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Syntheses, separation of diastereomers, NMR studies and molecular properties in solution are reported for [CH 3 (t-C 4 H 9 )P (S)] 2  (1 and 2), and [CH 3 (t-C 4 H 9 )P(S)] 2 S (3) in the preceding paper [1], For further characterization the crystal structures of the diastereom eric disphosphane disulphides (1 and 2) as well as of the related sulphane (3) have been determ ined. 1 is triclinic (space group P1̄; Z = 1), 1792 independent reflections yielded R = 0.03. 2: monoclinic (P2 1 ; Z = 2), 973 reflections, R = 0.07. 3: orthorhombic (Pbca; Z = 8), 2607 reflections, R = 0.05. Molecules of 1 and 2 are diastereomers. The configuration of 1 is meso (point symmetry 1̄-C i  , all ligands trans) whereas 2 is an enantiomeric form of the prepared racemic mixture (S atom s and methyl gauche, t-butyl trans). The distance P - P is 226.6(1) and 226.9(3) pm, respectively. Molecules of 3 are enantiomers in racemic crystals (S atoms and t-butyl close to gauche). The molecule is bent by an angle P -S -P of 104.78(5)°.

Diastereomere Organophosphorverbindungen, II [1] Molekül- und Kristallstrukturen von [CH 3 (t-C 4 H 9 )P(S)] 2 und [CH 3 (t-C 4 H 9 )P(S)] 2 S