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Chemija / Chemistry

ISSN 0235-7216
ISSN 2424-4538 (online)

2012 m. Nr. 1

Synthesis of monoselenanedisulfanediphosphonate by the reaction of selenous acid with thiophosphate in the presence of ascorbic acid
Feliksas SAVICKAS, Vitalijus JANICKIS

The reaction between selenous acid, H2SeO3, potassium dihydrogenmonothiophosphate, KH2SPO3, and ascorbic acid, C6H8O6, in the solution of acetic acid proceeds with the formation of monoselenanedi(monothiophosphate) – monoselenanedisulfanediphosphonate, Se(SPO3)2 4– – SeS2P2O6 4–, which in certain conditions is isolated from the reaction mixture as the crystalline salt trans-dipyridine-bis (dimethylglyoximato)cobalt(III) trihydrogenmonoselenane-disulfanediphosphonate dihydrate, [Co(DH)2Py2]H3SeS2P2O6 · 2H2O. The isolated compound is characterized by the chemical analysis, XRD pattern, thermogravimetric and differential thermal analysis methods, and IR spectra. The dehydration of the isolated compound proceeds at a temperature of ~55–100 °C and its decomposition begins at ~120 °C.
The final product of [Co(DH)2Py2]H3SeS2P2O6 · 2H2O decomposition at high temperature is cobalt(II) metaphosphate, Co(PO3)2. The IR spectra of the isolated compound showed the maxima of absorption bands characteristic of monoselenanedisulfanediphosphonate anion at 255; 278; 360, 386, 390; 424, 442; 470, 514, 589; 652, 693, 744, 769; 917, 953, 980, 1 037; 1 070, 1 092, 1 147, 1 173 and 1 238 cm–1; they are assigned to δ (S–Se–S), ν (Se–S), γr (PO3), ν (P–S), δas (O–P–O), δs (O–P–O), νs (P–O), νas (P–O), respectively.

Keywords: monoselenanedisulfanediphosphonate, formation, thermogravimetry, IR spectra

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