Phosphorus-31 solid-state nuclear magnetic resonance spectroscopy, individual gauge for localized orbitals calculations and crystal structures of dithiadiphosphetanes [RSP(S)S]2(R = alkyl or aryl)

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Abstract
For a number of dithiadiphosphetanes [RSP(S)S]21 the 31P nuclear magnetic shielding tensor has been investigated. Phosphorus chemical shift δiso and principal values of the shielding tensor σii have been calculated from CP MAS (cross polarization magic angle spinning) spectra. The orientation of the principal axes of the shielding tensor with respect to the dipolar coupling vector has been determined from the static powder spectra of [MeSP(S)S]21a. Ab initio calculations of the 31P shielding tensor have been performed using the individual gauge for localized orbitals method. The calculated data correspond well with the experimental. The most shielded component (the corresponding axis is 3) is approximately perpendicular to the PS2P ring plane {angle P P–3 ≈ 107° for [MeSP(S)S]2}. Axis 2 is perpendicular to the SP–S(3) plane. Since axis 1 is perpendicular to axes 2 and 3 it intersects the S–P–S angle of both the terminal S atoms. The crystal structures of compounds [C6H11SP(S)S]21c and [PhCH2SP(S)S]21d have been determined. Both compounds crystallize in the monoclinic space group no. 14 (1cP21/a, 1dP21/n). The unit cell of 1c contains two crystallographically independent molecules.

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