One kind of new cefazolin sodium hydrate crystal was obtained in the isopropyl alcohol-water system.There are two symmetry independent molecules in the asymmetric unit,both being well ordered in the lattice,and ten in...One kind of new cefazolin sodium hydrate crystal was obtained in the isopropyl alcohol-water system.There are two symmetry independent molecules in the asymmetric unit,both being well ordered in the lattice,and ten independent water positions but generally four to six(mean five)water molecules and one sodium ion present in the unit cell structure.Huge solvent tunnels can be found.Again there are two general regions of water molecules,those in the large solvent tunnels and those in proximity of the sodium ion and the tetrazole moieties of the drug molecule.The physical and chemical characteristics of the new cefazolin sodium hydrate crystal are similar to that of the α-form cefazolin sodium crystal,and the new crystal has better chemical stability than amorphous cefazolin sodium powder.展开更多
Capillarin was isolated from Artemisia Ordosica Kraschen and characterized by IR, 1H-NMR, 13C-NMR, 1H-1HCOSY, HMQC, HMBC and EIMS, and its crystal structure was determined by single-crystal X-ray diffraction analysis ...Capillarin was isolated from Artemisia Ordosica Kraschen and characterized by IR, 1H-NMR, 13C-NMR, 1H-1HCOSY, HMQC, HMBC and EIMS, and its crystal structure was determined by single-crystal X-ray diffraction analysis with the following data: triclinic, space group P1, Z = 2, a = 7.226(6), b = 7.297(6), c = 11.042(8) ?, α = 74.695(12), β = 78.479(12), γ = 62.063(10)°, V = 494.2(6) ?3, Mr = 198.21, Dc = 1.332 g/cm3, F(000) = 208, μ = 0.089 mm-1, S = 1.023, (?/σ)max = 0.000, the final R = 0.0408 and wR = 0.1110. The largest peak and deepest hole on the final difference Fourier map are 0.219 and –0.161 e/?3, respectively. The bond lengths and bond angles of the molecule are also given.展开更多
Two new triterpenoid saponins named notoginsenoside-Ng3(1) and notoginsenoside-Ng4(2) along with three known saponins (3-5), were isolated from a water extract of the leaves of Panax notoginseng. Their structures were...Two new triterpenoid saponins named notoginsenoside-Ng3(1) and notoginsenoside-Ng4(2) along with three known saponins (3-5), were isolated from a water extract of the leaves of Panax notoginseng. Their structures were elucidated by HRESIMS, NMR, X-ray techniques and acid hydrolysis. Moreover,compound 2 was characterized with the conjugated double bonds side-chain, which was rarely found in this plant. The absolute configuration of notoginsenoside Fa (3) with five sugars was confirmed by the single-crystal X-ray diffraction for the first time. Acetylcholinesterase inhibitory activity experiments were also conducted, all the isolated saponins showed weak inhibitory activities in the final concentration of 0.16 mmol/L.展开更多
In an attempt to compare crystal structure determination from powder data and single-crystal data,crystal structure of griseofulvin(C 17 H 17 ClO 6) was tested by both powder and single-crystal X-ray diffraction.Latti...In an attempt to compare crystal structure determination from powder data and single-crystal data,crystal structure of griseofulvin(C 17 H 17 ClO 6) was tested by both powder and single-crystal X-ray diffraction.Lattice parameters of griseofulvin are α=90.0°,a=b=8.9757,c=19.9345,V=1605.99 3 from powder data coinciding with α=90.0°,a=b=8.9714,c=19.8848,V=1600.46 3 from single-crystal data.Main processes of structure elucidating of griseofulvin by the two approaches were analyzed.Powder X-ray diffraction was demonstrated to be a powerful auxiliary implement to single-crystal X-ray diffraction in structure characterization,and its application can be popularized in the field of structure research of small organic molecules.展开更多
The crystal structure of the title compound （Z）-5-fluoro-3-（phenyl（（5-（pyridin-3- ylmethyl）thiophen-2-yl）amino）methylene） indolin-2-one （C25H18FN3OS, Mr = 427.50） has been prepared and determined by single...The crystal structure of the title compound （Z）-5-fluoro-3-（phenyl（（5-（pyridin-3- ylmethyl）thiophen-2-yl）amino）methylene） indolin-2-one （C25H18FN3OS, Mr = 427.50） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 5.931（1）, b = 12.413（1）, c = 28.102（2） A, V= 2090.4（3） A3, Z = 4, Dc = 1.358 g/cm3, F（000） = 888, μ= 0.186 mm-1, MoKa radiation （2 = 0.71073）, R = 0.041 and wR = 0.105 for 4567 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and thiophene rings are not coplanar with a dihedral angle of 46.26（5）°. Intramolecular and intermolecular N-H＇..O hydrogen bonds together with C-H...π interations can be observed in the lattice.展开更多
Dexmedetomidine and its novel salt have been synthesized and characterized by single-crystal XRD and TGA/DSG. Components of the crystalline phase have also been investigated in terms of their corresponding Hirshfeld s...Dexmedetomidine and its novel salt have been synthesized and characterized by single-crystal XRD and TGA/DSG. Components of the crystalline phase have also been investigated in terms of their corresponding Hirshfeld surface. In the crystal lattice, a three-dimensional hydrogen-bonded network is observed. In this work, the salt strategy has been applied successfully to dexmedetomidine. One important parameter, i.e. stability, has also been significantly improved, which proves to be an important factor for solid dosage formulation. Furthermore, DSC/TGA analysis indicates that the salt maintains its crystallinity up to 300℃, suggesting a higher stability of the salt compared to pure dexmedetomidine.展开更多
文摘One kind of new cefazolin sodium hydrate crystal was obtained in the isopropyl alcohol-water system.There are two symmetry independent molecules in the asymmetric unit,both being well ordered in the lattice,and ten independent water positions but generally four to six(mean five)water molecules and one sodium ion present in the unit cell structure.Huge solvent tunnels can be found.Again there are two general regions of water molecules,those in the large solvent tunnels and those in proximity of the sodium ion and the tetrazole moieties of the drug molecule.The physical and chemical characteristics of the new cefazolin sodium hydrate crystal are similar to that of the α-form cefazolin sodium crystal,and the new crystal has better chemical stability than amorphous cefazolin sodium powder.
