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1 Bulletin of the Polish Academy of Sciences. Chemistry

1 2002

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Dithiocarbonate and trithiocarbonate complexes derived from VV, MoVI, ReVII tetraoxothioprecursors

Dessapt R., Simonnet-Jegat C., Secheresse F.

Bulletin of the Polish Academy of Sciences. Chemistry

2002

Vol. 50, No. 1

15-25

Reactions of MoS(2)/(4), MoO(2)S(2)(2-), MoO(2)(4), ReSJ, ReO-(4), VS(3)/(4), and VO(3-)(4) with CS(2) are described. The syntheses and X-ray determinations of (NEt(4))(2) [Mo2(S)(2) (Mo(2) S)(2) (u -S)(2)], space group P2(1)/C, a = 9.3169(3) A,b = 16.3211(5) A, c = 22.8415(5) A, Beta = 92.590(1)°, V = 3469.8(2) A3, R = 0.0898 for 8720 independent reflections and (NEt(4))(2)[Mo(2)(O)(2)(Mi - S)(mi - O)(n(2) - COS(2)2] 0.5 CS(2), space group P2(1)/C, a = 9.8190(1) A, b = 20.6313(13) A, c = 15.7193(3) A, Beta = 92.353(1)°, V = 3181.71(8) A(3), R = 0.0576 for 5760 independent reflections are presented. A rationalization of the syntheses is discussed and the structure of (NH4)[HCOS(2) is described, space group Pca2i, a = 8.3174(9) A, b = 5.6562(6) A, c = 10.7125(12) A, V = 503.97(9) A3, R = 0.0402 for 952 independent reflections. (13)C NMR data for trithiocarbonate and dithiocarbonate complexes are presented.