The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n3- η222-C60) (n = 2, 3) complexes

Hongkyu Kang, Bo Keun Park, Md Arzu Miah, Hyunjoon Song, David G. Churchill, Sangwoo Park, Moon Gun Choi, Joon T. Park

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Abstract

Treatment of Re3(μ-H)3(CO) 9322: η2-C60) (1) with 2.2 equiv. of Me3NO in the presence of excess PMe3 in chlorobenzene (CB) gave the bisphosphine-substituted complex 1,2-Re3(μ-H)3(CO) 7(PMe3)232: η22-C60) as two diastereomers, 2a (major, 38%) and 2b (minor, 11%). The corresponding reaction of 1 with 3.3 equiv. of Me3NO, produced the trisphosphine-substituted isomeric product 1,2,3-Re3(μ-H)3(CO)6(PMe 3)3322: η2-C60) as two diastereomers, 3a (major, 37%) and 3b (minor, 15%). Complexes 2a-3b have been characterized by spectroscopic methods and elemental analyses. Single crystal X-ray diffraction studies were carried out for 2a and 3b. The hydrides were confirmed by 1H NMR spectroscopic method and directly located only for 3a by X-ray diffraction. The molecular structure of 2a confirms a face-capping μ3- η222-C60 ligand with one axial and one equatorial PMe3 ligand on adjacent rhenium atoms, whereas that for 3b exhibits pseudo-Cs symmetry with an additional equatorial PMe3 on the third rhenium atom. Molecular structures for 2b and 3a are proposed by axial PMe3 ligand placement and subsequent equatorial PMe3 placement, based on earlier observations of facile ligand site-exchange in closely related systems and were verified by 1H NMR spectroscopic method.

Original languageEnglish
Pages (from-to)4704-4711
Number of pages8
JournalJournal of Organometallic Chemistry
Volume690
Issue number21-22
DOIs
Publication statusPublished - 2005 Nov 1

All Science Journal Classification (ASJC) codes

  • Biochemistry
  • Physical and Theoretical Chemistry
  • Organic Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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    Kang, H., Park, B. K., Miah, M. A., Song, H., Churchill, D. G., Park, S., Choi, M. G., & Park, J. T. (2005). The synthesis and characterization of Re3(μ-H) 3(CO)9 - N(PMe3)n3- η222-C60) (n = 2, 3) complexes. Journal of Organometallic Chemistry, 690(21-22), 4704-4711. https://doi.org/10.1016/j.jorganchem.2005.07.052