A disubstituted triazine compound, namely, 2-amino-4,6-bis（diphenoxyl phosphorramide）-1,3,5-triazine, which is an inherent flame retardant monomer, was synthesized specifically, and its structure was characterized b...A disubstituted triazine compound, namely, 2-amino-4,6-bis（diphenoxyl phosphorramide）-1,3,5-triazine, which is an inherent flame retardant monomer, was synthesized specifically, and its structure was characterized by using NMR spectrum and X-ray single-crystal diffraction. Unit cell parameters： space group P21/c, Z=4, a=8.7494（15）, b=27.518（5）, c=12.511（2）,β=109.323（16） , Z=4, V=2842.7（9）β3 , Dc=1.380 g/cm3 , F（000）=1224 and Mr=590.46. All the atoms are in the general positions.展开更多
The reaction of 2,4,6-tris（2-pyridyl）-1,3,5-triazine （tptz） and K2PdCl4 in THF/H2O （10：1） results in the hydrolysis of tptz to bis（2-pyridylcarbonyl）amide anion （bpca）, and affords complex Pd（bpca）Cl 1, w...The reaction of 2,4,6-tris（2-pyridyl）-1,3,5-triazine （tptz） and K2PdCl4 in THF/H2O （10：1） results in the hydrolysis of tptz to bis（2-pyridylcarbonyl）amide anion （bpca）, and affords complex Pd（bpca）Cl 1, which is the first example of Pd（Ⅱ）-promoted hydrolysis of ligands. Crystal data for 1： orthorhombic, space group Pbcn, a = 12.0136（17）, b = 14.180（2）, c = 6.9747（11）A, V= 1188.2（3） A3, Z = 4, Mr = 368.06, Dc = 2.058 g/cm3, F（000） = 720,μ = 1.786 mm^-1, λ（MoKα） = 0.71073 A, T= 293（2） K, 2θmax = 54.9°, GOOF = 1.085, the final R= 0.0647 and wR = 0.1051 for 1234 observed reflections with I 〉 2σ（I） （refinement on F2）. Complex 1 is connected through hydrogen bonding to give a 2D network. And weak Pd...Pd interactions are also found between adjacent molecules with the distance of 3.6074（5） A, so the complex is further extended into a 3D supramolecular structure. Thermal gravity analysis （TGA） shows that 1 exhibits high thermal stability below 310℃. X-ray powder diffraction （XRD） and UV/Vis spectrum of 1 are also discussed.展开更多
Two new transition metal dicyanamide complexes [Co2（tppz）（dca）4]·CH3CN （1） [tppz=tetra（2-pyridyl）pyrazine, dca=dicyanamide] and [Co（tptz）（dca）（H20）]（dca） （2） [tptz=2,4,6-tri（2-pyridyl）-1,3,5-t...Two new transition metal dicyanamide complexes [Co2（tppz）（dca）4]·CH3CN （1） [tppz=tetra（2-pyridyl）pyrazine, dca=dicyanamide] and [Co（tptz）（dca）（H20）]（dca） （2） [tptz=2,4,6-tri（2-pyridyl）-1,3,5-triazine] were synthesized and characterized by single crystal X-ray diffraction analysis. In 1 each cobalt（Ⅱ） atom is coordinated to three dca anions and one tppz molecule to form a distorted octahedral geometry, the neigbour two cobalt（Ⅱ） atoms are bridged by one tppz ligand to form a dimer, then the cobalt（Ⅱ） atoms in each dimer are joined together to form a ladder chain structure. In 2 the coordination geometry around the central metal is also distorted octahedral, each cobalt（Ⅱ） atom is coordinated by two dca anions, one tptz molecule and one water ligand to form a cationic part, and the cationic part is linked with the free dca anions via the electrostatic attraction to give an infinite chain structure. Magnetic susceptibility measurement in the range of 2-300 K indicates that there are antiferromagnetic couplings between adjacent metal ions in 1 （T〉29 K, θ=-9.78 K, C=4.92 cm^3·K·mo1-1） and ferromagnetic couplings in 2 （T〉 150 K, θ=7.97 K, C=2.59 cm^3·K·mol^-1） respectively.展开更多
文摘A disubstituted triazine compound, namely, 2-amino-4,6-bis（diphenoxyl phosphorramide）-1,3,5-triazine, which is an inherent flame retardant monomer, was synthesized specifically, and its structure was characterized by using NMR spectrum and X-ray single-crystal diffraction. Unit cell parameters： space group P21/c, Z=4, a=8.7494（15）, b=27.518（5）, c=12.511（2）,β=109.323（16） , Z=4, V=2842.7（9）β3 , Dc=1.380 g/cm3 , F（000）=1224 and Mr=590.46. All the atoms are in the general positions.
基金supported by 973 Program (2006CB932900)the National Natural Science Foundation of China (20571074)
文摘The reaction of 2,4,6-tris（2-pyridyl）-1,3,5-triazine （tptz） and K2PdCl4 in THF/H2O （10：1） results in the hydrolysis of tptz to bis（2-pyridylcarbonyl）amide anion （bpca）, and affords complex Pd（bpca）Cl 1, which is the first example of Pd（Ⅱ）-promoted hydrolysis of ligands. Crystal data for 1： orthorhombic, space group Pbcn, a = 12.0136（17）, b = 14.180（2）, c = 6.9747（11）A, V= 1188.2（3） A3, Z = 4, Mr = 368.06, Dc = 2.058 g/cm3, F（000） = 720,μ = 1.786 mm^-1, λ（MoKα） = 0.71073 A, T= 293（2） K, 2θmax = 54.9°, GOOF = 1.085, the final R= 0.0647 and wR = 0.1051 for 1234 observed reflections with I 〉 2σ（I） （refinement on F2）. Complex 1 is connected through hydrogen bonding to give a 2D network. And weak Pd...Pd interactions are also found between adjacent molecules with the distance of 3.6074（5） A, so the complex is further extended into a 3D supramolecular structure. Thermal gravity analysis （TGA） shows that 1 exhibits high thermal stability below 310℃. X-ray powder diffraction （XRD） and UV/Vis spectrum of 1 are also discussed.
文摘Two new transition metal dicyanamide complexes [Co2（tppz）（dca）4]·CH3CN （1） [tppz=tetra（2-pyridyl）pyrazine, dca=dicyanamide] and [Co（tptz）（dca）（H20）]（dca） （2） [tptz=2,4,6-tri（2-pyridyl）-1,3,5-triazine] were synthesized and characterized by single crystal X-ray diffraction analysis. In 1 each cobalt（Ⅱ） atom is coordinated to three dca anions and one tppz molecule to form a distorted octahedral geometry, the neigbour two cobalt（Ⅱ） atoms are bridged by one tppz ligand to form a dimer, then the cobalt（Ⅱ） atoms in each dimer are joined together to form a ladder chain structure. In 2 the coordination geometry around the central metal is also distorted octahedral, each cobalt（Ⅱ） atom is coordinated by two dca anions, one tptz molecule and one water ligand to form a cationic part, and the cationic part is linked with the free dca anions via the electrostatic attraction to give an infinite chain structure. Magnetic susceptibility measurement in the range of 2-300 K indicates that there are antiferromagnetic couplings between adjacent metal ions in 1 （T〉29 K, θ=-9.78 K, C=4.92 cm^3·K·mo1-1） and ferromagnetic couplings in 2 （T〉 150 K, θ=7.97 K, C=2.59 cm^3·K·mol^-1） respectively.
