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Captain, Burjor
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article
New disulfido molybdenum-manganese complexes exhibit facile addition of small molecules to the sulfur atoms
Abstract
<p>The reaction of Mn<sub>2</sub>(CO)<sub>7</sub>(μ-S<sub>2</sub>) (1) with [CpMo(CO)<sub>3</sub>]<sub>2</sub> (Cp = C<sub>5</sub>H<sub>5</sub>) and [Cp*Mo(CO)<sub>3</sub>]<sub>2</sub> (Cp* = C<sub>5</sub>(CH<sub>3</sub>)<sub>5</sub>) yielded the new mixed-metal disulfide complexes CpMoMn(CO)<sub>5</sub>(μ-S<sub>2</sub>) (2) and Cp*MoMn(CO)<sub>5</sub>(μ-S<sub>2</sub>) (3) by a metal-metal exchange reaction. Compounds 2 and 3 both contain a bridging disulfido ligand lying perpendicular to the Mo-Mn bond. The bond distances are Mo-Mn = 2.8421(10) and 2.8914(5) Å and S-S = 2.042(2) and 1.9973(10) Å for 2 and 3, respectively. A tetranuclear metal side product CpMoMn<sub>3</sub>(CO)<sub>13</sub>(μ<sub>3</sub>-S)(μ<sub>4</sub>-S) (4) was also isolated from the reaction of 1 with [CpMo(CO)<sub>3</sub>]<sub>2</sub>. Compounds 2 and 3 react with CO to yield the dithiocarbonato complexes CpMoMn- (CO)<sub>5</sub>[μ-SC(=O)S] (5) and Cp*MoMn(CO)<sub>5</sub>[μ-SC(=O)S] (6) by insertion of CO into the S-S bond. Similarly, tert-butylisocyanide was inserted into the S-S bond of 2 and 3 to yield the complexes CpMoMn(CO)<sub>5</sub>[μ-S(C=NBu<sup>t</sup>)S] (7) and Cp*MoMn(CO)<sub>5</sub>[μ-S(C=NBu<sup>t</sup>)S] (8), respectively. Ethylene and dimethylacetylene dicarboxylate also inserted into the S-S bond of 2 and 3 at room temperature to yield the ethanedithiolato ligand bridged complexes CpMoMn- (CO)<sub>5</sub>(μ-SCH<sub>2</sub>CH<sub>2</sub>S) (9), Cp*MoMn(CO)<sub>5</sub>(μ-SCH<sub>2</sub>CH<sub>2</sub>S) (10), CpMoMn(CO)<sub>5</sub>[μ-SC(CO<sub>2</sub>Me)=C(CO<sub>2</sub>Me)S] (11), and Cp*MoMn(CO)<sub>5</sub>[μ-SC(CO<sub>2</sub>Me)=C(CO<sub>2</sub>Me)S] (12). Allene was found to insert into the S-S bond of 2 by using one of its two double bonds to yield the complex CpMoMn(CO)<sub>5</sub>[μ-SCH<sub>2</sub>C(=CH<sub>2</sub>)S] (13). The molecular structures of the new complexes 2-7 and 9-13 were established by single-crystal X-ray diffraction analyses.</p>