摘要
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.
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.
基金
Project supported by the National Natural Science Foundation of China （No. 20471008）.
