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

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 in the literature.

SUBMITTER: Danker F 

PROVIDER: S-EPMC7057377 | biostudies-literature | 2020 Mar

REPOSITORIES: biostudies-literature