The crystal structure of the title compound C16H17N2OPS2, has beendetermined by single-crystal X-ray diffraction at 299K. The crystal is monoclinic withspace group P21/n, a=9. 549(2), b= 7- 954(5), c=23. 039(8) A, β=...The crystal structure of the title compound C16H17N2OPS2, has beendetermined by single-crystal X-ray diffraction at 299K. The crystal is monoclinic withspace group P21/n, a=9. 549(2), b= 7- 954(5), c=23. 039(8) A, β= 96. 30(2)°,V= 1739(2) A 3, Z=4, Mr= 348. 3, F(000) = 728, μ(MoKa) =0. 386 mm-1, Dc=1. 331 g/cm3- The final R factor is 0. 044 and Rw is 0. 047 for 1002 observed reflections[I≥3δ(I)]. The five-membered heterocycle has a coplanar structure. The P - N (1)bond length(1. 636 A ) indicates the existence of the d-p π bond between P and N(1)atoms of the title compound.展开更多
One phosphorus heterocycle compound 1, C13H13N2OPS, was synthesized by the reaction of Lawesson＇s reagent （LR） with o-phenylene diamine. The crystal belongs to the orthorhombic system, space group P212121 with a = ...One phosphorus heterocycle compound 1, C13H13N2OPS, was synthesized by the reaction of Lawesson＇s reagent （LR） with o-phenylene diamine. The crystal belongs to the orthorhombic system, space group P212121 with a = 5.5274（11）, b = 8.1603（16）, c = 28.830（6） A, V = 1300.4（4） A^3, Z = 4, Mr= 276.28, Dc = 1.411 g/cm^3, F（000） = 576,μ = 0.360 mm^-1, R = 0.0259 and wR = 0.0652 for 1414 observed reflections with I 〉 2σ（I）. While compound 2, C14H17N2O2PS, was obtained as a ring-cleavage product of compound 1. This crystal is of monoclinic system, space group P21/c with a = 9.5619（19）, b = 21.879（4）, c = 7.3618（15） A, β= 103.03（3）°, V=1500.4（5） A^3, Z = 4, Mr= 308.33, Dc = 1.365 g/cm^3, F（000） = 648,μ = 0.325 mm^-1, R = 0.0383 and wR =0.0742 for 2283 observed reflections with I 〉 2σ（I）. Phosphorus atom in each compound bonds with sulfur and carbon atoms using sp^3 hybrid orbitals, and crystals of these two compounds are formed and stabilized by intermolecular hydrogen bonds and Van der Waals＇ forces. The special structure of compound 1 leads to its good antimicrobial activity against staphylococcus aureus.展开更多
The title compound, C31H30N3OPS3, crystallizes in monoclinic system, space group P21/n,with a = 11.839(7), b = 8.975(5), c = 29.15(2)? b = 100.07(1), V = 3049(3)?, Z = 4, Dc = 1.280g/cm3, Mr = 587.73, F(000) = 1232, m...The title compound, C31H30N3OPS3, crystallizes in monoclinic system, space group P21/n,with a = 11.839(7), b = 8.975(5), c = 29.15(2)? b = 100.07(1), V = 3049(3)?, Z = 4, Dc = 1.280g/cm3, Mr = 587.73, F(000) = 1232, m = 0.324mm-1, the final R = 0.0434 and wR = 0.1140 for 4787 observed reflections with I >2s(I). The title compound is a five-membered heterocycle containing a phosphorus, two nitrogen and two carbon atoms.The analysis result shows that the five-membered ring is nearly coplanar. The P(1)N(1) bond length(1.685? indicates the existence of pd?bond between N(1) and P(1) atoms of the title compound.展开更多
2-Phenoxy-4H-spiro { naphtho[2,3-e] [ 1,4,2]oxazaphosphinane-5,10-dione, 1′-cyclo- hexane}2-oxide （C22H20NO5P） was synthesized by the Mannich-type reaction of 2-amino-3- hydroxy-l,4-naphthoquinone with phenyl phosp...2-Phenoxy-4H-spiro { naphtho[2,3-e] [ 1,4,2]oxazaphosphinane-5,10-dione, 1′-cyclo- hexane}2-oxide （C22H20NO5P） was synthesized by the Mannich-type reaction of 2-amino-3- hydroxy-l,4-naphthoquinone with phenyl phosphorodichloridite and cyclohexanone, and structurally characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P2 1/n with a = 7.9133（11）, b = 13.0269（18）, c = 19.091（3） ,A,β = 101.906（2）°, V= 1925.6（5） ,A^3, Z= 4, Mr = 409.36, Dr = 1.412 g/cm^3, F（000） = 856,μ = 0.178 mm^-1, S = 1.015, the final R = 0.0381 and wR = 0.0906 for 2718 observed reflections with 1 〉 2σ（I） and 262 variable parameters. This compound may be used as DNA-intercalator. Its cytotoxic activities were also tested in vitro on four human tumor cell lines.展开更多
The crystal structure of the title compound, C14H13N2OPS2, has beendetermined by single crystal X-ray diffraction at 299(±1 )K. The crystal is monoclinicwith space group P21/n, a= 11. 310(2), b=8. 363(3), c= 16. ...The crystal structure of the title compound, C14H13N2OPS2, has beendetermined by single crystal X-ray diffraction at 299(±1 )K. The crystal is monoclinicwith space group P21/n, a= 11. 310(2), b=8. 363(3), c= 16. 847(4) A, β= 105. 01(2)°, V= 1539(1) A3, Z=4, Dx= 1. 38g/cm3, μ(M0Ka) = 0. 43mm-1, Mr= 320. 7,F(000) = 644. The final R factor is 0. 051, and R. is 0.052. The result of X-raydiffraction analysis indicates that the atoms P.S(2) 1 N (2).C(11) and N (1) constitutea distorted tetrahedron with sp3 hybridized phosphorus atom in the center.展开更多
文摘The crystal structure of the title compound C16H17N2OPS2, has beendetermined by single-crystal X-ray diffraction at 299K. The crystal is monoclinic withspace group P21/n, a=9. 549(2), b= 7- 954(5), c=23. 039(8) A, β= 96. 30(2)°,V= 1739(2) A 3, Z=4, Mr= 348. 3, F(000) = 728, μ(MoKa) =0. 386 mm-1, Dc=1. 331 g/cm3- The final R factor is 0. 044 and Rw is 0. 047 for 1002 observed reflections[I≥3δ(I)]. The five-membered heterocycle has a coplanar structure. The P - N (1)bond length(1. 636 A ) indicates the existence of the d-p π bond between P and N(1)atoms of the title compound.
