Synthesis and crystal structure of (1,4,7,10-tetraazacyclododecane- κ 4N)(tetrasulfido- κ 2S1,S4)manganese(II)

The title compound, [Mn(S4)(C8H20N4)], was accidentally obtained by the hydrothermal reaction of Mn(ClO4)2 · 6H2O, cyclen (cyclen = 1,4,7,10-tetraazacyclododecane) and Na3SbS4 · 9H2O in water at 413   K, indicating that polysulfide anions might represent intermediates in the synthesis of thiometallate 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 intermolecular N — H...S and C — H...S hydrogen bonding. It is noted that only one similar complex with MnII is reported in the literature.

Source: Acta Crystallographica Section E - February 27, 2020 Category: Chemistry Authors: Danker, F. N ä ther, C. Bensch, W. Tags: crystal structure polysulfide manganese(II) discrete complex hydrogen bonding research communications Source Type: research