One novel cobalt coordination polymer, {[Co（HTCB）（4,4＇btb）]＇HzO}n （1, H3TCB = 1,3,5-tris（4-carboxyphenyl）benzene, 4,4＇-btb = 4,4＇-bis（1,2,4-triazol-3-yl）biphenyl）, has been synthesized and characterized ...One novel cobalt coordination polymer, {[Co（HTCB）（4,4＇btb）]＇HzO}n （1, H3TCB = 1,3,5-tris（4-carboxyphenyl）benzene, 4,4＇-btb = 4,4＇-bis（1,2,4-triazol-3-yl）biphenyl）, has been synthesized and characterized by elemental analysis, IR, powder X-ray diffraction （PXRD）, and thermogravimetric （TG） analyses. X-ray diffraction analysis reveals that complex 1 is a 2D 2-fold interpenetrated {44,62}-sql [Co（HTCB）（4,4＇-btb）] sheet based on the 1D [Co（HTCB）]n chains and 1D [Co（4,4＇-btb）]n chains. The crystal of 1 crystallizes in triclinic, space group P1 with a = 9.529（12）, b = 13.914（16）, c = 14.906（17） A, V= 1903（4） A3, Z = 2, C45H34N6CoO71 Mr= 829.71, Dc = 1.448 g/cm3, F（000） = 858 andμ（MoKa） = 0.514 mm-1. The final R = 0.0655 and wR = 0.1136 for 6603 observed reflections with 1 〉 2a（/） and R = 0.1136 and wR = 0.1747 for all data.展开更多
Tetraiodo-4,4＇-bi-l,2,4-triazole （1） was synthesized from a reaction of iodine monochloride witb 4,4＇ bi- 1,2,4-triazole （2）, which was prepared by a transamination reaction between 4-amine-1,2,4-triazole and N,...Tetraiodo-4,4＇-bi-l,2,4-triazole （1） was synthesized from a reaction of iodine monochloride witb 4,4＇ bi- 1,2,4-triazole （2）, which was prepared by a transamination reaction between 4-amine-1,2,4-triazole and N,N-dimethylformamide azine dihydrochloride （3） obtained via a Vilsmeier reaction. The title compound was extensively characterized by melting point, elemental analysis, 1R, HRMS and single crystal X-ray diffraction. The single crystal X-ray structural analysis reveals that compound 1 exhibits a stable conformation with the two triazole rings being perpendicular to minimize three-dimensional steric hindrance and stacking through aromatic zr. analysis from TGA and DSC indicates that resnectivelv. Jr packing interactions between molecules. The therma compound I decomposes at 275.40 ℃ and 338.35 C展开更多
A series of guanidine salts of 4,4＇-azo-l,2,4-triazol-5-one with guanidine（1）, aminoguanidine（2）, diaminoguanidine（3） and triaminoguanidine（4） was prepared. Compounds 2--4 were characterized by infrared（IR）...A series of guanidine salts of 4,4＇-azo-l,2,4-triazol-5-one with guanidine（1）, aminoguanidine（2）, diaminoguanidine（3） and triaminoguanidine（4） was prepared. Compounds 2--4 were characterized by infrared（IR） spectroscopy, elemental analysis and single-crystal X-ray diffraction. Thermal decomposition processes of compounds 1--4 were investigated by differential scanning calorimetry（DSC）, and all the compounds showed good thermal stability up to 190 ℃. Moreover, these four guanidine salts are more unstable with the increasing number of amino groups. Thermal stability parameters（Te,0 and Tb）and thermodynamic functions（△S≠, △H≠ and △G≠） for compounds 1-4 were calculated. The constant-volume combustion heats（AcU） for compounds 2--4 were determined and tended to increase with the increase of the number of amino groups. The calculated standard molar enthalpies of forma- tion（△ρH0m） of compounds 2-4 are -541.04, -178.67 and-83.08 kJ/mol, respectively. The impact sensitivities results indicate that these four energetic salts are less sensitive than 1,3,5-trinitrotriazacyccohexane（RDX） and 1,3,5,7- tetranitrotetraqza-cyclo-octane（HMX）.展开更多
基金supported by the National Natural Science Foundation of China(20873150)the Natural Science Foundation of Shandong Province(ZR2010BQ023)
文摘One novel cobalt coordination polymer, {[Co（HTCB）（4,4＇btb）]＇HzO}n （1, H3TCB = 1,3,5-tris（4-carboxyphenyl）benzene, 4,4＇-btb = 4,4＇-bis（1,2,4-triazol-3-yl）biphenyl）, has been synthesized and characterized by elemental analysis, IR, powder X-ray diffraction （PXRD）, and thermogravimetric （TG） analyses. X-ray diffraction analysis reveals that complex 1 is a 2D 2-fold interpenetrated {44,62}-sql [Co（HTCB）（4,4＇-btb）] sheet based on the 1D [Co（HTCB）]n chains and 1D [Co（4,4＇-btb）]n chains. The crystal of 1 crystallizes in triclinic, space group P1 with a = 9.529（12）, b = 13.914（16）, c = 14.906（17） A, V= 1903（4） A3, Z = 2, C45H34N6CoO71 Mr= 829.71, Dc = 1.448 g/cm3, F（000） = 858 andμ（MoKa） = 0.514 mm-1. The final R = 0.0655 and wR = 0.1136 for 6603 observed reflections with 1 〉 2a（/） and R = 0.1136 and wR = 0.1747 for all data.
基金supported by the National Key Projects(No.00402040103)Youth Innovation Research Team of Sichuan for Carbon Nanomaterials(No.2011JTD0017)
文摘Tetraiodo-4,4＇-bi-l,2,4-triazole （1） was synthesized from a reaction of iodine monochloride witb 4,4＇ bi- 1,2,4-triazole （2）, which was prepared by a transamination reaction between 4-amine-1,2,4-triazole and N,N-dimethylformamide azine dihydrochloride （3） obtained via a Vilsmeier reaction. The title compound was extensively characterized by melting point, elemental analysis, 1R, HRMS and single crystal X-ray diffraction. The single crystal X-ray structural analysis reveals that compound 1 exhibits a stable conformation with the two triazole rings being perpendicular to minimize three-dimensional steric hindrance and stacking through aromatic zr. analysis from TGA and DSC indicates that resnectivelv. Jr packing interactions between molecules. The therma compound I decomposes at 275.40 ℃ and 338.35 C
文摘A series of guanidine salts of 4,4＇-azo-l,2,4-triazol-5-one with guanidine（1）, aminoguanidine（2）, diaminoguanidine（3） and triaminoguanidine（4） was prepared. Compounds 2--4 were characterized by infrared（IR） spectroscopy, elemental analysis and single-crystal X-ray diffraction. Thermal decomposition processes of compounds 1--4 were investigated by differential scanning calorimetry（DSC）, and all the compounds showed good thermal stability up to 190 ℃. Moreover, these four guanidine salts are more unstable with the increasing number of amino groups. Thermal stability parameters（Te,0 and Tb）and thermodynamic functions（△S≠, △H≠ and △G≠） for compounds 1-4 were calculated. The constant-volume combustion heats（AcU） for compounds 2--4 were determined and tended to increase with the increase of the number of amino groups. The calculated standard molar enthalpies of forma- tion（△ρH0m） of compounds 2-4 are -541.04, -178.67 and-83.08 kJ/mol, respectively. The impact sensitivities results indicate that these four energetic salts are less sensitive than 1,3,5-trinitrotriazacyccohexane（RDX） and 1,3,5,7- tetranitrotetraqza-cyclo-octane（HMX）.
