Plasma density and temperature can be diagnosed by x-ray line emission measurement with crystal,and bent crystals such as von Hamos and Hall structures are proposed to improve the diffraction brightness.In this study,...Plasma density and temperature can be diagnosed by x-ray line emission measurement with crystal,and bent crystals such as von Hamos and Hall structures are proposed to improve the diffraction brightness.In this study,a straightforward solution for the focusing schemes of flat and bent crystals is provided.Simulations with XOP code are performed to validate the analytical model,and good agreements are achieved.The von Hamos or multi-cone crystal can lead to several hundred times intensity enhancements for a 200μm plasma source.This model benefits the applications of the focusing bent crystals.展开更多
The lattice parameter,measured with sufficient accuracy,can be utilized to evaluate the quality of single crystals and to determine the equation of state for materials.We propose an iterative method for obtaining more...The lattice parameter,measured with sufficient accuracy,can be utilized to evaluate the quality of single crystals and to determine the equation of state for materials.We propose an iterative method for obtaining more precise lattice parameters using the interaction points for the pseudo-Kossel pattern obtained from laser-induced X-ray diffraction(XRD).This method has been validated by the analysis of an XRD experiment conducted on iron single crystals.Furthermore,the method was used to calculate the compression ratio and rotated angle of an LiF sample under high pressure loading.This technique provides a robust tool for in-situ characterization of structural changes in single crystals under extreme conditions.It has significant implications for studying the equation of state and phase transitions.展开更多
It is important to acquire the composition of Si1-xGex layer, especially that with high Ge content, epitaxied on Si substrate. Two nondestructive examination methods, double crystals X-ray diffraction （DCXRD） and mi...It is important to acquire the composition of Si1-xGex layer, especially that with high Ge content, epitaxied on Si substrate. Two nondestructive examination methods, double crystals X-ray diffraction （DCXRD） and micro-Raman measurement, were introduced comparatively to determine x value in Si1-xGex layer, which show that while the two methods are consistent with each other when x is low, the results obtained from double crystals X-ray diffraction are not credible due to the large strain relaxation occurring in Si1-xGex layers when Ge content is higher than about 20%. Micro-Raman measurement is more appropriate for determining high Ge content than DCXRD.展开更多
The Schiff bases bearing ferrocenylphenyl and diferrocenylphenyl groups were synthesized by the reactions of m-ferrocenylaniline with salicylaldehyde or 1, 4-bis (2′-formyl- phenyl)-1, 4-dioxabutane. The title compou...The Schiff bases bearing ferrocenylphenyl and diferrocenylphenyl groups were synthesized by the reactions of m-ferrocenylaniline with salicylaldehyde or 1, 4-bis (2′-formyl- phenyl)-1, 4-dioxabutane. The title compounds were characterized by elemental analysis, IR, 1H NMR and X-ray structural determination.展开更多
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
By the method of descending crucible with rotation, crack-free CdGeAs2single crystals of U15 mm 950 mm were grown in a furnace with three independen heating zones after optimizing the temperature field, and the descen...By the method of descending crucible with rotation, crack-free CdGeAs2single crystals of U15 mm 950 mm were grown in a furnace with three independen heating zones after optimizing the temperature field, and the descending and rotational speed to meet the need of CdGeAs2crystal growth. The properties of as-grown crysta were characterized by a variety of techniques. The results of X-ray diffraction（XRD） show that there are two cleavage faces, which are（110） and（101）. The peaks are in high intensity and good symmetry, which demonstrates that the crystal is integral in structure and well crystallized. The energy-dispersive spectrometry results indicate that the wafer of the CdGeAs2crystal is closer to the stoichiometry The IR transmittance of the wafer is ＊48.6 % at 5.5 lm, and the maximum value is up to 51.6 % in the range of2.3–18.0 lm. Etch pits of（001） face are observed and the density of the etch pits is evaluated to be 1 9 105cm-2.展开更多
