A sandwich-type anionic cluster of a new lacunary building block [P(2)W(13)O(51)](14-) has been prepared: [H(6){P(2)W(13)O(51)}(2)Sb(4)](10-) (1) was synthesized in a one-pot self-assembly reaction of [H(2)P(2)W(12)O(48)](12-) with C(4)H(4)KO(7)Sb.0.5H(2)O and characterized by single-crystal X-ray analysis, IR, thermogravimetric analysis, elemental analysis, UV, NMR and electrochemistry. 1 represents the first dimetric, antimony-containing polyoxoanion derived from a vacant Dawson-type tungstophosphate.
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