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The new thiostannate Na4Sn2S6 was prepared by directed crystal water removal from the hydrate Na4Sn2S6 ⋅ 5H2O at moderate temperatures. While the structure of the hydrate comprises isolated [Sn2S6]4− anions, that of the anhydrate contains linear chains composed of corner‐sharing SnS4 tetrahedra, a structural motif not known in thiostannate chemistry. This structural rearrangement requires bond‐breakage...
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