A series of 2,2＇-dialkyl bis（3-methyl-6,7-dihydrobenzofuran-4（5H）-one） derivatives was prepared through H2SO4·SiO2 catalyzed condensation reaction under solvent-free conditions as potential anti-tumor agents...A series of 2,2＇-dialkyl bis（3-methyl-6,7-dihydrobenzofuran-4（5H）-one） derivatives was prepared through H2SO4·SiO2 catalyzed condensation reaction under solvent-free conditions as potential anti-tumor agents. All of them were characterized by ESI-MS, IR and NMR spectra. Meanwhile, the single crystal of the target compound （4b）, C24H28O4, was also obtained and determined by X-ray crystallography. Crystal data： triclinic system, space group P , a = 8.463（10）, b = 9.612（11）, c = 13.828（15） , α = 74.29（5）, β = 80.93（5）, γ = 69.90（3）°, V = 1014（2） 3, Z = 2, F（000） = 408, Dc = 1.246 g/cm3, μ = 0.084 mm？1, R = 0.0883 and wR = 0.2440 for 4616 independent reflections （Rint = 0.1200） and 3490 observed ones （I 〉 2σ（I））.展开更多
The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferre...The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferred into cytotoxic triazoles by alkylation and ＂click＂ synthesis in satisfactory yields of 87%^95%. Their structures were characterized by IR, H-RESI-MS and NMR analysis. Meanwhile, the crystal of Ⅲ was obtained and determined by X-ray single-crystal diffraction. Crystal data： orthorhombic system, space group P212121, a = 5.189（4）, b = 8.661（6）, c = 23.498（17） A, V = 1056.2（13） A^3, Z = 4, F（000） = 464, Dc = 1.392 g/cm^3, μ =0.284 mm^-1, R = 0.0637 and wR = 0.1668 for 8182 independent reflections（R（int） = 0.1580） and 2166 observed ones（I 〉 2σ（I））.展开更多
Bis[1-methoxy-2,2,2-tris-（pyrazol-l-yl-KN2）ethane]-copper（Ⅱ） bis-perchlorate （2） was synthesized by reacting of pyrazole based tripodal scorpionate ligand 1-methoxy-2,2,2-tris（pyrazol-1-yl）ethane （1） with c...Bis[1-methoxy-2,2,2-tris-（pyrazol-l-yl-KN2）ethane]-copper（Ⅱ） bis-perchlorate （2） was synthesized by reacting of pyrazole based tripodal scorpionate ligand 1-methoxy-2,2,2-tris（pyrazol-1-yl）ethane （1） with copper（Ⅱ） perchlorate hexahydrate in methanol, acetonitrile and water mixture as solvent. Slow evaporation of the filtered reaction mixture in air produced blue color block crystals suitable for single crystal X-ray diffraction study of the title complex. Compound 2 crystallizes in the monoclinic space group P21/n with unit cell parameters, α = 8.1269（1） ,A, b = 21.8348（2）A, c = 9.1522（1） A, a = γ= 90° , β = 99.7611 （4）°. The structure of the compound was characterized by IR Spectroscopy, elemental analysis and single crystal X-ray diffraction analysis.展开更多
Crystal structures and thermal expansion properties of Yb2-xFexMo3O12（x=0.0,0.6,1.0,1.1,1.4） solid solutions have been studied by X-ray powder diffraction（XRPD） at different temperatures.Rietveld analysis of the X...Crystal structures and thermal expansion properties of Yb2-xFexMo3O12（x=0.0,0.6,1.0,1.1,1.4） solid solutions have been studied by X-ray powder diffraction（XRPD） at different temperatures.Rietveld analysis of the XRPD data shows that Yb2-xFexMo3O12 solid solutions adopt orthorhombic structure and have variable thermal expansion coefficients controlled by the ratio of Yb^3＋ to Fe^3＋.Yb2Mo3O12 shows anisotropic negative thermal expansion property,induced by the reductions in average Yb-O-Mo angle and average apparent Mo2-O bond length with increasing temperatures.As more Yb^3＋ substituted by Fe^3＋,the linear thermal expansion coefficients of Yb2-xFexMo3O12 increase from negative to positive.A near-zero thermal expansion coefficient of 0.55×10^-6K^-1 for Yb0.6Fe1.4Mo3O12 is observed in the temperature range of 573-873 K.展开更多
A new scheme for recording a dynamic phase grating with an asymmetric profile in C60-doped homeotropically aligned nematic liquid crystal（NLC） was presented.An oblique incidence beam was used to record the thin asym...A new scheme for recording a dynamic phase grating with an asymmetric profile in C60-doped homeotropically aligned nematic liquid crystal（NLC） was presented.An oblique incidence beam was used to record the thin asymmetric dynamic phase holographic grating.The diffraction efficiency we achieved is more than 40%,exceeding the theoretical limit for symmetric profile gratings.Both facts can be explained by assuming that a grating with an asymmetric saw-tooth profile is formed in the NLC.Finally,physical mechanism and mathematical model for characterizing the asymmetric phase holographic grating were presented,based on the photo-refractive-like（PR-like） effect.展开更多
