Fe+ ion beams with the energy of 110 keV were implanted into films of L(+)-cysteine (HSCH2CH(NH2)COOH). One of the single crystals grown in hydrochloric acid solution with the implanted samples through slow evaporatio...Fe+ ion beams with the energy of 110 keV were implanted into films of L(+)-cysteine (HSCH2CH(NH2)COOH). One of the single crystals grown in hydrochloric acid solution with the implanted samples through slow evaporation was structurally characterized by the X-ray crystallography. The crystal is monoclinic, space group C2, with a = 1.8534(4) nm, b=0.5234(1) nm, c = 0.7212(1) nm, β=103.722°, V = 0.67965(3) nm3, Z = 4, F(000) = 144.0, Dclac = 1.763 g·cm-3, μ (MoKa) = 1.06 mm-1, T = 293(2) K.R = 0.0379, wR = 0.0835 for 660 observed reflections (I】2σ(I)). The structural formula of the crystal compound is (CH2CH(NH2)NO2)ClFe (Mr = 180.38u). Products of heavy ion beam irradiation were purified and it was directly confirmed that the implanted Fe+ ions had been deposited in the novel molecules. The same doses of Fe+ ion beams of the same energy were implanted into films of L(+)-cysteine hydrochloride monohydrate. FTIR spectroscopy of the implanted samples proved that some of the original molecules were展开更多
The crystalline syndiotactic 1,2-polybutadiene was synthesized with a catalytic system consisting of iron acetylacetonate , triisobutylaluminum and diethyl phosphite (DEP), and its single crystal structure was studied...The crystalline syndiotactic 1,2-polybutadiene was synthesized with a catalytic system consisting of iron acetylacetonate , triisobutylaluminum and diethyl phosphite (DEP), and its single crystal structure was studied by transmission electron microscopy (TEM) and electron diffraction (ED) techniques. The polymer with melting point 179 ℃ was found to have 89.3% 1,2 content and 86.5% sydiotacticity based on 13C NMR measurement. The single crystals of the polymer were achieved by melt crystallization of the solution cast thin films at 150 ℃ for 2 h. Bright field electron micrograph shows that the single crystal exhibits a hexagonal prism shape with its long axis along the crystallographic b-axis, as revealed by the corresponding ED pattern. The strong (hk 0) reflections of the ED pattern indicate that the single crystal possesses a very good crystallographic orientation with the c-axis perpendicular to the film plane. According to the orthorhombic packing of the planar zigzag chains, all of the diffraction points can be indexed, and the unit cell parameters calculated from the ED result are a=1.102 nm and b=0.664 nm. In order to obtain the unit cell parameter c, α highly oriented thin film of the polymer was prepared with a special melt drawn technique. The TEM bright field image indicates that the melt drawn thin films contain highly oriented lamellae with their growing direction perpendicular to the drawing direction. The corresponding ED pattern reveals the molecular chains are highly oriented, with the c-axis parallel to the drawing direction. The unit cell parameter c is 0.513 nm, as calculated from the (hk 0) reflections.展开更多
Single crystals of two liquid crystal compounds, 5-{[4＇-（（（pentyl）oxy）-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO5） and 5-{[（4＇-nonyloxy-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO9）, have been prepared b...Single crystals of two liquid crystal compounds, 5-{[4＇-（（（pentyl）oxy）-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO5） and 5-{[（4＇-nonyloxy-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO9）, have been prepared by solution growth technique. The morphologies and structures of A3EO5 and A3EO9 crystals were investigated by wide angle X-ray diffraction （WXRD）, atom force microscope （AFM） and transmission electron microscope （TEM）. In contrast to the same series of compounds which have a longer alkyl tail, 5-{[（4＇-heptoxy-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO7）, 5-{[（4＇-heptoxy-4-biphenylyl）oxy]carbonyl}-1-pentyne （A3E＇O7） and A3EO9, A3EO5 shows strikingly different crystalline behavior. The former three compounds have only one crystal form, whereas A3EO5 exhibits polymorphism. Specifically, A3EO5 crystals grown from toluene solution show two crys- tal forms. The first one is crystal I which adopts a monoclinic P112/m space group with unit cell parameters of a= 5.79A, b=8.34A, c=43.92/k, y=96°, and the other one is crystal II which adopts a monoclinic P112 space group with unit cell parameters of a=5.55A, b=7.38A, c=31.75 ]k, y=94°. When using dioxane as the solvent to grow A3EO5 crystal, we can selectively obtain crystal Ⅰ. A3EO5 melt-grown crystals also have two crystal forms which derive from crystal I and crystal Ⅱ, respectively. The different crystalline behavior of the compounds should correlate with their different electron dipole moment resulting from the different length of alkyl tail.展开更多
