The reaction of 4-（p-fluobenzoyl）-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4（p-fluo-a-aminothiocar...The reaction of 4-（p-fluobenzoyl）-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4（p-fluo-a-aminothiocarbonyl hydrazonobenzal）-2,5-dihydro-3-methyl- 1-phenyl pyrazol-5-one 1. It crystallizes in orthorhombic, space group Pbca with a = 18.445（4）, b = 11.987（2）, c = 19.249（4） °A,, V= 4256.1（18）°A^3, Z = 8, Mr = 415.49, Dc= 1.297 g/cm^3, T = 296（2） K, F（000） = 1744,μ（MoKα） = 0.186 cm^-1, R = 0.0521 and wR = 0.1211 for 1661 observed reflections with I 〉 2σ（I）. The compound was structurally characterized by elemental analyses, IR and ^1H NMR. The intermolecular hydrogen bonds are present and a two-dimensional framework is formed by two intermolecular hydrogen bonds in the （001） plane.展开更多
Trans-2,2?,4,4?-tetramethyl-6,6?-dinitro azobenzene (C16H16N4O4, Mr = 328.32) was isolated from benzene extract of the leaves of Aconitum sungpanense Hand. Mazz. as a new compound, and characterized by spectral method...Trans-2,2?,4,4?-tetramethyl-6,6?-dinitro azobenzene (C16H16N4O4, Mr = 328.32) was isolated from benzene extract of the leaves of Aconitum sungpanense Hand. Mazz. as a new compound, and characterized by spectral methods and X-ray diffraction analysis. It crystallizes in monoclinic system, space group P21/c with a = 8.544(1), b = 13.997(2), c = 7.161(1) ? ?= 112.97(1), V = 788.4(2) ?, Z = 4, Dc = 1.383 g/cm3, F(000) = 344 and ?MoKa) = 0.102 mm-1. The final R = 0.0395 and wR = 0.1140 for 1913 independent reflections with Rint = 0.0109 and 1329 observed reflections with I > 2s(I). The molecule is composed of two phenyl rings through trans N=N.展开更多
The complex {[Mn(H2O)4(3, 3?azpy)](3, 3?azpy)3(PF6)2}n (3, 3?azpy = 3, 3? azobispyridine) has been synthesized and characterized. The crystal (C40H40F12MnN16O4P2, Mr = 1153.76) belongs to the triclinic system, space g...The complex {[Mn(H2O)4(3, 3?azpy)](3, 3?azpy)3(PF6)2}n (3, 3?azpy = 3, 3? azobispyridine) has been synthesized and characterized. The crystal (C40H40F12MnN16O4P2, Mr = 1153.76) belongs to the triclinic system, space group P with the following crystallographic parameters: a = 10.761(2), b = 11.040(2), c = 23.365(4) ? a = 85.52(1), b = 82.69(1), g = 70.44(1)? V = 2592.5(8) 3, Dc = 1.478 g/cm3, m(MoKa) = 4.16 cm-1, F(000) = 1174, Z = 2, final R = 0.0493 and wR = 0.1158 for the observed reflections (I > 2.00s(I)). The X-ray analysis revealed that manganese(Ⅱ) cation coordination environment is a distorted octahedral geometry, and the Mn2+ cation is coordinated by four oxygen atoms of water in the equatorial plane, while the two nitrogen atoms of 3, 3?azpy occupy the axial positions. The complex forms a one-dimensional chain structure via 3, 3?azpy bridging ligand.展开更多
The title complex [Nd(Gly)(H 2O) 7]Cl 3 was synthesized and its crystal structure was determined by X ray diffraction to obtain a final R value of 0 026 0 and a wR value of 0 086 8. The crystal is of m...The title complex [Nd(Gly)(H 2O) 7]Cl 3 was synthesized and its crystal structure was determined by X ray diffraction to obtain a final R value of 0 026 0 and a wR value of 0 086 8. The crystal is of monoclinic system with a space groug Pm . Every two neodymium ions in the crystal are connected with a carboxyl group to form a polymeric chain molecule. And each neodymium ion is further coordinated with seven oxygen atoms from water molecules. The counter ion(Cl -) is non coordinated to fill up the space between the polymeric chains. So the Nd 3+ cation is nine coordinated and the coordination polyhedron is a trigonotetradecahedron. In addition, there exists the mirror symmetry in the complex.展开更多