Lanthanum malonate crystals were grown by single tube ionic diffusion through silica gel. The crystallinity of the grown crystals was analyzed by powder X-ray diffraction studies. Fourier transform infrared spectrosco...Lanthanum malonate crystals were grown by single tube ionic diffusion through silica gel. The crystallinity of the grown crystals was analyzed by powder X-ray diffraction studies. Fourier transform infrared spectroscopy （FTIR） and fourier transform （FT） Raman studies confirmed the presence of functional groups in the title compound. The optical band gap energy of the material was extracted from diffuse reflectance spectrum.展开更多
A new series of 11-pyridyl substituted dibenzo-diazepin-l-one derivatives 1 was synthesized by a two step cyclocondensation reaction. All the compounds were characterized by IR, MS, and H NMR. And crystals of la and l...A new series of 11-pyridyl substituted dibenzo-diazepin-l-one derivatives 1 was synthesized by a two step cyclocondensation reaction. All the compounds were characterized by IR, MS, and H NMR. And crystals of la and lb were obtained and determined by X-ray single-crystal diffraction. Crystal data of la： C48H52N607, monoclinic system, space group C2/c, a = 28.39（4）, b = 9.275（12）, c = 16.84（2） A, β = 104.98（3）°, V= 4284（10） A3, Z= 4, F（000） = 1752, Dc = 1.279 g/cm3, R = 0.0603, and wR = 0.1314. Crystal data of 1b： C24H21N30, monoclinic system, space group P21/c, a = 11.625（5）, b = 19.055（9）, c = 8.741（4） A, fl = 95.547（6）°, V= 1927.2（15） A3, Z = 4, F（000） = 776, Dc = 1.266 g/cm3, R = 0.0494, and wR = 0.1287.展开更多
A novel thiocyanate-controlled copper（Ⅱ）-L-arginine complex with the formula of Cu（Arg）（SCN）2（1,Arg：L-arginine） has been obtained from aqueous solution and structurally characterized by single-crystal X-ray ...A novel thiocyanate-controlled copper（Ⅱ）-L-arginine complex with the formula of Cu（Arg）（SCN）2（1,Arg：L-arginine） has been obtained from aqueous solution and structurally characterized by single-crystal X-ray diffraction method.Crystal data：orthorhombic,space group P212121,a = 6.0156（5）,b = 12.1905（11）,c = 18.4203（16） A°,V = 1350.8（2） A°3,Z = 4,μ = 1.933mm^（-1）,F（000） = 724,S = 1.084,the final R = 0.0410,wR = 0.0754 for 1893 observed reflections with I 〉 2σ（I）,and R = 0.0559,wR = 0.0820 for all reflections.In addition,elemental analysis,IR,TG-DTG and magnetism characterization are presented.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
Three new compounds, namely siderochelins D （2）, E （3）, and F （4）, together with one known siderochelin A （1）, were isolated from Amycolatopsis sp. LZ149 and elucidated by spectroscopic analyses includinglD- a...Three new compounds, namely siderochelins D （2）, E （3）, and F （4）, together with one known siderochelin A （1）, were isolated from Amycolatopsis sp. LZ149 and elucidated by spectroscopic analyses includinglD- and 2D-NMR and X-ray single crystal diffraction. Compounds 1-3 showed antibacterial activity against Mycobacterium smegmatis.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
An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-o...An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-of-fight mass spectrometer. Taking advantage of the nano-electrospray ionization source, polyvalent ions are usually produced in the ＂ionization＂ process and the obtained mass resolution of the equipment is over 8000. The molecular ion peaks of metal cluster compounds [Au20（PPhpy2）10Cl2]（SbF6）4, where PPhpy2=bis（2- pyridyl）phenylphosphine, and [AuaAg2（C）L6]（BF4）4, where L=2-（diphenylphosphino）-5- methylpyridine, are distinguished in the respective mass spectrum, accompanied by some fragment ion peaks. In addition, the mass-to-charge ratios of the parent ions are determi- nated. Preliminary results suggest that the device is a powerful tool for the study of metal cluster compounds. It turns out that the information obtained by the instrumentation serves as an essential supplement to single crystal X-ray diffraction for structure characterization of metal cluster compounds.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
