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Enantiomeric resolution and X-ray optical activity of a tricobalt extended metal atom chain.
Chemical Science 2018 Februrary 8
A simple procedure based on anion exchange was employed for the enantiomeric resolution of the extended metal atom chain (EMAC) [Co3 (dpa)4 (MeCN)2 ]2+ . Use of the chiral salt (NBu4 )2 [As2 (tartrate)2 ], (Λ- 1 or Δ- 1 ), resulted in the selective crystallization of the EMAC enantiomers as [Δ-Co3 (dpa)4 (MeCN)2 ](NBu4 )2 [Λ-As2 (tartarte)2 ]2 , (Δ- 2 ) and [Λ-Co3 (dpa)4 (MeCN)2 ](NBu4 )2 [Δ-As2 (tartrate)2 ]2 (Λ- 2 ), respectively, in the P 421 2 space group, whereas a racemic mixture of 1 yielded [Co3 (dpa)4 (MeCN)2 ][As2 (tartrate)2 ]·2MeCN ( rac - 3 ), which crystallized in the C 2/ c space group. The local electronic and magnetic structure of the EMAC enantiomers was studied, exploiting a variety of dichroisms in single crystals. A strong linear dichroism at the Co K-edge was observed in the orthoaxial configuration, whereas it vanished in the axial orientation, thus spectroscopically confirming the D 4 crystal symmetry. Compounds Δ- 2 and Λ- 2 are shown to be enantiopure materials as evidenced by mirror-image natural circular dichroism spectra in the UV/vis in solution and in the X-ray range at the Co K-edge in single crystals. The surprising absence of detectable X-ray magnetic circular dichroism or X-ray magnetochiral dichroism signals at the Co K-edge, even at low temperature (3 K) and a high magnetic field (17 T), is ascribed to a strongly delocalized spin density on the tricobalt core.
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