Six new N4-[bi-（4-fluorophenyl）-methyl]-piperazine thiosemicarbazones 3a-f have been prepared starting from [bi-（4-fluorophenyl）-methyl]-piperazine in solvent-free condition under microwave irradiation with excell...Six new N4-[bi-（4-fluorophenyl）-methyl]-piperazine thiosemicarbazones 3a-f have been prepared starting from [bi-（4-fluorophenyl）-methyl]-piperazine in solvent-free condition under microwave irradiation with excellent yields. Their structures have been determined by elemental analysis, IR, MS and 1H NMR data.展开更多
A new Cd（II） coordination polymer, namely, [Cd3（1,2,3-BTC）2（L）2]·2.25H2O （1, L = 2-（2-chloro-6-fluorophenyl）-1H-imidazo[4,5-A][1,10]phenanthroline and 1,2,3-BTC = 1,2,3-ben- zenetricarboxylate）, has bee...A new Cd（II） coordination polymer, namely, [Cd3（1,2,3-BTC）2（L）2]·2.25H2O （1, L = 2-（2-chloro-6-fluorophenyl）-1H-imidazo[4,5-A][1,10]phenanthroline and 1,2,3-BTC = 1,2,3-ben- zenetricarboxylate）, has been synthesized under hydrothermal conditions. The compound was characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group Pī with α = 11.650（2）, b = 12.240（2）, c = 19.760（4） A, α = 72.01（3）, β = 77.11（3）, γ = 83.48（3）°, V = 2609.4（9） A3, Z = 2, C56H31Cd3Cl2F2N8O14.25, Mr = 1489.99, Dc = 1.896 g/cm3, F（000） = 1466, μ（MoKa） = 1.401 mm^-1, R = 0.0401 and wR = 0.1104. Compound 1 shows a 1D chain structure, and the neigh- boring 1D chains of 1 are joined together by π···π interactions to result in a 2D supramolecular layer. In addition, the luminescent property of 1 has been studied in the solid state at room temperature.展开更多
The crystal structure of the title compound 1-（4-fluorophenyl） -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H） -one（C23H21FN4O2S,Mr = 436.5） has been prepared and determined by single-cr...The crystal structure of the title compound 1-（4-fluorophenyl） -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H） -one（C23H21FN4O2S,Mr = 436.5） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854（3） ,b = 17.2678（4） ,c = 18.1828（5）A,β = 99.364（2） °,V = 4332.58（18） A^3,Z = 4,Dc = 1.338,F（000） =1824,μ = 0.185 mm^-1,MoKa radiation（λ = 0.71073） ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ（I） . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5（1H） -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.展开更多
The title compound has been synthesized by the reaction of 1-bromo-3,3-dime- thyl- 1 - （1 H- 1,2,4-triazol- 1 -yl）butan-2-one with 1 -（2-fluorophenyl）thiourea, and its crystal struc- ture was determined by single-...The title compound has been synthesized by the reaction of 1-bromo-3,3-dime- thyl- 1 - （1 H- 1,2,4-triazol- 1 -yl）butan-2-one with 1 -（2-fluorophenyl）thiourea, and its crystal struc- ture was determined by single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbca with a = 15.2568（6）, b = 12.1533（5）, c = 16.7307（7） A, Z = 8, V = 3102.2（2） A3, Mr = 317.39, Dc = 1.359 g/cm3, S = 1.05, μ = 0.223 mm-1, F（000） = 1328, the final R = 0.034 and wR = 0.097 for 2590 observed reflections （I 〉 2σ（I））. X-ray crystal structure presents the intramolecular N-H…N hydrogen bond, which plays an important role in stabilizing the crystal structure. In addition, the preliminary biological test on the title compound shows good antitumor activity, with IC50 of 0.122 μmol/mL against the Hela cell line.展开更多
