (19)

Data collection: X-AREA (Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT6942 ).


Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/3-1) and the State of Schleswig-Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facilities.

References

Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [IUCr Journals]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.
Stults, B. R., Marianelli, R. S. & Day, V. W. (1975). Inorg. Chem. 14, 722-730.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m657  [ doi:10.1107/S1600536813030407 ]

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