Niduenes A-F(1-6),six novel sesterterpenoids with unprecedented 5/5/5/5/6 pentacyclic ring skeleton were isolated from endophytic fungus Aspergillus nidulans.Compounds 1 and 2 represent the first examples of aromatic ...Niduenes A-F(1-6),six novel sesterterpenoids with unprecedented 5/5/5/5/6 pentacyclic ring skeleton were isolated from endophytic fungus Aspergillus nidulans.Compounds 1 and 2 represent the first examples of aromatic pentacyclic sesterterpenoids.Their structures and configurations were elucidated by spectroscopic data and single-crystal X-ray diffraction analyses.Compound 4 demonstrated potent resensitization of SW620/AD300 cells to paclitaxel(PTX).Rhodamine 123 accumulation assay and docking analysis further support that 4 inhibitory the efflux function of P-glycoprotein(P-gp).展开更多
Monosescinol A(1),the first example of sesquiterpene–polycyclic polyprenylated acylphloroglucinol(PPAP)adduct,which represented a new subclass of PPAP-type natural products,along with two new congeners with normal sp...Monosescinol A(1),the first example of sesquiterpene–polycyclic polyprenylated acylphloroglucinol(PPAP)adduct,which represented a new subclass of PPAP-type natural products,along with two new congeners with normal spiro 6/6/5 tricyclic architecture,were isolated from Hypericum longistylum.Monosescinol A possessed an unprecedented 6/5/5/6/6 pentacyclic carbon skeleton that might be assembled from the 6/6/5 carbon skeleton,via the splitting decomposition of C-3/C-14,and the attack from the C-3 in the PPAP core to C-28 in sesquiterpene section.In addition,we have firstly confirmed that 24R configuration was existed in sec–Bu containing PPAPs by single crystal diffraction data analysis of monosescinol B(2),that might provide an enlightenment in the configurational determination of sec–Bu containing PPAPs.Significantly,further pharmacological research has found that compound 1 exhibited remarkable pharmacological effects against acute myeloid leukemia(AML)cell lines,with direct inhibition of mitochondrial complex V and an increase in mitochondrial membrane potential,and led to an induction of oxidative stress,endogenous inflammation,and apoptosis of AML cells.展开更多
Nine undescribed dihydro-β-agarofuran sesquiterpenoid derivatives(1—9),along with a known analogue(10),were obtained from the leaves of Tripterygium wilfordii.Their gross structures were determined via extensive spe...Nine undescribed dihydro-β-agarofuran sesquiterpenoid derivatives(1—9),along with a known analogue(10),were obtained from the leaves of Tripterygium wilfordii.Their gross structures were determined via extensive spectroscopic data,and the absolute configurations were elucidated by means of single-crystal X-ray diffraction analysis and electron circular dichroism(ECD)techniques,which include ECD exciton chirality,octant rule of saturated cyclohexanone and comparison between the experimental and calculated ECD spectra.All the isolated compounds were tested for their neuroprotective activities against H2O2-induced cell injury in human neuroblastoma SH-SY5Y cells.Compounds 5 and 6 improved cell viability by 16.15%and 15.12%compared with the H2O2 treated group at 25μmol·L^(-1),respectively.展开更多
In this study,we explored the deformation mechanisms of Mg single crystals using a combination of scanning electron microscopy and electron backscattered diffraction in conjunction with a dedicated four-point bending ...In this study,we explored the deformation mechanisms of Mg single crystals using a combination of scanning electron microscopy and electron backscattered diffraction in conjunction with a dedicated four-point bending tester.We prepared two single-crystal samples,oriented along the<1120>and<1010>directions,to assess the mechanisms of deformation when the initial basal slip was suppressed.In the<1120>sample,the primary{1012}twin(T1)was confirmed along the<1120>direction of the sample on the compression side with an increase in bending stress.In the<1010>sample,T1 and the secondary twin(T2)were confirmed to be along the<1120>direction,with an orientation of±60°with respect to the bending stress direction,and their direction matched with(0001)in T1 and T2.This result implies that crystallographically,the basal slip occurs readily.In addition,the<1010>sample showed the double twin in T1 on the compression side and the tertiary twin along the<1010>direction on the tension side.These results demonstrated that the maximum bending stress and displacement changed significantly under the bend loading because the deformation mechanisms were different for these single crystals.Therefore,the correlation between bending behavior and twin orientation was determined,which would be helpful for optimizing the bending properties of Mg-based materials.