Azilsartan (2-ethoxy-1-([2’-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl)-1H-benzimidazole-7-carboxylic acid) is a new angiotensin II receptor antagonist used in the treatment of hypertension. This pa...Azilsartan (2-ethoxy-1-([2’-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl)-1H-benzimidazole-7-carboxylic acid) is a new angiotensin II receptor antagonist used in the treatment of hypertension. This paper describes the preparation of type I crystal and its single crystal diffraction data, the comparison of the powder diffraction data for both type I and II crystals as well as their stability and solubility in methanol.展开更多
New transition metal complex of Cobalt(III) of the ligand (E)-3-(1-(2-aminoethylimino)ethyl)-4-hydroxy-2H-chromen-2-one, derived from condensation of ethylene diamine with 3-acetyl-4-hydroxy-chromene-2-one have been s...New transition metal complex of Cobalt(III) of the ligand (E)-3-(1-(2-aminoethylimino)ethyl)-4-hydroxy-2H-chromen-2-one, derived from condensation of ethylene diamine with 3-acetyl-4-hydroxy-chromene-2-one have been synthesized by reaction of cobalt(III) salt and the ligand, in amounts equal to metal-ligand molar ratio of 1:2. Both the Schiff base and the complex of Co(III) were characterized by IR, UV-Vis, 1H NMR- and 13C NMR-spectroscopy techniques. Single crystal X-ray diffraction investigation, at low temperature T = 120 K, shows that the cobalt complex is triclinic P-1, a = 10.426(5) ?, b = 11.3234(2) ?, c = 15.729(5) ?, α(°) = 70.102(4), β(°) = 86.049(4), γ(°) = 82.497(4), Z = 2, and its structure consists of isolated [Co(III)(C13H13N2O3)2]+ complex cations with distorted octahedral geometry, ClO-4 counter anions, acetone solvent and water molecules. The crystal cohesion is stabilized by hydrogen bonds between ligands and water molecules, and ionic interactions between complex cations and counter anions.展开更多
The condensation reaction between 5-amino-4, 6-dichloro-2-methylpyrimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4, 6-dichloro-2-methyl-5-(1-acetyl-tetra- hydro-imidazo-2-ylidene)-aminopyrimidine...The condensation reaction between 5-amino-4, 6-dichloro-2-methylpyrimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4, 6-dichloro-2-methyl-5-(1-acetyl-tetra- hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4, 6-dichloro-2-methyl-5-{1-[1-(2- oxo-tetrahydro-imidazolyl)]-acetyene}-aminopyrimidine as by-product. No 4, 6-dichloro-2- methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi- cation-addition-elimination mechanism.展开更多
A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crysta...A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crystal X-ray diffraction. It is indicated that the complex has a 3D architecture through the silver-silver interactions and the bridging eyano groups. This complex displays interesting luminescent properties caused by argentophilieity at room temperature in solid state.展开更多
A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined...A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.展开更多
Two hitherto unknown iboga-type indole alkaloids,namely(3R)-7,19-di-epi-3-methoxytabernoxidine(1)and(3R,19R)-19-hydroxy-3-(2-oxopropyl)voacangine(2),together with eight known alkaloids(3-10),were isolated from the twi...Two hitherto unknown iboga-type indole alkaloids,namely(3R)-7,19-di-epi-3-methoxytabernoxidine(1)and(3R,19R)-19-hydroxy-3-(2-oxopropyl)voacangine(2),together with eight known alkaloids(3-10),were isolated from the twigs and leaves of Tabernaemontana divaricata.Their structures were established on the basis of spectroscopic data interpretation,single crystal X-ray diffraction analysis and circular dichroism spectrum.展开更多
A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-sti...A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium tosylate （DAST） with the benzene sulfonate replacing p-toluenesulfonate. Single crystal XRD demonstrated that the crystal structure of DASBS. H20 was triclinic. The thermal analysis of this new crystal was also conducted, and the melting point was obtained to be 232℃.展开更多
基金We are grateful to the National Natural Science Foundation of China(project 20072034)the Foundation for Young Teacher in Zhenzhou University for the financial support.
文摘Azilsartan (2-ethoxy-1-([2’-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl)-1H-benzimidazole-7-carboxylic acid) is a new angiotensin II receptor antagonist used in the treatment of hypertension. This paper describes the preparation of type I crystal and its single crystal diffraction data, the comparison of the powder diffraction data for both type I and II crystals as well as their stability and solubility in methanol.
文摘New transition metal complex of Cobalt(III) of the ligand (E)-3-(1-(2-aminoethylimino)ethyl)-4-hydroxy-2H-chromen-2-one, derived from condensation of ethylene diamine with 3-acetyl-4-hydroxy-chromene-2-one have been synthesized by reaction of cobalt(III) salt and the ligand, in amounts equal to metal-ligand molar ratio of 1:2. Both the Schiff base and the complex of Co(III) were characterized by IR, UV-Vis, 1H NMR- and 13C NMR-spectroscopy techniques. Single crystal X-ray diffraction investigation, at low temperature T = 120 K, shows that the cobalt complex is triclinic P-1, a = 10.426(5) ?, b = 11.3234(2) ?, c = 15.729(5) ?, α(°) = 70.102(4), β(°) = 86.049(4), γ(°) = 82.497(4), Z = 2, and its structure consists of isolated [Co(III)(C13H13N2O3)2]+ complex cations with distorted octahedral geometry, ClO-4 counter anions, acetone solvent and water molecules. The crystal cohesion is stabilized by hydrogen bonds between ligands and water molecules, and ionic interactions between complex cations and counter anions.
文摘The condensation reaction between 5-amino-4, 6-dichloro-2-methylpyrimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4, 6-dichloro-2-methyl-5-(1-acetyl-tetra- hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4, 6-dichloro-2-methyl-5-{1-[1-(2- oxo-tetrahydro-imidazolyl)]-acetyene}-aminopyrimidine as by-product. No 4, 6-dichloro-2- methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi- cation-addition-elimination mechanism.
文摘A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crystal X-ray diffraction. It is indicated that the complex has a 3D architecture through the silver-silver interactions and the bridging eyano groups. This complex displays interesting luminescent properties caused by argentophilieity at room temperature in solid state.
文摘A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.
基金This work was financially supported by the“Large-scale Compound Library”project of National Development and Reform Commission of China.
文摘Two hitherto unknown iboga-type indole alkaloids,namely(3R)-7,19-di-epi-3-methoxytabernoxidine(1)and(3R,19R)-19-hydroxy-3-(2-oxopropyl)voacangine(2),together with eight known alkaloids(3-10),were isolated from the twigs and leaves of Tabernaemontana divaricata.Their structures were established on the basis of spectroscopic data interpretation,single crystal X-ray diffraction analysis and circular dichroism spectrum.
文摘A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium tosylate （DAST） with the benzene sulfonate replacing p-toluenesulfonate. Single crystal XRD demonstrated that the crystal structure of DASBS. H20 was triclinic. The thermal analysis of this new crystal was also conducted, and the melting point was obtained to be 232℃.
