Synthesis and crystal structure of (1,4,7,10-tetra-aza-cyclo-dodecane-κ4N )(tetra-sulfido-κ2S1 ,S4 )manganese(II)

Acta Crystallographica. Section E, Crystallographic Communications
Felix DankerWolfgang Bensch

Abstract

The title compound, [Mn(S4)(C8H20N4)], was accidentally obtained by the hydro-thermal reaction of Mn(ClO4)2·6H2O, cyclen (cyclen = 1,4,7,10-tetra-aza-cyclo-dodeca-ne) and Na3SbS4·9H2O in water at 413 K, indicating that polysulfide anions might represent inter-mediates in the synthesis of thio-metallate compounds using Na3SbS4·9H2O as a reactant. X-ray powder diffraction proves that the sample is slightly contaminated with NaSb(OH)6 and an unknown crystalline phase. The crystal investigated was twinned with a twofold rotation axis as the twin element, and therefore a twin refinement using data in HKLF-5 format was performed. The asymmetric unit of the title compound consists of one MnII cation, one [S4]2- anion and one cyclen ligand in general positions. The MnII cation is sixfold coordinated by two cis-S atoms of the [S4]2- anions, as well as four N atoms of the cyclen ligand within an irregular coordination. The complexes are linked via pairs of N-H⋯S hydrogen bonds into chains, which are further linked into layers by additional N-H⋯S hydrogen bonding. These layers are connected into a three-dimensional network by inter-molecular N-H⋯S and C-H⋯S hydrogen bonding. It is noted that only one similar complex with MnII is reported ...Continue Reading

References

Feb 15, 2001·Acta Crystallographica. Section C, Crystal Structure Communications·R StählerW Bensch
Dec 25, 2007·Acta Crystallographica. Section A, Foundations of Crystallography·George M Sheldrick
Jul 14, 2011·Environmental Science & Technology·Britta Planer-Friedrich, Andreas C Scheinost
Jan 9, 2015·Acta Crystallographica. Section C, Structural Chemistry·George M Sheldrick
Apr 7, 2016·Acta Crystallographica Section B, Structural Science, Crystal Engineering and Materials·Colin R GroomSuzanna C Ward
Jan 11, 2020·Acta Crystallographica. Section E, Crystallographic Communications·Anthony L Spek

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Citations

Jul 3, 2021·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Melyssa L GrieveBrett M Paterson

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Methods Mentioned

BETA
X-ray

Software Mentioned

PLATON

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