Synthesis and crystal structure of (1,4,7,10-tetra-aza-cyclo-dodecane-κ(4) N)(tetra-sulfido-κ(2) S (1),S (4))manganese(II).

The title compound, [Mn(S(4))(C(8)H(20)N(4))], was accidentally obtained by the hydro-thermal reaction of Mn(ClO(4))(2)·6H(2)O, cyclen (cyclen = 1,4,7,10-tetra-aza-cyclo-dodeca-ne) and Na(3)SbS(4)·9H(2)O in water at 413†K, indicating that polysulfide anions might represent inter-mediates in the synthesis of thio-metallate compounds using Na(3)SbS(4)·9H(2)O 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 Mn(II) cation, one [S(4)](2-) anion and one cyclen ligand in general positions. The Mn(II) cation is sixfold coordinated by two cis-S atoms of the [S(4)](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 Mn(II) is reported in the literature.