
Phosphorus, Sulfur and Silicon and the Related Elements p. 231 - 250 (1998)
Update date:2022-08-02
Topics:
Roesler, Roland
Stanciu, Mihaela
Yang, Jincai
Drake, John E.
Silvestru, Cristian
Haiduc, Ionel
The synthesis of isomeric (SPMe2)(OPPh2)NH 1 and (OPMe2)(SPPh2)NH 2 from Li[HN(S)PR2] and R'2P(O)Cl, as well as of their K and Na salts, are presented. The compounds were characterized by means of IR and multinuclear NMR spectroscopy. The crystal and molecular structure of both free acids was determined using X-ray diffractometry. Compound 1 crystallizes in monoclinic space group P21/n, a = 16.798(6) A, b = 17.526(8) A, c = 18.095(7) A, β = 114.72(2)°, Z = 12, and the unit cell contains three independent molecules. Compound 2 crystallizes in orthorhombic space group Fdd2, a = 15.072(7) A, b = 43.078(6) A, c = 9.912(8) A, Z = 16. In both compounds the molecular units are associated into polymeric chains through N-H...O [1.96 A (mean) in 1, and 1.8 A in 2] hydrogen bonds, which involve only the oxygen atom of each molecule. The conformation of the SPNPO system is discussed.
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