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
The crystal structure of a new compound （Z）-N-（2-（diethylamino）ethyl）-7-（5- fluoro-2-oxoindolin-3-ylidene）-2-methyl-4,5,6,7-tetrahydro- 1H-indole-3 -carboxamidemethanol solvate （C24H29FNaO2CH40, Mr = 456.55）...The crystal structure of a new compound （Z）-N-（2-（diethylamino）ethyl）-7-（5- fluoro-2-oxoindolin-3-ylidene）-2-methyl-4,5,6,7-tetrahydro- 1H-indole-3 -carboxamidemethanol solvate （C24H29FNaO2CH40, Mr = 456.55） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P2 1/c with a = 14.560（3）, b = 7.3200（2）, c = 22.233（4） A, β = 101.78（3）°, V = 2319.7（8） A3, Z = 4, Dc = 1.307 g/cm^3, F（000） = 976, p = 0.092 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0604 and wR = 0.1644 for 4262 observed reflections with 1 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and pyrrole are almost coplanar. Intramolecular C-H---O and N-H---O hydrogen bonds together with rc-zr interactions are found in the structure.展开更多
The crystal structure of the new title compound 2,2-dimethyl-4-oxochroman-3-ylmorpholine-4-carbodithioate（C16H19NO3S2,Mr = 337.44） has been prepared and determined by single-crystal X-ray diffraction.The crystal is ...The crystal structure of the new title compound 2,2-dimethyl-4-oxochroman-3-ylmorpholine-4-carbodithioate（C16H19NO3S2,Mr = 337.44） has been prepared and determined by single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 9.5518（7）,b = 9.7172（7）,c = 11.0220（8）,α = 67.08（1）,β = 74.66（1）,= 61.31（1）°,V = 822.72（10）3,Z = 2,Dc = 1.362 g/cm3,F（000） = 356,μ = 0.092 mm-1,MoKa radiation（λ = 0.71073）,R = 0.0515 and wR = 0.1389 for 2623 observed reflections with I 2（I）.X-ray diffraction analysis reveals that the chroman ring adopts a half-chair conformation while the morpholine ring shows a chair conformation.Intramolecular and intermolecular C–H···S and C–H···O hydrogen bonds together with π-π interations are found in the structure.The result of MTT assay shows the title compound displays good antiproliferative activity against two human cancer cell lines.展开更多
The novel crystal of the title compound 2-（（（5-（（（5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl）thio）methyl）-4-phenyl-4H-1,2,4-triazol-3-yl）thio）methyl）-4H-chromen-4-one methanol solvate（C27H25N7O3...The novel crystal of the title compound 2-（（（5-（（（5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl）thio）methyl）-4-phenyl-4H-1,2,4-triazol-3-yl）thio）methyl）-4H-chromen-4-one methanol solvate（C27H25N7O3S2, Mr = 559.66） has been prepared and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monocline system, space group P21/c with a = 11.9879（9）, b = 14.0743（10）, c = 15.9706（11）A, β = 98.509（2）°, V = 2664.9（3）A3, Z = 4, Dc = 1.395 g/cm^3, F（000） = 1168, μ = 0.116 mm-1, MoKa radiation（λ = 0.71073）, R = 0.0652, and wR = 0.1425 for 5220 observed reflections with I 〉 2σ（I）. X-ray diffraction analyses reveal that the molecule adopts a C-shape. The planes of the benzopyrone and triazolopyrimidine were nearly parallel to each other, with a dihedral angle of 1.21（3）°. Intramolecular and intermolecular hydrogen bonds together with π-π interations are found to exist in the structure. The results of MTT assay indicate that the title compound displays excellent antiproliferative activity against two human cancer cell lines.展开更多
