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• W1978714596 abstract "Syntheses and 31P and 183W NMR structural characterization of a novel Dawson-type tungstophosphate [H4PW18O62]7– and of its lacunary and zinc-substituted derivatives [H4PW17O61]11– and [Zn(H2O)(H4PW17O61)]9–. Three novel polyoxotungstophosphates have been synthesized as potassium salts: a Dawson-type octadecatungstomonophosphate, K7[H4PW18O62] and its lacunary and zinc-substituted derivatives K11[H4PW17O61] and K9[Zn(H2O)(H4PW17O61]. The saturated compound was obtained by refluxing for 60 h a mixture of sodium tungstate and phosphoric acid (W/P=20) at pH 2.2. 31P-NMR spectroscopy showed the formation of a single product only after prolonged heating, while a mixture of three isomers was initially obtained. The derivatives were obtained by controlled alkaline degradation as usual for Dawson-type compounds. The structure of [H4PW18O62]7– (abbreviated as PW18) and of its derivatives was inferred from the comparison of their spectroscopic and electrochemical features with those of [P2W18O62]6– (P2W18). The 31P-NMR spectrum of each of these species displays a unique signal at −6.7 ppm for PW18, −2.05 ppm for PW17 and −2.95 ppm for PW17Zn. When compared with P2W18 (−12.45 ppm), with the PW8 unit of α2-P2W17 (−7.1 ppm) and the PW8Zn unit of α2-P2W17Zn (−8.6 ppm), the data for PW17 and PW17Zn are consistent with the removal or the replacement of one tungsten atom in a PW9 half-unit. Moreover, in the region of the PO stretching vibrations the IR spectra of PW17 and PW17Zn exhibit only one band, which is in favour of the removal of a tungsten atom from the cap of the PW9 unit. The 183W-NMR spectrum of PW18 exhibits four resonances at −181.3 (6W; d, 2JWOP=1.46 Hz) and −144.9 ppm (3W; d, 2JWOP=1.26 Hz) assigned to the PW9 unit, and at −127.8 ppm (6W; s) and −135.7 ppm (3W; s) assigned to the HnW9 unit. The three homonuclear 2JWOW coupling constants are in the range 20–27 Hz, which further confirms that the PW18 anion, like P2W18 consists of two A-type half-anions. Attempts to locate the four protons by 1H-NMR and to solve the crystal structure of PW18 by X-ray diffraction have been so far unsuccessful; however the isolated compound is probably the α isomer and the two minor products could be the β or γ isomers. The related tungstoarsenates were also obtained in similar conditions. © 2000 Académie des sciences / Éditions scientifiques et médicales Elsevier SASpolyoxometalates / Dawson-type tungstophosphates / 31P NMR / 183W NMR Trois nouveaux polytungstophosphates ont été synthetisés sous forme de sels de potassium : un octadécatungstomonophosphate, K7[H4PW18O62] et deux de ses dérivés, K11[H4PW17O61] et K9[Zn(H2O)(H4PW17O61)]. Leurs caractéristiques électrochimiques et spectroscopiques (IR et RMN 31P et 183W) ont été déterminées et comparées à celles du polyanion K6[P2W18O62] et de ses dérivés. Cette étude a démontré que le polyanion [H4PW18O62]7– possède une structure de type Dawson, constituée de deux demi-anions Aα-XW9 différents. C’est, à notre connaissance, la première description d’un polyoxotungstate de type Dawson ne contenant qu’un hetéroatome central. Comme K6[P2W18O62], cet anion permet d’accéder aux dérivés lacunaires et substitués." @default.
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• W1978714596 title "Synthèse et étude structurale par RMN 31P et 183W d’un octadécatungstomonophosphate de type Dawson [H4PW18O62]7– et de deux de ses dérivés, [H4PW17O61]11– et [Zn(H2O)(H4PW17O61)]9–" @default.
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• W1978714596 doi "https://doi.org/10.1016/s1387-1609(00)00112-2" @default.
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