- Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaamino-1-oxo-1λ5,3λ 5-diphosphaz-2-ene, (NH2)2(O)P-N=P(NH2)3
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Coarse crystalline (NH2)2(O)P-N=P(NH2)3 is obtained from a NH3 saturated CH2Cl2 suspension of (NH2)2(O)P-N=P(NH2)3·NH 4Cl at room temperature. (NH2)2(O)P-N=P(NH2)3·NH 4Cl is synthesized by slow addition of Cl2(O)P-N=PCl3 to a solution of NH3 in CH2Cl2 at -78 °C. Excess NH4Cl is removed by treatment with HNEt2 followed by extraction with CH2Cl2. The crystal structure of (NH2)2(O)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P21/c; a = 1462.8(3) b = 944.8(2), c = 1026.9(2) pm, β= 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H...N ≥ 313 pm, N-H-...O ≥ 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80°C.
- Stock,Schnick
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p. 1079 - 1083
(2007/10/03)
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- Optimized Synthesis and Mechanism of Formation of 2,4-Dichloro-1,3-bis(dichlorophosphoryl)-2,4-dioxocyclodiphosph(v)azane from Phosphoryl Chloride and Ammonium Chloride
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Detailed investigation of the reaction between Cl and an excess of POCl3 has established a procedure for isolation of the main product, the novel title cyclodiphosph(v)azane, and permitted the identification of three other reaction products, namely, pyrophosphoryl chloride, hexachlorocyclotriphosph(v)azane, and PPP-trichloro-N-dichlorophosphorylmonophosph(v)azane.A reaction mechanism is proposed which accounts for the formation of all four products.
- Jaeger, Roger De,Taylor, David R.
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p. 851 - 853
(2007/10/02)
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