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A yellow [(HPO(3))(2)(P(2)O(7))Mo(30)O(90)](8-) anion was prepared as a tetrapropylammonium (Pr(4)N(+)) salt from a 50 mM Mo(VI)-2 mM P(2)O(7)(4-)-4 mM HPO(3)(2-)-0.95 M HCl-60% (v/v) CH(3)CN system at ambient temperature. The (Pr(4)N)(8)[(HPO(3))(2)(P(2)O(7))Mo(30)O(90)] salt crystallized in the orthorhombic space group P(nma) (No. 62), with a = 30.827(2) A, b = 22.8060(15) A, c = 30.928(2) A, V = 21743(3) A(3), and Z = 4. The structure contained a (P(2)O(7))Mo(12)O(42) fragment derived from the removal of each corner-shared Mo(3)O(13) unit in a polar position from a [(P(2)O(7))Mo(18)O(54)](4-) structure, and each side of the (P(2)O(7))Mo(12)O(42) fragment was capped by a B-type (HPO(3))Mo(9)O(24) unit. The [(HPO(3))(2)(P(2)O(7))Mo(30)O(90)](8-) anion was characterized by voltammetry and IR, UV-vis, and (31)P NMR spectroscopy. Unlike the Keggin and Dawson anions and the parent [(P(2)O(7))Mo(18)O(54)](4-) anion, the [(HPO(3))(2)(P(2)O(7))Mo(30)O(90)](8-) anion exhibited two-electron redox waves in CH(3)CN with and without acid.


Sayuri Maeda, Takuya Goto, Masayo Takamoto, Kazuo Eda, Sadayuki Himeno, Hiroki Takahashi, Toshitaka Hori. An approach to the synthesis of polyoxometalate encapsulating different kinds of oxoanions as heteroions: bisphosphitopyrophosphatotriacontamolybdate [(HPO3)2(P2O7)Mo30O90]8-. Inorganic chemistry. 2008 Dec 1;47(23):11197-201

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PMID: 18928278

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