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Coarse crystalline (NH 2 ) 2 (O)P-N=P(NH 2 ) 3  is obtained from a NH 3  saturated CH 2 Cl 2  suspension of (NH 2 ) 2 (O)P-N=P(NH 2 ) 3  NH 4 Cl at room temperature. (NH 2 ) 2 (O)P-N=P(NH 2 ) 3 ·NH 4 Cl is synthesized by slow addition of Cl 2 (O)P-N=PCl 3  to a solution of NH 3  in CH 2 Cl 2  at -78 °C. Excess NH 4 Cl is removed by treatment with HNEt 2  followed by extraction with CH 2 Cl 2 . The crystal structure of (NH 2 ) 2 (O)P-N=P(NH 2 ) 3  has been determined by single crystal X-ray methods (P2 1 /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 NH 3  above 80 °C.

zeitschrift für naturforschung b

Synthese, Kristallstruktur und Eigenschaften von 1,1,3,3,3-Pentaamino-1-oxo- 1λ 5  ,3λ 5 -diphosphaz-2-en, (NH 2 ) 2 (O)P-N=P(NH 2 ) 3  / Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaamino-1-oxo-1λ 5 , 3λ 5 -diphosphaz-2-ene, (NH 2 ) 2 (O)P-N=P(NH 2 ) 3