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A single-crystal X-band ESR study at 100 K of X-irradiated dipyrrolidinochlorophosphine sulfide (1) and di- morpholinofluorophosphine sulfide (2) reveals the existence of two phosphoranyl radicals la and 2a formed by electron capture at phosphorus. The principal values and direction cosines of the hyperfine and g tensors are determined. It is found that la represents a u* structure: Le., the unpaired electron is located in the antibonding MO of the phosphorus-chlorine bond, whereas 2a possesses a trigonal-bipyramidal (TBP) configuration with fluorine and sulfur in the apical positions and the odd electron in an equatorial position (TBP-e). On annealing, the radicals la and 2a dissociate irreversibly by cleavage of the phosphorus-halogen bond and the isostructural thiophosphonyl radicals lb and 2b are obtained. An explanation for the striking difference in electron capture of 1 and 2 is presented.

The .sigma.* and TBP-e radicals obtained by electron capture of four-coordinated phosphorus compounds. A single-crystal ESR study