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Manson, Josiah
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article
Nickel-Manganese Sulfido Carbonyl Cluster Complexes. Synthesis, Structure, and Properties of the Unusual Paramagnetic Complexes Cp2Ni 2Mn(CO)3(μ3-E)2, E = S, Se
Abstract
<p>The reaction of Mn<sub>2</sub>(CO)<sub>7</sub>(μ-S<sub>2</sub>) with [CpNi(CO)]<sub>2</sub> yielded the paramagnetic new compound Cp <sub>2</sub>Ni<sub>2</sub>Mn(CO)<sub>3</sub>(μ<sub>3</sub>-S)<sub>2</sub> (1) and a new hexanuclear metal product Cp<sub>2</sub>Ni<sub>2</sub>Mn <sub>4</sub>(CO)<sub>14</sub>(μ<sub>6</sub>-S<sub>2</sub>)(μ <sub>3</sub>-S)<sub>2</sub> (2). Structurally, compound 1 contains two triply bridging sulfido ligands on opposite sides of an open Ni<sub>2</sub>Mn triangular cluster. EPR and temperature-dependent magnetic susceptibility measurements of 1 show that it contains one unpaired electron. The electronic structure of 1 was determined by Fenske-Hall molecular orbital calculations which show that the unpaired electron occupies a low lying antibonding orbital delocalized unequally across the three metal atoms. The selenium homologue Cp<sub>2</sub>Ni<sub>2</sub>Mn(CO)<sub>3</sub>(μ<sub>3</sub>-Se)<sub>2</sub> (3) was obtained from the reaction of a mixture of Mn<sub>2</sub>(CO) <sub>10</sub> and [CpNi(CO)]<sub>2</sub> with elemental selenium and Me <sub>3</sub>NO·<sub>2</sub>H<sub>2</sub>O. It also has one unpaired electron. Compound 1 reacted with elemental sulfur to yield the dinickeldimanganese compound, Cp<sub>2</sub>Ni<sub>2</sub>Mn <sub>2</sub>(CO)<sub>6</sub>(μ<sub>4</sub>-S<sub>2</sub>)(μ <sub>4</sub>-S<sub>5</sub>), 4, which can also be made from the reaction of Mn<sub>2</sub>(CO)<sub>7</sub>(μ-S<sub>2</sub>) with [CpNi(CO)]<sub>2</sub> and sulfur. Compound 4 was converted back to 1 by sulfur abstraction using PPh<sub>3</sub>. The reaction of Mn<sub>2</sub>(CO)<sub>10</sub> with [CpNi(CO)]<sub>2</sub> in the presence of thiirane yielded the ethanedithiolato compound CpNiMn(CO)<sub>3</sub>(μ-SCH<sub>2</sub>CH<sub>2</sub>S) (5), which was also obtained from the reaction of Mn<sub>4</sub>(CO)<sub>15</sub>(μ <sub>3</sub>-S<sub>2</sub>)(μ<sub>4</sub>-S<sub>2</sub>) with [CpNi-(CO)]<sub>2</sub> in the presence of thiirane. Compound 5 reacted with additional quantities of thiirane to yield the new compound CpNiMn(CO) <sub>3</sub>[μ-S(CH<sub>2</sub>CH<sub>2</sub>S)<sub>2</sub>], 6, which contains a 3-thiapentanedithiolato ligand that bridges the two metal atoms. Compound 6 was also obtained from the reaction of Mn<sub>2</sub>(CO) <sub>10</sub> with CpNi(CO)12 and thiirane. The molecular structures of the new compounds 1-6 were established by single-crystal X-ray diffraction analyses.</p>