Treatment of the β-diketiminate-supported ytterbium dichloride LYbCl2（THF）2 1 （L = N,N＇-bis（2,6-dimethylphenyl）-2,4-pentanediiminate） with 2 equiv of C5H5Na gave rise to the title complex LYb（C5H5）2 2 （C31H...Treatment of the β-diketiminate-supported ytterbium dichloride LYbCl2（THF）2 1 （L = N,N＇-bis（2,6-dimethylphenyl）-2,4-pentanediiminate） with 2 equiv of C5H5Na gave rise to the title complex LYb（C5H5）2 2 （C31H35N2Yb, Mr = 608.65）, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2 1/n with a = 14.417（2）, b = 10.432（2）, c = 18.040（4） ,A°, β= 95.73（2）°, V= 2699.6（9） ,A°, Dc = 1.498 g/cm^3, Z = 4, 2（MoKa） = 0.71073 ,A°,μ = 3.485 mm^-1, F（000） = 1220, the final R = 0.0304 and wR = 0.0703 for 3962 observed reflections with I 〉 2σ（I）. In the molecular structure of the title complex, the central metal atom Yb is eight-coordinated by two cyclopentadienyl groups and two nitrogen atoms of ,β- diketiminate group to form a distorted tetrahedral geometry.展开更多
The Schiff base isonicotinaldehyde thiosemicarbazone prepared by the condensation of thiosemicarbazide with pyridine-4-carbaldehyde in ethanol,has been characterized by IR,UV-Vis,element analysis and its stucture dete...The Schiff base isonicotinaldehyde thiosemicarbazone prepared by the condensation of thiosemicarbazide with pyridine-4-carbaldehyde in ethanol,has been characterized by IR,UV-Vis,element analysis and its stucture determined by singl-crystal X-ray diffraction techniques from diffractometer data,Crystal of C7H8N4S is Monoclinic,space group P21/n,with unit cell parameters:a=7.241(1),b=13.963(2),c= 8.416(1),β=90.92°,V=850.91(44)3,Dc=1.407Mg/m3,Z=4,Mr=180.23,μ= 0.327mm-1,F(000)=376,final R1= 0.0315 and wR2= 0.0821(I>2 σ(I)).The crystal packing is stabilized by an extensive two dimensional double layer network of hydrogen bonds(N-H...N and N-H...S).展开更多
The title compound, C16H20INo3, crystallizes in space group P1 (#2),triclinic, a=7. 970(1), b=9. 098(1), c= 12. 910(2) A, a=90. 00(1), β=81. 63(1), γ=65. 75(1)°, V=842. 6(2) A 3, Z=2, Dc= 1. 581 g/cm3,μ(MoKa) ...The title compound, C16H20INo3, crystallizes in space group P1 (#2),triclinic, a=7. 970(1), b=9. 098(1), c= 12. 910(2) A, a=90. 00(1), β=81. 63(1), γ=65. 75(1)°, V=842. 6(2) A 3, Z=2, Dc= 1. 581 g/cm3,μ(MoKa) = 1. 909mm-1, F(000) =400. The final R and (F2)R are 0. 0269 and0. 0632 for 2903 observed reflections (I>2σ(I) ), respectively. In the title molecule, two configurations,A and B were found for the slightly twisted cations, which take the same occupancy inthe crystal equally. Cations are connected through anions 1- and crystallized water,and anti-parallelly packed through intermolecular weak hydrogen bonding, van derWaals interactions and strong π-π interaction.展开更多
The crystal structure of the title compound carvedilol, C24H25N2O4(Mr= 406. 47), has determined by single-crystal X-ray diffraction. The crystal is mono-clinic with space group P21/c, a=9. 094(l), b= l2. 754(1), c= 18...The crystal structure of the title compound carvedilol, C24H25N2O4(Mr= 406. 47), has determined by single-crystal X-ray diffraction. The crystal is mono-clinic with space group P21/c, a=9. 094(l), b= l2. 754(1), c= 18. 330(2) A, β=97. 36(1 )°, V= 2l08. 5(4) A 3, Z= 4, D.= l. 280 g/cm3, F(000) = 864, μ=O. O88mm-1 and final R= O. O368, wR(F2) = 0.0787 for reflections (I>2σ(I) ). X-ray anal-ysis reveals that the crystal is composed of a pair of enantiomer, and there are hydrogenbonds O(3) -H(3O) -N(l ) between the two enantimers. There are two planes in themolecule.展开更多
Ethyl (Z)-α-formylamino-β-arylacrylates were obtained in good yields by the condensation of ethyl N, N-diformylamino acetate and aromatic aldehydes in the presence of sodium ethoxide in ethanol. The structure of eth...Ethyl (Z)-α-formylamino-β-arylacrylates were obtained in good yields by the condensation of ethyl N, N-diformylamino acetate and aromatic aldehydes in the presence of sodium ethoxide in ethanol. The structure of ethyl α-formylaminocinnamate was characterized by single crystal X-ray diffraction measurement.展开更多
Three 1:1 adducts have been obtained by heating benzaldoxime dehydrodimer with styrene. The main product possesses the structure of bis-nitrone type. A radical addition mechanism is pro- posed.
