1989
DOI: 10.1071/ch9890837
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Synthesis and X-Ray Structure of syn-Di-μ-thio-bis[(N,N-diethyldithiocarbamato-S,S')oxotungsten(V)]

Abstract: The reaction of WSCl4 and Me3SiS2CNEt2 in tetrahydrofuran produces a green solid which yields WS(S2)(S2CNEt2)2, WO(S2)(S2CNEt2)2 and syn-W2O2( �-S)2(S2CNEt2)2 upon exposure to oxygen. Crystals of syn-W2O2( �-S)2(S2CNEt2)2 are monoclinic and belong to space group C2/c with a 33.880(4), b 7.012(1), c 18.072(1) � ,β 105.94(1)� and Z 8. Refinement on 2651 data measured with Cu K α: radiation converged at R 0.070. The complex possesses a syn-[W2O2(�-S)2]2+ core with a W-W bond [2.808(1) � ] and two terminal W-O … Show more

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“…The monomeric tungsten precursor was deemed pure by elemental analyses. Other analytical data were in agreement with the literature. Peaks corresponding to protonated WS 3 L 2 as well as its acetonitrile adduct were dominant in the electrospray mass spectrum: ES-TOF + m / z : 576.94 (33%, [M + H] + ), 660.04 (100% [MeCN·M + H] + ). The isotope pattern of the complex from mass spectrometry confirms the inclusion of only one tungsten center.…”
supporting
confidence: 87%
“…The monomeric tungsten precursor was deemed pure by elemental analyses. Other analytical data were in agreement with the literature. Peaks corresponding to protonated WS 3 L 2 as well as its acetonitrile adduct were dominant in the electrospray mass spectrum: ES-TOF + m / z : 576.94 (33%, [M + H] + ), 660.04 (100% [MeCN·M + H] + ). The isotope pattern of the complex from mass spectrometry confirms the inclusion of only one tungsten center.…”
supporting
confidence: 87%