title: A strategy for the preparation of thioantimonates based on the concept of weak acids and corresponding strong bases.
abstract: By following a new synthetic approach, which is based on the in situ formation of a basic medium by the reaction between the strong base Sb(V)S4 (3-) and the weak acid H2 O, it was possible to prepare three layered thioantimonate(III) compounds of composition [TM(2,2'-bipyridine)3 ][Sb6 S10 ] (TM=Ni, Fe) and [Ni(4,4'-dimethyl-2,2'-bipyridine)3 ][Sb6 S10 ] under hydrothermal conditions featuring two different thioantimonate(III) network topologies. The antimony source, Na3 SbS4 ⋅ 9 H2 O, undergoes several decomposition reactions and produces the Sb(III) S3 species, which condenses to generate the layered anion. The application of transition-metal complexes avoids crystallization of dense phases. The reactions are very fast compared to conventional hydrothermal/solvothermal syntheses and are much less sensitive to changes of the reaction parameters.
authors.affiliation: Institute for Inorganic Chemistry, Christian-Albrechts University of Kiel, Max-Eyth-Straße 2, 24118 Kiel (Germany).
authors.forename: Carolin
authors.initials: C
authors.lastname: Anderer
authors.forename: Natalie
authors.initials: N
authors.lastname: Delwa de Alarcón
authors.forename: Christian
authors.initials: C
authors.lastname: Näther
authors.forename: Wolfgang
authors.initials: W
authors.lastname: Bensch
keywords: antimony; crystal structures; solvothermal synthesis; synthesis design; thioantimonates