基金This project was supported by the National Natural Science Foundation of China (No. 20462007) and Xinjiang Bureau of Education (No. XJEDU2004S06)
文摘The reaction of 4-（p-fluobenzoyl）-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4（p-fluo-a-aminothiocarbonyl hydrazonobenzal）-2,5-dihydro-3-methyl- 1-phenyl pyrazol-5-one 1. It crystallizes in orthorhombic, space group Pbca with a = 18.445（4）, b = 11.987（2）, c = 19.249（4） °A,, V= 4256.1（18）°A^3, Z = 8, Mr = 415.49, Dc= 1.297 g/cm^3, T = 296（2） K, F（000） = 1744,μ（MoKα） = 0.186 cm^-1, R = 0.0521 and wR = 0.1211 for 1661 observed reflections with I 〉 2σ（I）. The compound was structurally characterized by elemental analyses, IR and ^1H NMR. The intermolecular hydrogen bonds are present and a two-dimensional framework is formed by two intermolecular hydrogen bonds in the （001） plane.
基金This work was supported by the Natural Science Foundation of Shaanxi Province (No. 01JK080 and 02JS40).
文摘Trans-2,2?,4,4?-tetramethyl-6,6?-dinitro azobenzene (C16H16N4O4, Mr = 328.32) was isolated from benzene extract of the leaves of Aconitum sungpanense Hand. Mazz. as a new compound, and characterized by spectral methods and X-ray diffraction analysis. It crystallizes in monoclinic system, space group P21/c with a = 8.544(1), b = 13.997(2), c = 7.161(1) ? ?= 112.97(1), V = 788.4(2) ?, Z = 4, Dc = 1.383 g/cm3, F(000) = 344 and ?MoKa) = 0.102 mm-1. The final R = 0.0395 and wR = 0.1140 for 1913 independent reflections with Rint = 0.0109 and 1329 observed reflections with I > 2s(I). The molecule is composed of two phenyl rings through trans N=N.
基金Supported by the funds of Organic Syntheses Key Laboratory of Jiangsu Province
文摘The complex {[Mn(H2O)4(3, 3?azpy)](3, 3?azpy)3(PF6)2}n (3, 3?azpy = 3, 3? azobispyridine) has been synthesized and characterized. The crystal (C40H40F12MnN16O4P2, Mr = 1153.76) belongs to the triclinic system, space group P with the following crystallographic parameters: a = 10.761(2), b = 11.040(2), c = 23.365(4) ? a = 85.52(1), b = 82.69(1), g = 70.44(1)? V = 2592.5(8) 3, Dc = 1.478 g/cm3, m(MoKa) = 4.16 cm-1, F(000) = 1174, Z = 2, final R = 0.0493 and wR = 0.1158 for the observed reflections (I > 2.00s(I)). The X-ray analysis revealed that manganese(Ⅱ) cation coordination environment is a distorted octahedral geometry, and the Mn2+ cation is coordinated by four oxygen atoms of water in the equatorial plane, while the two nitrogen atoms of 3, 3?azpy occupy the axial positions. The complex forms a one-dimensional chain structure via 3, 3?azpy bridging ligand.