基金This work was supported by the National Natural Science Foundation of China (20271046), Natural Science Foundation of Henan Education Department (2004150004) and Natural Foundation of Henan Province (200011500027)
文摘One phosphorus heterocycle compound 1, C13H13N2OPS, was synthesized by the reaction of Lawesson＇s reagent （LR） with o-phenylene diamine. The crystal belongs to the orthorhombic system, space group P212121 with a = 5.5274（11）, b = 8.1603（16）, c = 28.830（6） A, V = 1300.4（4） A^3, Z = 4, Mr= 276.28, Dc = 1.411 g/cm^3, F（000） = 576,μ = 0.360 mm^-1, R = 0.0259 and wR = 0.0652 for 1414 observed reflections with I 〉 2σ（I）. While compound 2, C14H17N2O2PS, was obtained as a ring-cleavage product of compound 1. This crystal is of monoclinic system, space group P21/c with a = 9.5619（19）, b = 21.879（4）, c = 7.3618（15） A, β= 103.03（3）°, V=1500.4（5） A^3, Z = 4, Mr= 308.33, Dc = 1.365 g/cm^3, F（000） = 648,μ = 0.325 mm^-1, R = 0.0383 and wR =0.0742 for 2283 observed reflections with I 〉 2σ（I）. Phosphorus atom in each compound bonds with sulfur and carbon atoms using sp^3 hybrid orbitals, and crystals of these two compounds are formed and stabilized by intermolecular hydrogen bonds and Van der Waals＇ forces. The special structure of compound 1 leads to its good antimicrobial activity against staphylococcus aureus.
基金This project was supported by Foundation for University Key Teacher by the Ministry of Education
文摘The title compound, C31H30N3OPS3, crystallizes in monoclinic system, space group P21/n,with a = 11.839(7), b = 8.975(5), c = 29.15(2)? b = 100.07(1), V = 3049(3)?, Z = 4, Dc = 1.280g/cm3, Mr = 587.73, F(000) = 1232, m = 0.324mm-1, the final R = 0.0434 and wR = 0.1140 for 4787 observed reflections with I >2s(I). The title compound is a five-membered heterocycle containing a phosphorus, two nitrogen and two carbon atoms.The analysis result shows that the five-membered ring is nearly coplanar. The P(1)N(1) bond length(1.685? indicates the existence of pd?bond between N(1) and P(1) atoms of the title compound.
文摘2-Phenoxy-4H-spiro { naphtho[2,3-e] [ 1,4,2]oxazaphosphinane-5,10-dione, 1′-cyclo- hexane}2-oxide （C22H20NO5P） was synthesized by the Mannich-type reaction of 2-amino-3- hydroxy-l,4-naphthoquinone with phenyl phosphorodichloridite and cyclohexanone, and structurally characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P2 1/n with a = 7.9133（11）, b = 13.0269（18）, c = 19.091（3） ,A,β = 101.906（2）°, V= 1925.6（5） ,A^3, Z= 4, Mr = 409.36, Dr = 1.412 g/cm^3, F（000） = 856,μ = 0.178 mm^-1, S = 1.015, the final R = 0.0381 and wR = 0.0906 for 2718 observed reflections with 1 〉 2σ（I） and 262 variable parameters. This compound may be used as DNA-intercalator. Its cytotoxic activities were also tested in vitro on four human tumor cell lines.
文摘The crystal structure of the title compound, C14H13N2OPS2, has beendetermined by single crystal X-ray diffraction at 299(±1 )K. The crystal is monoclinicwith space group P21/n, a= 11. 310(2), b=8. 363(3), c= 16. 847(4) A, β= 105. 01(2)°, V= 1539(1) A3, Z=4, Dx= 1. 38g/cm3, μ(M0Ka) = 0. 43mm-1, Mr= 320. 7,F(000) = 644. The final R factor is 0. 051, and R. is 0.052. The result of X-raydiffraction analysis indicates that the atoms P.S(2) 1 N (2).C(11) and N (1) constitutea distorted tetrahedron with sp3 hybridized phosphorus atom in the center.