Thin films of zinc-doped cadmium oxide with different Zn-doping levels（0, 2, 4, 6, and 8 at%） were deposited on glass substrates by employing an inexpensive, simplified spray technique using perfume atomizer at rela...Thin films of zinc-doped cadmium oxide with different Zn-doping levels（0, 2, 4, 6, and 8 at%） were deposited on glass substrates by employing an inexpensive, simplified spray technique using perfume atomizer at relatively low substrate temperature（375 °C） compared with the conventional spray method. The effect of Zn doping on the structural,morphological, optical, and electrical properties of the films was investigated. XRD patterns revealed that all the films are polycrystalline in nature having cubic crystal structure with a preferential orientation along the（1 1 1） plane irrespective of Zn-doping level. Zn-doping level causes a slight shift in the（1 1 1） diffraction peak toward higher angle. The crystallite size of the films was found to be in the range of 28–37 nm. The band gap value increases with Zn doping and reaches a maximum of 2.65 eV for the film coated with 6 at% Zn doping and for further higher doping concentration it decreases.Electrical studies indicate that Zn doping causes a reduction in the resistivity of the films and a minimum resistivity of15.69 X cm is observed for the film coated with 6 at% Zn.展开更多
基金Project supported by the National Natural Science Fundation of China(Grant Nos.11775203 and 12075219)the China Academy of Engineering Physics(CAEP)Foundation(Grant No.CX20210019).
文摘Plasma density and temperature can be diagnosed by x-ray line emission measurement with crystal,and bent crystals such as von Hamos and Hall structures are proposed to improve the diffraction brightness.In this study,a straightforward solution for the focusing schemes of flat and bent crystals is provided.Simulations with XOP code are performed to validate the analytical model,and good agreements are achieved.The von Hamos or multi-cone crystal can lead to several hundred times intensity enhancements for a 200μm plasma source.This model benefits the applications of the focusing bent crystals.
基金National Natural Science Foundation of China(12102410)Fund of National Key Laboratory of Shock Wave and Detonation Physics(JCKYS2022212005)。
文摘The lattice parameter,measured with sufficient accuracy,can be utilized to evaluate the quality of single crystals and to determine the equation of state for materials.We propose an iterative method for obtaining more precise lattice parameters using the interaction points for the pseudo-Kossel pattern obtained from laser-induced X-ray diffraction(XRD).This method has been validated by the analysis of an XRD experiment conducted on iron single crystals.Furthermore,the method was used to calculate the compression ratio and rotated angle of an LiF sample under high pressure loading.This technique provides a robust tool for in-situ characterization of structural changes in single crystals under extreme conditions.It has significant implications for studying the equation of state and phase transitions.
基金This work is supported by the National Natural Science Foundation of China （Grant Nos. 60336010 ＆ 90401001）973 Program （Grant No. TG 2000036603）the Student Innovation Program of CAS （No. 1731000500010）.
文摘It is important to acquire the composition of Si1-xGex layer, especially that with high Ge content, epitaxied on Si substrate. Two nondestructive examination methods, double crystals X-ray diffraction （DCXRD） and micro-Raman measurement, were introduced comparatively to determine x value in Si1-xGex layer, which show that while the two methods are consistent with each other when x is low, the results obtained from double crystals X-ray diffraction are not credible due to the large strain relaxation occurring in Si1-xGex layers when Ge content is higher than about 20%. Micro-Raman measurement is more appropriate for determining high Ge content than DCXRD.
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The Schiff bases bearing ferrocenylphenyl and diferrocenylphenyl groups were synthesized by the reactions of m-ferrocenylaniline with salicylaldehyde or 1, 4-bis (2′-formyl- phenyl)-1, 4-dioxabutane. The title compounds were characterized by elemental analysis, IR, 1H NMR and X-ray structural determination.
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.
