Abstract
The structure of Na[NMe4]3S2Mo5O23·4H2O has been determined by the single-crystal X-ray method: monoclinic, space group P2/c, a= 29.25(2), b= 12.85(1), c= 18.24(1)A, and β= 123.89(2)° and Z= 6. The structure was refined by full-matrix least squares to R′= 0.0678 for 5532 reflections. The existence of the Strandberg-type heteropolyion [S2Mo5O23]4–1 in the crystals has been confirmed. The geometry of 1 was compared systematically with various analogues containing SIVO32–, PO43–, MePO32– or NH3C2H4PO3– as the central polyhedron. The UV spectrum of the salts Na[NMe4]3S2Mo5O23·4H2O and [NMe4]4S2Mo5O23 in neat MeCN, hence the kernel heteropolyion 1 showed absorption maxima at λ= 213 and 243 nm (Iµ= 3.2 × 104 and 3.3 × 104 dm3 mol–1 cm–1). Spectroscopic measurements also indicate that 1 and [Mo6O19]2– form simultaneously in aqueous–MeCN media containing MoVI and H2SO4.
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