A new cobalt（Ⅱ） coordination polymer with the formula of [Co（iqnc）2]n（1, iqnc = l-isoquinolinecarboxylate） has been synthesized through hydrothermal synthesis and structurally characterized by single-crystal X-...A new cobalt（Ⅱ） coordination polymer with the formula of [Co（iqnc）2]n（1, iqnc = l-isoquinolinecarboxylate） has been synthesized through hydrothermal synthesis and structurally characterized by single-crystal X-ray diffraction method. The title coordination polymer represents a two-dimensional layer structure featuring adjacent one-dimensional [Co（iqnc）2]n chains connected with each other by uncoordinated oxygen atoms of carboxylate. Crystal data： monoclinic, space group P21/c, a = 15.4302（2）, b = 5.6743（7）, c = 9.2307（1） A, β = 98.459（2）o, V = 799.41（2） A3, Z = 2, S = 1.019, the final R = 0.0346, w R = 0.0876（I 2σ（I）） and R = 0.0477 and wR = 0.1159 for all reflections. In addition, elemental analysis, IR, and magnetism properties are presented.展开更多
Screening active natural products, rapid identification, and accurate isolation are of great important for modern natural lead compounds discovery1. We hereby reported the isolation of seven new neotecleanin-type limo...Screening active natural products, rapid identification, and accurate isolation are of great important for modern natural lead compounds discovery1. We hereby reported the isolation of seven new neotecleanin-type limonoids(1–7), seven new limonoids with 5-oxatricyclo[5.4.0.11,4]hendecane ring system(8–14), and two new precursors(15–16) together with four known limonoids(17–20) from the root barks of Walsura robusta. Their structures, including their absolute configurations, were elucidated based on analyses of HR-ESI-MS, 1D/2D NMR, ECD spectrum calculations and singlecrystal X-ray diffraction techniques. Compounds 2, 8, 9, 11, 13, 14, 18 showed significant anti-inflammatory activities in LPS-induced RAW 264.7 cell line, BV2 microglial cells, and Propionibacterium acnes-stimulated THP-1 human monocytic cells. Walrobsin M(11) exhibited anti-inflammatory activity with IC50 value of 7.9670.36 μmol/L, and down-regulated phosphorylation levels of ERK and p38 in a dose-dependent manner.展开更多
Two new lanthanide coordination polymers [Ln（C5H2N2O4）（H2O）2（C2O4）0.5]nH2O （Ln = CeⅢ （1） or PrⅢ （2）; C5H2N2O4 = imidazole-4,5-dicarboxylate anion; C2O4 = oxalate anion） have been synthesized and structur...Two new lanthanide coordination polymers [Ln（C5H2N2O4）（H2O）2（C2O4）0.5]nH2O （Ln = CeⅢ （1） or PrⅢ （2）; C5H2N2O4 = imidazole-4,5-dicarboxylate anion; C2O4 = oxalate anion） have been synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectrum. Both compounds crystallize in monoclinic, space group P21/c with a = 7.5225（3）, b = 17.2416（6）, c = 8.6089（3） A, β = 110.9610（10）°, V = 1042.68（7） A3, Z = 4, C6H8N2O9Ce, Mr = 392.26, Dc = 2.499 g/cm3, μ（MoKa） = 4.414 mm^-1, F（000） = 752, the final R = 0.0167 and wR = 0.0412 for 1; a = 7.4973（3）, b = 17.2113（8）, c = 8.5729（4） A, β = 110.9440（10）°, V = 1033.14（8） A3, Z = 4, C6HgN2O9Pr, Mr = 393.05, Dc = 2.527 g/cm3, μ（MoKa） = 4.764 mm^-1, F（000） = 756, the final R = 0.0192 and wR = 0.0455 for 2. X-ray diffraction analyses reveal that the lanthanide cations in compound 1 or 2 are linked by imidazole-4,5-dicarboxylate and in situ generated oxalate anions via Ln-O and Ln-N covalent bonds to form two-dimensional layered networks. The successful synthesis of compound 1 or 2 also indicates a crystallographic confirmation for the decomposition of curcumin to form oxalate anion under solvothermal conditions.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.
