The synthesis, X-ray and solid state NMR studies of 2-N,N-diisopropylamino-1,3,2λ5- oxaselenaphospholane-2-selone

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Marek J. Potrzebowski, Jarosław BŁaszczyk, Michał W. Wieczorek, Konrad Misiura and Wojciech J. Stec


Abstract

31P and 77Se high resolution solid state NMR spectroscopy was employed to study structural properties of 2-N,N-diisopropylamino-1,3,2λ5- oxaselenaphospholane-2-selone 5 the compound made in the course of developing reagents for stereocontrolled synthesis of nucleoside–phosphorothioates. Both 31P CP/MAS and 77Se CP/MAS experiments revealed that the asymmetric unit consists of two independent molecules with different geometry around phosphorus and selenium centres. The principal elements δii of the 31P chemical shift tensor were calculated from spinning sideband intensities employing the WIN-MAS program. The established values of anisotropy and asymmetry parameters reflect the distortion of the phosphorus environment and correspond well with X-ray diffraction data. Crystals of 2-N,N-diisopropylamino-1,3,2λ5- oxaselenaphospholane-2-selone grown from diethyl ether are triclinic, space group P[1 with combining macron] with a = 7.586(2), b = 13.003(1), c = 13.649(1) Å, α = 89.683(8)°, β = 75.42(1)°, γ = 8.74(1)°, V = 1285(6) Å3, Dc = 1.722(2) g cm-3 and Z = 4. Refinement using 5243 reflections for 235 variables gives R = 0.047.


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