展开更多
Talaroclauxins A and B(1 and 2),two novel duclauxin hybrids,were obtained from Talaromyces stipitatus,along with three new(3-5)and one known analogue(6).Their structures were determined by NMR spectroscopy,HRESIMS,sin...Talaroclauxins A and B(1 and 2),two novel duclauxin hybrids,were obtained from Talaromyces stipitatus,along with three new(3-5)and one known analogue(6).Their structures were determined by NMR spectroscopy,HRESIMS,single-crystal X-ray diffraction,and quantum chemical calculations.Compound 1 is the first example of duclauxin-ergosterol hybrid featuring an unprecedented dodecacyclic ring system formed via a[4+2]cycloaddition,while compound 2,bearing an unusual 6/6/6/5/6/6/6/6 ring system,is a new member of the rare duclauxin-polyketide hybrid class of natural products.Plausible biosynthetic pathways for 1-6 are proposed.Compound 5 displayed moderate neuroprotective effects in glutamate sodium-induced SH-SY5Y cells.展开更多
基金This work was supported by the National Natural Science Foundation of China (Grant No.19975060)the Scientific Foundation of "95" Fundamental Research from the Chinese Academy of Sciences (Grant No. KJ952-S1-424).
文摘Fe+ ion beams with the energy of 110 keV were implanted into films of L(+)-cysteine (HSCH2CH(NH2)COOH). One of the single crystals grown in hydrochloric acid solution with the implanted samples through slow evaporation was structurally characterized by the X-ray crystallography. The crystal is monoclinic, space group C2, with a = 1.8534(4) nm, b=0.5234(1) nm, c = 0.7212(1) nm, β=103.722°, V = 0.67965(3) nm3, Z = 4, F(000) = 144.0, Dclac = 1.763 g·cm-3, μ (MoKa) = 1.06 mm-1, T = 293(2) K.R = 0.0379, wR = 0.0835 for 660 observed reflections (I】2σ(I)). The structural formula of the crystal compound is (CH2CH(NH2)NO2)ClFe (Mr = 180.38u). Products of heavy ion beam irradiation were purified and it was directly confirmed that the implanted Fe+ ions had been deposited in the novel molecules. The same doses of Fe+ ion beams of the same energy were implanted into films of L(+)-cysteine hydrochloride monohydrate. FTIR spectroscopy of the implanted samples proved that some of the original molecules were
文摘The crystalline syndiotactic 1,2-polybutadiene was synthesized with a catalytic system consisting of iron acetylacetonate , triisobutylaluminum and diethyl phosphite (DEP), and its single crystal structure was studied by transmission electron microscopy (TEM) and electron diffraction (ED) techniques. The polymer with melting point 179 ℃ was found to have 89.3% 1,2 content and 86.5% sydiotacticity based on 13C NMR measurement. The single crystals of the polymer were achieved by melt crystallization of the solution cast thin films at 150 ℃ for 2 h. Bright field electron micrograph shows that the single crystal exhibits a hexagonal prism shape with its long axis along the crystallographic b-axis, as revealed by the corresponding ED pattern. The strong (hk 0) reflections of the ED pattern indicate that the single crystal possesses a very good crystallographic orientation with the c-axis perpendicular to the film plane. According to the orthorhombic packing of the planar zigzag chains, all of the diffraction points can be indexed, and the unit cell parameters calculated from the ED result are a=1.102 nm and b=0.664 nm. In order to obtain the unit cell parameter c, α highly oriented thin film of the polymer was prepared with a special melt drawn technique. The TEM bright field image indicates that the melt drawn thin films contain highly oriented lamellae with their growing direction perpendicular to the drawing direction. The corresponding ED pattern reveals the molecular chains are highly oriented, with the c-axis parallel to the drawing direction. The unit cell parameter c is 0.513 nm, as calculated from the (hk 0) reflections.