基金Supported by Policy Guiding Project of Science and Technology Bureau of Xinjiang Production and Construction Corps(2006YD29)Open Project of Xinjiang Prodution and Constrction Key Laboratory of Protection and Utilization of Biological Resources in Tarim Basin(BR0609)
基金supported by the major research plan of drug design and development (No.2009ZX09102-002)scientific/technical innovation and commercialization of Jiangsu province (BE2011602)
文摘The crystal structure of a new compound （Z）-N-（2-（diethylamino）ethyl）-7-（5- fluoro-2-oxoindolin-3-ylidene）-2-methyl-4,5,6,7-tetrahydro- 1H-indole-3 -carboxamidemethanol solvate （C24H29FNaO2CH40, Mr = 456.55） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P2 1/c with a = 14.560（3）, b = 7.3200（2）, c = 22.233（4） A, β = 101.78（3）°, V = 2319.7（8） A3, Z = 4, Dc = 1.307 g/cm^3, F（000） = 976, p = 0.092 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0604 and wR = 0.1644 for 4262 observed reflections with 1 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and pyrrole are almost coplanar. Intramolecular C-H---O and N-H---O hydrogen bonds together with rc-zr interactions are found in the structure.
基金supported by the National Natural Science Foundation of China(No.21272086)China Postdoctoral Science Foundation(No.2012T50475)the Natural Science Foundation of Jiangsu Province(No.BK2011086)
文摘The crystal structure of the new title compound 2,2-dimethyl-4-oxochroman-3-ylmorpholine-4-carbodithioate（C16H19NO3S2,Mr = 337.44） has been prepared and determined by single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 9.5518（7）,b = 9.7172（7）,c = 11.0220（8）,α = 67.08（1）,β = 74.66（1）,= 61.31（1）°,V = 822.72（10）3,Z = 2,Dc = 1.362 g/cm3,F（000） = 356,μ = 0.092 mm-1,MoKa radiation（λ = 0.71073）,R = 0.0515 and wR = 0.1389 for 2623 observed reflections with I 2（I）.X-ray diffraction analysis reveals that the chroman ring adopts a half-chair conformation while the morpholine ring shows a chair conformation.Intramolecular and intermolecular C–H···S and C–H···O hydrogen bonds together with π-π interations are found in the structure.The result of MTT assay shows the title compound displays good antiproliferative activity against two human cancer cell lines.
基金Supported by the Natural Science Foundation of Jiangsu Province(No.BK2011088)
文摘The novel crystal of the title compound 2-（（（5-（（（5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl）thio）methyl）-4-phenyl-4H-1,2,4-triazol-3-yl）thio）methyl）-4H-chromen-4-one methanol solvate（C27H25N7O3S2, Mr = 559.66） has been prepared and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monocline system, space group P21/c with a = 11.9879（9）, b = 14.0743（10）, c = 15.9706（11）A, β = 98.509（2）°, V = 2664.9（3）A3, Z = 4, Dc = 1.395 g/cm^3, F（000） = 1168, μ = 0.116 mm-1, MoKa radiation（λ = 0.71073）, R = 0.0652, and wR = 0.1425 for 5220 observed reflections with I 〉 2σ（I）. X-ray diffraction analyses reveal that the molecule adopts a C-shape. The planes of the benzopyrone and triazolopyrimidine were nearly parallel to each other, with a dihedral angle of 1.21（3）°. Intramolecular and intermolecular hydrogen bonds together with π-π interations are found to exist in the structure. The results of MTT assay indicate that the title compound displays excellent antiproliferative activity against two human cancer cell lines.
基金Supported by the National Natural Science Foundation of China(No.21203160)Education Department Foundation of Shaanxi Province(No.12JK0631)+1 种基金Natural Science Foundation of Shaanxi Province(No.2013JM2013)Special Research Fund of Xianyang Normal University(No.11XSYK204,11XSYK205,12XSYK023)
文摘A new cobalt（Ⅱ） coordination polymer with the formula of [Co（iqnc）2]n（1, iqnc = l-isoquinolinecarboxylate） has been synthesized through hydrothermal synthesis and structurally characterized by single-crystal X-ray diffraction method. The title coordination polymer represents a two-dimensional layer structure featuring adjacent one-dimensional [Co（iqnc）2]n chains connected with each other by uncoordinated oxygen atoms of carboxylate. Crystal data： monoclinic, space group P21/c, a = 15.4302（2）, b = 5.6743（7）, c = 9.2307（1） A, β = 98.459（2）o, V = 799.41（2） A3, Z = 2, S = 1.019, the final R = 0.0346, w R = 0.0876（I 2σ（I）） and R = 0.0477 and wR = 0.1159 for all reflections. In addition, elemental analysis, IR, and magnetism properties are presented.
