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The new polyoxotungstate (NH 4 ) 6 Na 4 [Ni 4 (H 2 O) 2 (AsW 9 O 34 ) 2 ] · 20 H 2 O (1) was synthesized in aqueous solution and characterized by IR and UV/Vis spectroscopy, energy dispersive X-ray fluorescence and single-crystal X-ray analysis. It contains the tetra-nickel substituted [Ni 4 (H 2 O) 2 (AsW 9 O 34 ) 2 ] 10−  polyoxoanion, in which the four Ni atoms are in a common plane and form a regular rhombus. 1 crystallizes in the monoclinic crystal system, space group P2 1 /n with a = 11.849(2), b = 16.718(3), c = 21.243(4) Å , β = 100.48(3)◦, and Z = 2. The anions are linked via hydrogen bonds and sodium cations.

Synthesis and Crystal Structure of the Tetra-nickel Substituted [Ni 4 (H 2 O) 2 (AsW 9 O 34 ) 2 ] 10- Polyoxoanion