Abstract
Reaction of Cp ★CoI 2(P(OMe) 3) 8 with the chiral aminophosphine ( S)-(−)-diphenyl-phenylethylaminophosphine affords the diastereomeric phosphonate complexes ( R, S) Co, S C-Cp ★CoI(P(0)(OMe) 2)(PPh 2NHC ★H(Me)Ph) ( 10a,10b) via Arbuzov dealkylation. 10a,10b are separable and configurationally stable in solution for extended periods. The structure and absolute configuration of the lower R f diastereomer (−)- 436- 10b were determined via single-crystal X-ray diffraction. It crystallizes as a toluene solvate in space group P2 1 with a 13.194(6), b 9.062(4), c 17.023(5) Å, β 108.78(3)°, Z = 2, and was refined to R = 0.067 for 6318 reflections. Spectroscopic and structural evidence demonstrate a strong 1,6 intramolecular NH ⋯ OP hydrogen bond between the aminophosphine NH and the basic phosphoryl oxygen, which establishes a quasi-boat conformation. Proton nuclear Overhauser difference spectra show that the conformation in solution is the same as that observed in the solid state.
Published Version
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