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The effect of cations in a reaction mixture for the preparation of the Preyssler‐Jeannin‐Pope type 30‐tungsto‐5‐phosphate [P5W30O110Na]14– is investigated. Reaction of phosphate and tungstate with a P/W ratio of ca. 3.9 in an acidic aqueous solution without cations selectively leads to the Dawson‐type 18‐tungsto‐2‐phosphate, [P2W18O62]6–. Amongst all the alkali cations, only Na+ allows formation of...
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