文摘The title complex [Nd(Gly)(H 2O) 7]Cl 3 was synthesized and its crystal structure was determined by X ray diffraction to obtain a final R value of 0 026 0 and a wR value of 0 086 8. The crystal is of monoclinic system with a space groug Pm . Every two neodymium ions in the crystal are connected with a carboxyl group to form a polymeric chain molecule. And each neodymium ion is further coordinated with seven oxygen atoms from water molecules. The counter ion(Cl -) is non coordinated to fill up the space between the polymeric chains. So the Nd 3+ cation is nine coordinated and the coordination polyhedron is a trigonotetradecahedron. In addition, there exists the mirror symmetry in the complex.
基金Supported by the National Natural Science Foundation of China (20072027)
文摘Treatment of the β-diketiminate-supported ytterbium dichloride LYbCl2（THF）2 1 （L = N,N＇-bis（2,6-dimethylphenyl）-2,4-pentanediiminate） with 2 equiv of C5H5Na gave rise to the title complex LYb（C5H5）2 2 （C31H35N2Yb, Mr = 608.65）, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2 1/n with a = 14.417（2）, b = 10.432（2）, c = 18.040（4） ,A°, β= 95.73（2）°, V= 2699.6（9） ,A°, Dc = 1.498 g/cm^3, Z = 4, 2（MoKa） = 0.71073 ,A°,μ = 3.485 mm^-1, F（000） = 1220, the final R = 0.0304 and wR = 0.0703 for 3962 observed reflections with I 〉 2σ（I）. In the molecular structure of the title complex, the central metal atom Yb is eight-coordinated by two cyclopentadienyl groups and two nitrogen atoms of ,β- diketiminate group to form a distorted tetrahedral geometry.
文摘The Schiff base isonicotinaldehyde thiosemicarbazone prepared by the condensation of thiosemicarbazide with pyridine-4-carbaldehyde in ethanol,has been characterized by IR,UV-Vis,element analysis and its stucture determined by singl-crystal X-ray diffraction techniques from diffractometer data,Crystal of C7H8N4S is Monoclinic,space group P21/n,with unit cell parameters:a=7.241(1),b=13.963(2),c= 8.416(1),β=90.92°,V=850.91(44)3,Dc=1.407Mg/m3,Z=4,Mr=180.23,μ= 0.327mm-1,F(000)=376,final R1= 0.0315 and wR2= 0.0821(I>2 σ(I)).The crystal packing is stabilized by an extensive two dimensional double layer network of hydrogen bonds(N-H...N and N-H...S).
文摘The title compound, C16H20INo3, crystallizes in space group P1 (#2),triclinic, a=7. 970(1), b=9. 098(1), c= 12. 910(2) A, a=90. 00(1), β=81. 63(1), γ=65. 75(1)°, V=842. 6(2) A 3, Z=2, Dc= 1. 581 g/cm3,μ(MoKa) = 1. 909mm-1, F(000) =400. The final R and (F2)R are 0. 0269 and0. 0632 for 2903 observed reflections (I>2σ(I) ), respectively. In the title molecule, two configurations,A and B were found for the slightly twisted cations, which take the same occupancy inthe crystal equally. Cations are connected through anions 1- and crystallized water,and anti-parallelly packed through intermolecular weak hydrogen bonding, van derWaals interactions and strong π-π interaction.
文摘The crystal structure of the title compound carvedilol, C24H25N2O4(Mr= 406. 47), has determined by single-crystal X-ray diffraction. The crystal is mono-clinic with space group P21/c, a=9. 094(l), b= l2. 754(1), c= 18. 330(2) A, β=97. 36(1 )°, V= 2l08. 5(4) A 3, Z= 4, D.= l. 280 g/cm3, F(000) = 864, μ=O. O88mm-1 and final R= O. O368, wR(F2) = 0.0787 for reflections (I>2σ(I) ). X-ray anal-ysis reveals that the crystal is composed of a pair of enantiomer, and there are hydrogenbonds O(3) -H(3O) -N(l ) between the two enantimers. There are two planes in themolecule.
文摘Ethyl (Z)-α-formylamino-β-arylacrylates were obtained in good yields by the condensation of ethyl N, N-diformylamino acetate and aromatic aldehydes in the presence of sodium ethoxide in ethanol. The structure of ethyl α-formylaminocinnamate was characterized by single crystal X-ray diffraction measurement.
文摘Three 1:1 adducts have been obtained by heating benzaldoxime dehydrodimer with styrene. The main product possesses the structure of bis-nitrone type. A radical addition mechanism is pro- posed.