Three novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles were designed,synthesized and characterized by IR,NMR and APCI-MS.3-o-Fluorophenyl-6-（4-decarboxydehydroabietyl）-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole（6a,C28H3...Three novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles were designed,synthesized and characterized by IR,NMR and APCI-MS.3-o-Fluorophenyl-6-（4-decarboxydehydroabietyl）-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole（6a,C28H31FN4S） was structurally determined by single-crystal X-ray diffraction.The crystal belongs to the orthorhombic system,space group P212121 with a=6.0153（14）,b=12.2577（19）,c=34.055（3）A,V=2511.0（7）A^3,Z=4,Mr=474.63,Dc=1.255Mg/m^3,λ=0.71073 A,μ（MoKα）=0.160 mm^-1,F（000）=1008,the final R=0.0555 and wR=0.1248 for 3094 observed reflections with I〉2σ（I）.There are six rings in the crystal structure of the title compound.The dihedral angle between 1,2,4-triazole and 1,3,4-thiadiaole rings is 1.4o,and that between 1,2,4-triazole and benzene ring D 25.5o.展开更多
The chiral molecule （＋）-N-[（3S）-3-（4-fluorophenyl）heptanoyl]bornane-10,2-sultam （C23H32FNO3S, Mr = 421.56）, a fluorine-containing derivative of camphorsultam, was conveniently obtained and crystallized in the...The chiral molecule （＋）-N-[（3S）-3-（4-fluorophenyl）heptanoyl]bornane-10,2-sultam （C23H32FNO3S, Mr = 421.56）, a fluorine-containing derivative of camphorsultam, was conveniently obtained and crystallized in the orthorhombic space group P212121 with a = 7.9044（11）, b = 11.6680（16）, c = 24.899（3） , V = 2296.4（5） 3, Z = 4, Dc = 1.219 Mg/m3, λ = 0.71073 , μ（MoKα） = 0.172 mm-1 and F（000） = 904. X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat conformation （Fig. 1）. The planes constructed by （（C6）, （C7）, （C8）, （C9）） and （（C4）, （C5）, （C6）, （C9）） form a dihedral angle of 70.3（3）°. The plane of （C1）-（C2）-（C3） forms dihedral angles to the aforementioned planes of 85.9（4） and 89.5（4）°, respectively. The molecules are linked via C-H···O/F interactions.展开更多
Geometry optimization and subsequent harmonic vibration calculations of prior synthesized （E）-3-（4-fluorophenyl）-N-[4-（phenyl-amino） quinazoline-7-yl] acrylamide were carried out by DFT/B3LYP method with both 6-...Geometry optimization and subsequent harmonic vibration calculations of prior synthesized （E）-3-（4-fluorophenyl）-N-[4-（phenyl-amino） quinazoline-7-yl] acrylamide were carried out by DFT/B3LYP method with both 6-31G and 6-311G basis sets.The Infrared （IR） spectrum of the title compound was recorded in the field of 400-4000 cm 1 and then assigned.The correlation analyses between the scaled theoretical vibration frequencies and the experimental ones indicate that there exist good linearity relationships since the correlation coefficients R 2 are larger than 0.999.The intramolecular interactions existed in the title molecule were confirmed by the Atoms in molecules （AIM） method,and their influences on the absorption frequency were also investigated.展开更多
基金Natural Foundation of Southwest University for Nationalities(No.234688).
文摘Six new N4-[bi-（4-fluorophenyl）-methyl]-piperazine thiosemicarbazones 3a-f have been prepared starting from [bi-（4-fluorophenyl）-methyl]-piperazine in solvent-free condition under microwave irradiation with excellent yields. Their structures have been determined by elemental analysis, IR, MS and 1H NMR data.
基金Supported by the Science and Technology Research Projects of the Education Committee of Jilin Province(No.2013212)
文摘A new Cd（II） coordination polymer, namely, [Cd3（1,2,3-BTC）2（L）2]·2.25H2O （1, L = 2-（2-chloro-6-fluorophenyl）-1H-imidazo[4,5-A][1,10]phenanthroline and 1,2,3-BTC = 1,2,3-ben- zenetricarboxylate）, has been synthesized under hydrothermal conditions. The compound was characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group Pī with α = 11.650（2）, b = 12.240（2）, c = 19.760（4） A, α = 72.01（3）, β = 77.11（3）, γ = 83.48（3）°, V = 2609.4（9） A3, Z = 2, C56H31Cd3Cl2F2N8O14.25, Mr = 1489.99, Dc = 1.896 g/cm3, F（000） = 1466, μ（MoKa） = 1.401 mm^-1, R = 0.0401 and wR = 0.1104. Compound 1 shows a 1D chain structure, and the neigh- boring 1D chains of 1 are joined together by π···π interactions to result in a 2D supramolecular layer. In addition, the luminescent property of 1 has been studied in the solid state at room temperature.
