The hydrothermal reaction of thiosalicylic acid, (C₆H₄(CO₂H)(SH)-1,2) with manganese(III) acetate leads to formation of the coordination solid [Mn₅((C₆H₄(CO₂)(S)-1,2)₂)₄(μ₃-OH)₂] (1) via a redox reaction, where resulting manganese(II) centres are coordinated by oxygen donor atoms and S–S disulfide bridge formation is simultaneously observed. Reaction of the same ligand under similar conditions with zinc(II) chloride yields the layered coordination solid [Zn(C₆H₄(CO₂)(S)-1,2)] (2). Hydrothermal treatment of manganese(III) acetate with 2-mercaptonicotinic acid, (NC₅H₃(SH)(CO₂H)-2,3) was found to produce the 1-dimensional chain structure [Mn₂((NC₅H₃(S)(CO₂)-2,3)₂)₂(OH₂)₄]·4H₂O (3) which also exhibits disulfide bridge formation and oxygen-only metal interactions. Compound 3 has been studied by thermogravimetric analysis and indicates sequential loss of lattice and coordinated water, prior to more comprehensive ligand fragmentation at elevated temperatures. The magnetic behaviour of 1 and 3 has been investigated and both exhibit antiferromagnetic interactions. The magnetic behaviour of 1 has been modelled as two corner-sharing isosceles triangles whilst 3 has been modelled as a 1-dimensional chain.