基金This work was financially supported by the National Natural Science Foundation of China(30500632)the National Science Fund for Distinguished Young Scholars to Y.-M.Shen(30325044)
基金Financial support for this study by the National Natural Science Foundation of China (31470416, China)the Outstanding Youth Fund of the Basic Research Program of Jiangsu Province (BK20160077, China)+1 种基金the Program for Changjiang Scholars and Innovative Research Team in University (IRT_15R63, China)the "Double First-Class" University project (CPU2018GY08, China)
文摘Screening active natural products, rapid identification, and accurate isolation are of great important for modern natural lead compounds discovery1. We hereby reported the isolation of seven new neotecleanin-type limonoids(1–7), seven new limonoids with 5-oxatricyclo[5.4.0.11,4]hendecane ring system(8–14), and two new precursors(15–16) together with four known limonoids(17–20) from the root barks of Walsura robusta. Their structures, including their absolute configurations, were elucidated based on analyses of HR-ESI-MS, 1D/2D NMR, ECD spectrum calculations and singlecrystal X-ray diffraction techniques. Compounds 2, 8, 9, 11, 13, 14, 18 showed significant anti-inflammatory activities in LPS-induced RAW 264.7 cell line, BV2 microglial cells, and Propionibacterium acnes-stimulated THP-1 human monocytic cells. Walrobsin M(11) exhibited anti-inflammatory activity with IC50 value of 7.9670.36 μmol/L, and down-regulated phosphorylation levels of ERK and p38 in a dose-dependent manner.
基金supported by the Natural Science Foundation of Heilongjiang Province (No.B200917)Education Office Foundation of Heilongjiang Province(No.11551484)+2 种基金Foundation of Jiamusi University (No.Szj2008-017)Sci.& Tech.Project of Heilongjiang Province (2009G1099-00)Doctoral Foundation of Material Science Key Discipline of Jiamusi University (No.E08050207)
文摘Two new lanthanide coordination polymers [Ln（C5H2N2O4）（H2O）2（C2O4）0.5]nH2O （Ln = CeⅢ （1） or PrⅢ （2）; C5H2N2O4 = imidazole-4,5-dicarboxylate anion; C2O4 = oxalate anion） have been synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectrum. Both compounds crystallize in monoclinic, space group P21/c with a = 7.5225（3）, b = 17.2416（6）, c = 8.6089（3） A, β = 110.9610（10）°, V = 1042.68（7） A3, Z = 4, C6H8N2O9Ce, Mr = 392.26, Dc = 2.499 g/cm3, μ（MoKa） = 4.414 mm^-1, F（000） = 752, the final R = 0.0167 and wR = 0.0412 for 1; a = 7.4973（3）, b = 17.2113（8）, c = 8.5729（4） A, β = 110.9440（10）°, V = 1033.14（8） A3, Z = 4, C6HgN2O9Pr, Mr = 393.05, Dc = 2.527 g/cm3, μ（MoKa） = 4.764 mm^-1, F（000） = 756, the final R = 0.0192 and wR = 0.0455 for 2. X-ray diffraction analyses reveal that the lanthanide cations in compound 1 or 2 are linked by imidazole-4,5-dicarboxylate and in situ generated oxalate anions via Ln-O and Ln-N covalent bonds to form two-dimensional layered networks. The successful synthesis of compound 1 or 2 also indicates a crystallographic confirmation for the decomposition of curcumin to form oxalate anion under solvothermal conditions.