文摘Single crystals of two liquid crystal compounds, 5-{[4＇-（（（pentyl）oxy）-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO5） and 5-{[（4＇-nonyloxy-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO9）, have been prepared by solution growth technique. The morphologies and structures of A3EO5 and A3EO9 crystals were investigated by wide angle X-ray diffraction （WXRD）, atom force microscope （AFM） and transmission electron microscope （TEM）. In contrast to the same series of compounds which have a longer alkyl tail, 5-{[（4＇-heptoxy-4-biphenylyl）carbonyl]oxy}-1-pentyne （A3EO7）, 5-{[（4＇-heptoxy-4-biphenylyl）oxy]carbonyl}-1-pentyne （A3E＇O7） and A3EO9, A3EO5 shows strikingly different crystalline behavior. The former three compounds have only one crystal form, whereas A3EO5 exhibits polymorphism. Specifically, A3EO5 crystals grown from toluene solution show two crys- tal forms. The first one is crystal I which adopts a monoclinic P112/m space group with unit cell parameters of a= 5.79A, b=8.34A, c=43.92/k, y=96°, and the other one is crystal II which adopts a monoclinic P112 space group with unit cell parameters of a=5.55A, b=7.38A, c=31.75 ]k, y=94°. When using dioxane as the solvent to grow A3EO5 crystal, we can selectively obtain crystal Ⅰ. A3EO5 melt-grown crystals also have two crystal forms which derive from crystal I and crystal Ⅱ, respectively. The different crystalline behavior of the compounds should correlate with their different electron dipole moment resulting from the different length of alkyl tail.
基金financially supported by the National Key Research and Development Program of China(No.2021YFA0910500)the National Natural Science Foundation of China(Nos.U22A20380,82104028,82173706 and 82373755)+2 种基金Innovative Research Groups of the National Natural Science Foundation of China(No.81721005)the Science and Technology Major Project of Hubei Province(No.2021ACA012)the Fundamental Research Funds for the Central Universities,HUST(No.2021JYCXJJ058)。
文摘Niduenes A-F(1-6),six novel sesterterpenoids with unprecedented 5/5/5/5/6 pentacyclic ring skeleton were isolated from endophytic fungus Aspergillus nidulans.Compounds 1 and 2 represent the first examples of aromatic pentacyclic sesterterpenoids.Their structures and configurations were elucidated by spectroscopic data and single-crystal X-ray diffraction analyses.Compound 4 demonstrated potent resensitization of SW620/AD300 cells to paclitaxel(PTX).Rhodamine 123 accumulation assay and docking analysis further support that 4 inhibitory the efflux function of P-glycoprotein(P-gp).
基金supported financially by the National Natural Science Foundation for Distinguished Young Scholars(No.81725021)the National Natural Science Foundation of China(Nos.82003633 and 82104043)the National Natural Science Foundation of Hubei Province(No.2023AFB791)。
文摘Monosescinol A(1),the first example of sesquiterpene–polycyclic polyprenylated acylphloroglucinol(PPAP)adduct,which represented a new subclass of PPAP-type natural products,along with two new congeners with normal spiro 6/6/5 tricyclic architecture,were isolated from Hypericum longistylum.Monosescinol A possessed an unprecedented 6/5/5/6/6 pentacyclic carbon skeleton that might be assembled from the 6/6/5 carbon skeleton,via the splitting decomposition of C-3/C-14,and the attack from the C-3 in the PPAP core to C-28 in sesquiterpene section.In addition,we have firstly confirmed that 24R configuration was existed in sec–Bu containing PPAPs by single crystal diffraction data analysis of monosescinol B(2),that might provide an enlightenment in the configurational determination of sec–Bu containing PPAPs.Significantly,further pharmacological research has found that compound 1 exhibited remarkable pharmacological effects against acute myeloid leukemia(AML)cell lines,with direct inhibition of mitochondrial complex V and an increase in mitochondrial membrane potential,and led to an induction of oxidative stress,endogenous inflammation,and apoptosis of AML cells.