基金Supported by the Natural Science Foundation of Hubei Province (2006ABB016)Key Science Research Project of Hubei Provincial Department of Education (No.D200724001)the Science Research Project of Yunyang Medical College (No.2008CXG01)
文摘The crystal structure of the title compound 1-（4-fluorophenyl） -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H） -one（C23H21FN4O2S,Mr = 436.5） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854（3） ,b = 17.2678（4） ,c = 18.1828（5）A,β = 99.364（2） °,V = 4332.58（18） A^3,Z = 4,Dc = 1.338,F（000） =1824,μ = 0.185 mm^-1,MoKa radiation（λ = 0.71073） ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ（I） . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5（1H） -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.
基金Project supported by the National Technology R&D Program (No. 2011 BAE06B01)
文摘The title compound has been synthesized by the reaction of 1-bromo-3,3-dime- thyl- 1 - （1 H- 1,2,4-triazol- 1 -yl）butan-2-one with 1 -（2-fluorophenyl）thiourea, and its crystal struc- ture was determined by single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbca with a = 15.2568（6）, b = 12.1533（5）, c = 16.7307（7） A, Z = 8, V = 3102.2（2） A3, Mr = 317.39, Dc = 1.359 g/cm3, S = 1.05, μ = 0.223 mm-1, F（000） = 1328, the final R = 0.034 and wR = 0.097 for 2590 observed reflections （I 〉 2σ（I））. X-ray crystal structure presents the intramolecular N-H…N hydrogen bond, which plays an important role in stabilizing the crystal structure. In addition, the preliminary biological test on the title compound shows good antitumor activity, with IC50 of 0.122 μmol/mL against the Hela cell line.
基金Supported by the Foundation of 100 Young and Middle-aged Discipline Leaders of Guangxi Province in the 21st century (No 2004219)the Natural Science Foundation of Guangxi Province (No 0731054)
文摘Three novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles were designed,synthesized and characterized by IR,NMR and APCI-MS.3-o-Fluorophenyl-6-（4-decarboxydehydroabietyl）-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole（6a,C28H31FN4S） was structurally determined by single-crystal X-ray diffraction.The crystal belongs to the orthorhombic system,space group P212121 with a=6.0153（14）,b=12.2577（19）,c=34.055（3）A,V=2511.0（7）A^3,Z=4,Mr=474.63,Dc=1.255Mg/m^3,λ=0.71073 A,μ（MoKα）=0.160 mm^-1,F（000）=1008,the final R=0.0555 and wR=0.1248 for 3094 observed reflections with I〉2σ（I）.There are six rings in the crystal structure of the title compound.The dihedral angle between 1,2,4-triazole and 1,3,4-thiadiaole rings is 1.4o,and that between 1,2,4-triazole and benzene ring D 25.5o.
基金the Student Research Fund of Huazhong Agricultural University (11094)the National Undergraduate Innovational Experimentation Program (1210504018)the National Natural Science Foundation of China (31101467)
文摘The chiral molecule （＋）-N-[（3S）-3-（4-fluorophenyl）heptanoyl]bornane-10,2-sultam （C23H32FNO3S, Mr = 421.56）, a fluorine-containing derivative of camphorsultam, was conveniently obtained and crystallized in the orthorhombic space group P212121 with a = 7.9044（11）, b = 11.6680（16）, c = 24.899（3） , V = 2296.4（5） 3, Z = 4, Dc = 1.219 Mg/m3, λ = 0.71073 , μ（MoKα） = 0.172 mm-1 and F（000） = 904. X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat conformation （Fig. 1）. The planes constructed by （（C6）, （C7）, （C8）, （C9）） and （（C4）, （C5）, （C6）, （C9）） form a dihedral angle of 70.3（3）°. The plane of （C1）-（C2）-（C3） forms dihedral angles to the aforementioned planes of 85.9（4） and 89.5（4）°, respectively. The molecules are linked via C-H···O/F interactions.
文摘Geometry optimization and subsequent harmonic vibration calculations of prior synthesized （E）-3-（4-fluorophenyl）-N-[4-（phenyl-amino） quinazoline-7-yl] acrylamide were carried out by DFT/B3LYP method with both 6-31G and 6-311G basis sets.The Infrared （IR） spectrum of the title compound was recorded in the field of 400-4000 cm 1 and then assigned.The correlation analyses between the scaled theoretical vibration frequencies and the experimental ones indicate that there exist good linearity relationships since the correlation coefficients R 2 are larger than 0.999.The intramolecular interactions existed in the title molecule were confirmed by the Atoms in molecules （AIM） method,and their influences on the absorption frequency were also investigated.
