3,5-二羟基-2,4,6-三硝基苯酚氨基脲铵盐半水合物的合成、晶体结构和热分解特性

A new compound, semicarbazidium 3,5-dihydroxy-2,4,6-trinitrophenolate hemihydrate （SCDHTNP·0.5H2P）, was synthesized by the reaction of the aqueous solutions of semicarbazide with trinitrophloroglucinol. Its structure was determined by single-crystal X-ray diffraction analysis and characterized by elemental analysis, FTIR, DSC and TG-DTG techniques. The crystal is monoclinic with space group P21/n and the empirical formula C7H9N6O10.50. The unit cell parameters are： a= 1.3791（3） nm, b=0.9256（2） nm, c=2.0468（4） nm,β= 106.93（3）°, V=2.4995（9）nm^3, Z=8, Dc= 1.835 g/cm^3, Mr=345.20, F（000）= 1416, s=0.945,μ（Mo Ka）=0.174 mm^-1. The final R and wR are 0.0401 and 0.0896. Its structure consists of two semicarbazidium cations, two 3,5-dihydroxy-2,4,6-trinitrophenolate anions and one crystal water molecule, which are interconnected by electrostatic forces and hydrogen bonds into layer structure, making the title compound very stable. Under a linear heating rate, the thermal decomposition processes of SCDHTNP·0.5H2O have one endothermal dehydration stage and two intensive exothermic decomposition stages at 178-241℃ to evolve abundant gas products.

Synthesis, X-ray Crystal Structure and Thermal Decomposition Character of Semicarbazidium 3,5-Dihydroxy-2,4,6-trinitrophenolate Hemihydrate

A new compound, semicarbazidium 3,5‐dihydroxy‐2,4,6‐trinitrophenolate hemihydrate (SCDHTNP·0.5H₂O), was synthesized by the reaction of the aqueous solutions of semicarbazide with trinitrophloroglucinol. Its structure was determined by single‐crystal X‐ray diffraction analysis and characterized by elemental analysis, FTIR, DSC and TG‐DTG techniques. The crystal is monoclinic with space group P2C_1/n and the empirical formula C₇H₉N₆O_10.50. The unit cell parameters are: a=1.3791(3) nm, b=0.9256(2) nm, c=2.0468(4) nm, β=106.93(3)°, V=2.4995(9) nm³, Z=8, D_c=1.835 g/cm³, M_r=345.20, F(000)=1416, s=0.945, μ(Mo Kα)=0.174 mm^‐1. The final R and wR are 0.0401 and 0.0896. Its structure consists of two semicarbazidium cations, two 3,5‐dihydroxy‐2,4,6‐trinitrophenolate anions and one crystal water molecule, which are interconnected by electrostatic forces and hydrogen bonds into layer structure, making the title compound very stable. Under a linear heating rate, the thermal decomposition processes of SCDHTNP·0.5H₂O have one endothermal dehydration stage and two intensive exothermic decomposition stages at 178‐241°C to evolve abundant gas products.