The （SCZ）（TNPG）.2H2O prepared by mixing semicarbazide （SCZ） and trinitrophloroglucinol （TNPG） was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray singl...The （SCZ）（TNPG）.2H2O prepared by mixing semicarbazide （SCZ） and trinitrophloroglucinol （TNPG） was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal belongs to triclinic,space group P1, （NH2CONHNH3）^＋（C6H2N3O9）^-·2H2O, Mr = 372.23, a = 0.68853（14）, b =0.93966（19）, c = 1.1925（2） nm, α = 67.48（3）, β = 77.56（3）, γ = 78.93（3）°, V = 0.6908（2） nm^3, Z = 2,Dc = 1.789 g/cm^3, Mr = 373.23, F（000） = 384, S = 0.999 and μ（MoKa） = 0.172 mm^-1. The final R and wR are 0.0394 and 0.1057 for 1724 observed reflections with I 〉 2σ（I）. It is concluded that （SCZ）（TNPG） 2H2O is an ionic compound composed of a cation SCZ^＋, an anion TNPG- and two water molecules. The TNPG anion and SCZ^＋ cation are bonded together by electrostatic attraction and hydrogen bonds, and the compound structure is stable. The thermal decomposition of （SCZ）（TNPG） 2H2O was studied by using TG-DTG and DSC techniques with a heating rate of 10 ℃/min, showing the compound contains one endothermic process of dehydrating stage and two intensive exothermic decomposition stages. The enthalpy of exothermic decomposition reaction is 452.31 kJ/mol.展开更多
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 str...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.展开更多
基金This work was supported by the National Natural Science Foundation of China (20471008) and the Foundation of BIT-UBF-200302B01
文摘The （SCZ）（TNPG）.2H2O prepared by mixing semicarbazide （SCZ） and trinitrophloroglucinol （TNPG） was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal belongs to triclinic,space group P1, （NH2CONHNH3）^＋（C6H2N3O9）^-·2H2O, Mr = 372.23, a = 0.68853（14）, b =0.93966（19）, c = 1.1925（2） nm, α = 67.48（3）, β = 77.56（3）, γ = 78.93（3）°, V = 0.6908（2） nm^3, Z = 2,Dc = 1.789 g/cm^3, Mr = 373.23, F（000） = 384, S = 0.999 and μ（MoKa） = 0.172 mm^-1. The final R and wR are 0.0394 and 0.1057 for 1724 observed reflections with I 〉 2σ（I）. It is concluded that （SCZ）（TNPG） 2H2O is an ionic compound composed of a cation SCZ^＋, an anion TNPG- and two water molecules. The TNPG anion and SCZ^＋ cation are bonded together by electrostatic attraction and hydrogen bonds, and the compound structure is stable. The thermal decomposition of （SCZ）（TNPG） 2H2O was studied by using TG-DTG and DSC techniques with a heating rate of 10 ℃/min, showing the compound contains one endothermic process of dehydrating stage and two intensive exothermic decomposition stages. The enthalpy of exothermic decomposition reaction is 452.31 kJ/mol.
基金Project supported by the National Natural Science Foundation of China （No. 20471008）.
文摘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.
