Extending the Time: Solvothermal Syntheses, Crystal Structures, and Properties of Two Non-isostructural Thioantimonates with the Composition [Mn(tren)]Sb(2)S(4).
The two novel compounds, [Mn(tren)]Sb(2)S(4) (1 and 2), were obtained by the reaction of elemental Mn, Sb, and S in aqueous solutions of tren (tren = tris(2-aminoethyl)amine, C(6)H(18)N(4)) after different reaction times. Compound 1 is formed up to a reaction time of 13 d, and an extension of the reaction time leads to the formation of 2. Both compounds crystallize in monoclinic space groups (1, P2(1)/c; 2, C2/c). In 1, the two unique SbS(3) trigonal pyramids share a common S atom to form a Sb(2)S(5) unit. Two S atoms of this group have a bond to Mn(2+) yielding a MnSb(2)S(3) heteroring in the boat conformation. The Sb(2)S(5) moieties are joined via common corners into the final undulated [Sb(2)S(4)](2)(-) anion which is directed along [001]. The structure of 2 contains the [Mn(tren)](2+) ion, one SbS(3) pyramid, and a SbS(4) unit. Two symmetry-related SbS(4) groups share an edge, forming a Sb(2)S(6) group containing a Sb(2)S(2) ring. This group is joined via corners to two SbS(3) pyramids on both sides producing a Sb(4)S(4) ring. The Sb(2)S(2) and Sb(4)S(4) rings are condensed into the final [Sb(2)S(4)](2)(-) anion which runs along [010]. The [Mn(tren)] groups are bound to the thioantimonate(III) backbone on opposite sides of the Sb(4)S(4) ring, and a small MnSbS(2) ring is formed. In both structures, weak S...H bonds are found which may contribute to the stability of the materials. The two compounds decompose in one step upon heating, and only MnS and Sb(2)S(3) could be identified as the crystalline part of the decomposition products. Both compounds can also be prepared under solvothermal conditions using MnSb(2)S(4) as starting material. Compounds 1 and 2 are obtained from this ternary material in a high yield.[1]References
- Extending the Time: Solvothermal Syntheses, Crystal Structures, and Properties of Two Non-isostructural Thioantimonates with the Composition [Mn(tren)]Sb(2)S(4). Schaefer, M., Kurowski, D., Pfitzner, A., Näther, C., Rejai, Z., Möller, K., Ziegler, N., Bensch, W. Inorganic chemistry. (2006) [Pubmed]
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