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The new compound K 2 [Ni(dien) 2 ]{[Ni(dien)] 2 Ta 6 O 19 }·11 H 2 O crystallized at room temperature applying a diffusion based reaction in a H 2 O/DMSO mixture using K 8 {Ta 6 O 19 }·16 H 2 O, Ni(NO 3 ) 2 ·6H 2 O and dien (diethylenetriamine). In the crystal structure, the Lindqvist-type anion [Ta 6 O 19 ] 8–  is structurally expanded by two octahedrally Ni 2+ -centered complexes via three Ni– µ   2 -O–Ta bonds thus generating the new {[Ni(dien)] 2 Ta 6 O 19 } 4–  anion. Two KO 8  polyhedra share a common edge to form a K 2 O 14  moiety, which connects the {[Ni(dien)] 2 Ta 6 O 19 } 4–  cluster shells into chains. The isolated [Ni(dien) 2 ] 2+  complexes are located in voids generated by the structural arrangement of the chains. An extended hydrogen bonding network between the different constituents generates a 3D network. The crystal water molecules can be thermally removed to form a highly crystalline dehydrated compound. Partial water uptake leads to the formation of a crystalline intermediate with a reduced unit cell volume compared to the fully hydrated sample. Water sorption experiments demonstrate that the fully dehydrated sample can be fully reconverted to the hydrated compound. The crystal field splitting parameters for the octahedrally coordinated Ni 2+ -centered complexes have been evaluated from an UV/Vis spectrum yielding  D   q  = 1056 cm −1  and  B  = 887 cm −1 .

Synthesis, crystal structure and selected properties of K 2 [Ni(dien) 2 ]{[Ni(dien)] 2 Ta 6 O 19 }·11 H 2 O