基金The project was supported by Henan Innovation Project for University Prominent Research Talents (2004)
文摘Capillarin was isolated from Artemisia Ordosica Kraschen and characterized by IR, 1H-NMR, 13C-NMR, 1H-1HCOSY, HMQC, HMBC and EIMS, and its crystal structure was determined by single-crystal X-ray diffraction analysis with the following data: triclinic, space group P1, Z = 2, a = 7.226(6), b = 7.297(6), c = 11.042(8) ?, α = 74.695(12), β = 78.479(12), γ = 62.063(10)°, V = 494.2(6) ?3, Mr = 198.21, Dc = 1.332 g/cm3, F(000) = 208, μ = 0.089 mm-1, S = 1.023, (?/σ)max = 0.000, the final R = 0.0408 and wR = 0.1110. The largest peak and deepest hole on the final difference Fourier map are 0.219 and –0.161 e/?3, respectively. The bond lengths and bond angles of the molecule are also given.
基金financially supported by the National Natural Science Foundation of China(Nos. 81630094and 81730093)CAMS Innovation Fund for Medical Sciences (CIFMS)(No. 2016-I2M-2-003)
文摘Two new triterpenoid saponins named notoginsenoside-Ng3(1) and notoginsenoside-Ng4(2) along with three known saponins (3-5), were isolated from a water extract of the leaves of Panax notoginseng. Their structures were elucidated by HRESIMS, NMR, X-ray techniques and acid hydrolysis. Moreover,compound 2 was characterized with the conjugated double bonds side-chain, which was rarely found in this plant. The absolute configuration of notoginsenoside Fa (3) with five sugars was confirmed by the single-crystal X-ray diffraction for the first time. Acetylcholinesterase inhibitory activity experiments were also conducted, all the isolated saponins showed weak inhibitory activities in the final concentration of 0.16 mmol/L.
基金Supported by national significant industry and technology special projects ( high-tech development and reform commission [2008]No. 2441)the president of Chinese Academy of Forestry foundation (CAFYBB2008009)the 948 program of the State Forestry Administration (2009 - 4 - 55)
文摘In an attempt to compare crystal structure determination from powder data and single-crystal data,crystal structure of griseofulvin(C 17 H 17 ClO 6) was tested by both powder and single-crystal X-ray diffraction.Lattice parameters of griseofulvin are α=90.0°,a=b=8.9757,c=19.9345,V=1605.99 3 from powder data coinciding with α=90.0°,a=b=8.9714,c=19.8848,V=1600.46 3 from single-crystal data.Main processes of structure elucidating of griseofulvin by the two approaches were analyzed.Powder X-ray diffraction was demonstrated to be a powerful auxiliary implement to single-crystal X-ray diffraction in structure characterization,and its application can be popularized in the field of structure research of small organic molecules.
基金Sponsored by the Natural Science Foundation of Jiangsu Province(No.BK2011088)
文摘The crystal structure of the title compound （Z）-5-fluoro-3-（phenyl（（5-（pyridin-3- ylmethyl）thiophen-2-yl）amino）methylene） indolin-2-one （C25H18FN3OS, Mr = 427.50） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 5.931（1）, b = 12.413（1）, c = 28.102（2） A, V= 2090.4（3） A3, Z = 4, Dc = 1.358 g/cm3, F（000） = 888, μ= 0.186 mm-1, MoKa radiation （2 = 0.71073）, R = 0.041 and wR = 0.105 for 4567 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and thiophene rings are not coplanar with a dihedral angle of 46.26（5）°. Intramolecular and intermolecular N-H＇..O hydrogen bonds together with C-H...π interations can be observed in the lattice.
基金supported by the prospective joint research project of Jiangsu province(BY20122193)the Fundamental Research Funds for the Central Universities(CXZZ12_0119)
文摘Dexmedetomidine and its novel salt have been synthesized and characterized by single-crystal XRD and TGA/DSG. Components of the crystalline phase have also been investigated in terms of their corresponding Hirshfeld surface. In the crystal lattice, a three-dimensional hydrogen-bonded network is observed. In this work, the salt strategy has been applied successfully to dexmedetomidine. One important parameter, i.e. stability, has also been significantly improved, which proves to be an important factor for solid dosage formulation. Furthermore, DSC/TGA analysis indicates that the salt maintains its crystallinity up to 300℃, suggesting a higher stability of the salt compared to pure dexmedetomidine.
