The synthesis and characterization of Re3(μ-H)3(CO)9 − n(PMe3)n(μ3-η2:η2:η2-C60) (n = 2, 3) complexes

The reaction of Re3(μ-H)3(CO)9(μ3-η2:η2:η2-C60) (1) with PMe3 in the presence of Me3NO produces di- and tri-substituted stereoisomeric compounds having the general formula Re3(μ-H)3(CO)9−n(PMe3)n(μ3-η2:η2:η2-C60) (n = 2, 2a and 2b; 3, 3a and 3b), depending on the stoichiometry of Me3NO. Single crystal X-ray structures were obtained for 2a and 3b. Ligand arrangements for 2b and 3a are proposed based on assigning one PMe3 ligand in an axial position and remaining PMe3 ligands according to low energy equatorial site exchanges known in related metal cluster complexes, and were verified by 1H NMR spectroscopic methods.