Synthesis and X‐ray Molecular Structure of (PNP)<sub>2</sub>[Mo<sup>IV</sup>(C<sub>6</sub>H<sub>4</sub>S<sub>2</sub>‐1,2)<sub>3</sub>] Completing the Structural Characterization of the Series [Mo(C<sub>6</sub>H<sub>4</sub>S<sub>2</sub>‐1,2)<sub>3</sub>]<sup><i>n</i>–</sup> (<i>n</i> = 0, 1, 2)

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<jats:title>Abstract</jats:title><jats:p>The tris(benzene‐1,2‐dithiolato) complex (Li)<jats:sub>2</jats:sub>[Mo<jats:sup>IV</jats:sup>(C<jats:sub>6</jats:sub>H<jats:sub>4</jats:sub>S<jats:sub>2</jats:sub>‐1,2)<jats:sub>3</jats:sub>] {(Li)<jats:sub>2</jats:sub>[Mo<jats:sup>IV</jats:sup>(bdt)<jats:sub>3</jats:sub>]} (bdt<jats:sup>2–</jats:sup> = C<jats:sub>6</jats:sub>H<jats:sub>4</jats:sub>S<jats:sub>2</jats:sub>‐1,2 dianion) was synthesized from [MoCl<jats:sub>4</jats:sub>(CH<jats:sub>3</jats:sub>CN)<jats:sub>2</jats:sub>], (H<jats:sub>2</jats:sub>bdt), and <jats:italic>n</jats:italic>BuLi in THF. Complex (Li)<jats:sub>2</jats:sub>[Mo<jats:sup>IV</jats:sup>(bdt)<jats:sub>3</jats:sub>] undergoes aerial oxidation to give Li[Mo<jats:sup>V</jats:sup>(bdt)<jats:sub>3</jats:sub>]. Both complexes were crystallized from methanol as the salts (PNP)<jats:sub>2</jats:sub>[Mo<jats:sup>IV</jats:sup>(bdt)<jats:sub>3</jats:sub>] and (PNP)[Mo<jats:sup>V</jats:sup>(bdt)<jats:sub>3</jats:sub>] {PNP<jats:sup>+</jats:sup> = bis(triphenylphosphoranylidene)ammonium cation}, and their molecular structures were determined by X‐ray diffraction. The molybdenum(<jats:sc>IV</jats:sc>) complex [Mo<jats:sup>IV</jats:sup>(bdt)<jats:sub>3</jats:sub>]<jats:sup>2–</jats:sup> assumes a distorted trigonal prismatic coordination geometry (average twist angle= 24.8°) while the coordination geometry of [Mo<jats:sup>V</jats:sup>(bdt)<jats:sub>3</jats:sub>]<jats:sup>–</jats:sup> is best described as distorted octahedral (average twist angle= 34.1°). (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005)</jats:p>

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