基金This work was supported by Career Development Support Plan for Young and Middle-aged Teachers in Shenyang Pharmaceutical University(ZQN2018006)the Project of Innovation Team Foundation(LT2015027).
文摘Nine undescribed dihydro-β-agarofuran sesquiterpenoid derivatives(1—9),along with a known analogue(10),were obtained from the leaves of Tripterygium wilfordii.Their gross structures were determined via extensive spectroscopic data,and the absolute configurations were elucidated by means of single-crystal X-ray diffraction analysis and electron circular dichroism(ECD)techniques,which include ECD exciton chirality,octant rule of saturated cyclohexanone and comparison between the experimental and calculated ECD spectra.All the isolated compounds were tested for their neuroprotective activities against H2O2-induced cell injury in human neuroblastoma SH-SY5Y cells.Compounds 5 and 6 improved cell viability by 16.15%and 15.12%compared with the H2O2 treated group at 25μmol·L^(-1),respectively.
基金supported by The AMADA FOUNDATION[grant number AF-2022030-B3]JSPS KAKENHI[grant numbers JP16K05961 and JP19K04065]。
文摘In this study,we explored the deformation mechanisms of Mg single crystals using a combination of scanning electron microscopy and electron backscattered diffraction in conjunction with a dedicated four-point bending tester.We prepared two single-crystal samples,oriented along the<1120>and<1010>directions,to assess the mechanisms of deformation when the initial basal slip was suppressed.In the<1120>sample,the primary{1012}twin(T1)was confirmed along the<1120>direction of the sample on the compression side with an increase in bending stress.In the<1010>sample,T1 and the secondary twin(T2)were confirmed to be along the<1120>direction,with an orientation of±60°with respect to the bending stress direction,and their direction matched with(0001)in T1 and T2.This result implies that crystallographically,the basal slip occurs readily.In addition,the<1010>sample showed the double twin in T1 on the compression side and the tertiary twin along the<1010>direction on the tension side.These results demonstrated that the maximum bending stress and displacement changed significantly under the bend loading because the deformation mechanisms were different for these single crystals.Therefore,the correlation between bending behavior and twin orientation was determined,which would be helpful for optimizing the bending properties of Mg-based materials.
基金the Program for Changjiang Scholars of Ministry of Education of the People's Republic of China(No.T2016088)the National Natural Science Foundation for Distinguished Young Scholars(No.81725021)+6 种基金the National Natural Science Foundation for Excellent Young Scholars(No.81922065)Innovative Research Groups of the National Natural Science Foundation of China(No.81721005)the National Natural Science Foundation of China(No.82173706)the Science and Technology Major Project of Hubei Province(No.2021ACA012)the Research and Development Program of Hubei Province(No.2020BCA058)the Academic Frontier Youth Team of HUST(No.2017QYTD19)the Integrated Innovative Team for Major Human Diseases Program of Tongji Medical College(HUST).
文摘Talaroclauxins A and B(1 and 2),two novel duclauxin hybrids,were obtained from Talaromyces stipitatus,along with three new(3-5)and one known analogue(6).Their structures were determined by NMR spectroscopy,HRESIMS,single-crystal X-ray diffraction,and quantum chemical calculations.Compound 1 is the first example of duclauxin-ergosterol hybrid featuring an unprecedented dodecacyclic ring system formed via a[4+2]cycloaddition,while compound 2,bearing an unusual 6/6/6/5/6/6/6/6 ring system,is a new member of the rare duclauxin-polyketide hybrid class of natural products.Plausible biosynthetic pathways for 1-6 are proposed.Compound 5 displayed moderate neuroprotective effects in glutamate sodium-induced SH-SY5Y cells.
