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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.
Highlights
Investigations on the synthesis and crystal structures of new inorganic–organic chalcogenidometallates are an important topic in inorganic chemistry and many such compounds have been reported in the literature (Sheldrick & Wachhold, 1988; Dehnen & Melullis, 2007; Seidlhofer et al, 2010, 2011; Wang et al, 2016; Zhou, 2016; Zhu & Dai, 2017; Nie et al, 2017)
The structure consists of discrete complexes, in which manganese is coordinated by one cyclen ligand and one tetrasulfide dianion that must have formed in situ from Na3SbS4
This finding is of special interest because it indicates that polysulfide species might represent intermediates in the synthesis of thiometallate compounds using Na3SbS4 as reactant
Summary
Investigations on the synthesis and crystal structures of new inorganic–organic chalcogenidometallates are an important topic in inorganic chemistry and many such compounds have been reported in the literature (Sheldrick & Wachhold, 1988; Dehnen & Melullis, 2007; Seidlhofer et al, 2010, 2011; Wang et al, 2016; Zhou, 2016; Zhu & Dai, 2017; Nie et al, 2017) In this context, thioantimonates are of special interest because they show a variety of coordination numbers and can form networks of different dimensionality (Schur et al, 2001; Jia et al, 2004; Powell et al, 2005; Zhang et al, 2007; Liu & Zhou, 2011; Engelke et al, 2004; Puls et al, 2006). The title compound cannot be obtained as a pure crystalline phase if the reaction conditions are varied and no further investigations were performed
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Schedule a callMore From: Acta crystallographica. Section E, Crystallographic communications
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