Abstract

The new transition metal oxo‐thiostannate {[Ni(cyclen)]6[Sn6S12O2(OH)6]}·2(ClO4)·19H2O (1) was prepared under hydrothermal conditions using Na4SnS4·14H2O and [Ni(cyclen)](ClO4)2 as reactants. In the crystal structure the rare [Sn6S12O2(OH)6]10– anion is observed, which is composed of SnS2O(OH)3 and SnS4O2 octahedra, and SnS4 tetrahedra sharing edges and corners. The anion is expanded by six Ni2+ centered complexes via Ni–S and Ni–OH bonds. The photocatalytic properties for the visible light driven hydrogen evolution reaction shows that 26.6 mmol·g–1 H2 were evolved after 3 h.

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