基金financially supported by the National Natural Science Foundation Key Programs of China (No. 50732005)the National High Technology Research and Development Program of China (No. 2007AA03Z443)
文摘By the method of descending crucible with rotation, crack-free CdGeAs2single crystals of U15 mm 950 mm were grown in a furnace with three independen heating zones after optimizing the temperature field, and the descending and rotational speed to meet the need of CdGeAs2crystal growth. The properties of as-grown crysta were characterized by a variety of techniques. The results of X-ray diffraction（XRD） show that there are two cleavage faces, which are（110） and（101）. The peaks are in high intensity and good symmetry, which demonstrates that the crystal is integral in structure and well crystallized. The energy-dispersive spectrometry results indicate that the wafer of the CdGeAs2crystal is closer to the stoichiometry The IR transmittance of the wafer is ＊48.6 % at 5.5 lm, and the maximum value is up to 51.6 % in the range of2.3–18.0 lm. Etch pits of（001） face are observed and the density of the etch pits is evaluated to be 1 9 105cm-2.
基金supported by the National Natural Science Foundation of China(No.21602123)China Scholarship Council(No.201508420062)Youth Talent Development Foundation of China Three Gorges University
文摘A series of 2,2＇-dialkyl bis（3-methyl-6,7-dihydrobenzofuran-4（5H）-one） derivatives was prepared through H2SO4·SiO2 catalyzed condensation reaction under solvent-free conditions as potential anti-tumor agents. All of them were characterized by ESI-MS, IR and NMR spectra. Meanwhile, the single crystal of the target compound （4b）, C24H28O4, was also obtained and determined by X-ray crystallography. Crystal data： triclinic system, space group P , a = 8.463（10）, b = 9.612（11）, c = 13.828（15） , α = 74.29（5）, β = 80.93（5）, γ = 69.90（3）°, V = 1014（2） 3, Z = 2, F（000） = 408, Dc = 1.246 g/cm3, μ = 0.084 mm？1, R = 0.0883 and wR = 0.2440 for 4616 independent reflections （Rint = 0.1200） and 3490 observed ones （I 〉 2σ（I））.
基金Supported by the National Natural Science Foundation of China(No.21272136)Scientific Foundation from graduate school(2015CX131)Youth Talent Development Foundation of China Three Gorges University
文摘The important synthetic precursor（Ⅲ）, 1-（prop-2-yn-1-yl）-7,8-dihydro-1Hbenzo[d][1,3]thiazine-2,5（4H,6H）-dione（C（11）H（11）NO2S）, was prepared through a three-component reaction, which was further transferred into cytotoxic triazoles by alkylation and ＂click＂ synthesis in satisfactory yields of 87%^95%. Their structures were characterized by IR, H-RESI-MS and NMR analysis. Meanwhile, the crystal of Ⅲ was obtained and determined by X-ray single-crystal diffraction. Crystal data： orthorhombic system, space group P212121, a = 5.189（4）, b = 8.661（6）, c = 23.498（17） A, V = 1056.2（13） A^3, Z = 4, F（000） = 464, Dc = 1.392 g/cm^3, μ =0.284 mm^-1, R = 0.0637 and wR = 0.1668 for 8182 independent reflections（R（int） = 0.1580） and 2166 observed ones（I 〉 2σ（I））.
文摘Bis[1-methoxy-2,2,2-tris-（pyrazol-l-yl-KN2）ethane]-copper（Ⅱ） bis-perchlorate （2） was synthesized by reacting of pyrazole based tripodal scorpionate ligand 1-methoxy-2,2,2-tris（pyrazol-1-yl）ethane （1） with copper（Ⅱ） perchlorate hexahydrate in methanol, acetonitrile and water mixture as solvent. Slow evaporation of the filtered reaction mixture in air produced blue color block crystals suitable for single crystal X-ray diffraction study of the title complex. Compound 2 crystallizes in the monoclinic space group P21/n with unit cell parameters, α = 8.1269（1） ,A, b = 21.8348（2）A, c = 9.1522（1） A, a = γ= 90° , β = 99.7611 （4）°. The structure of the compound was characterized by IR Spectroscopy, elemental analysis and single crystal X-ray diffraction analysis.
基金supported by the National Natural Science Foundation of China (No. 21403129)the Project of Shandong Province Higher Educational Science and Technology Program (No.J13LD13 & J15LC09)"Hundred Talents Project" of the Chinese Academy of Sciences
文摘Crystal structures and thermal expansion properties of Yb2-xFexMo3O12（x=0.0,0.6,1.0,1.1,1.4） solid solutions have been studied by X-ray powder diffraction（XRPD） at different temperatures.Rietveld analysis of the XRPD data shows that Yb2-xFexMo3O12 solid solutions adopt orthorhombic structure and have variable thermal expansion coefficients controlled by the ratio of Yb^3＋ to Fe^3＋.Yb2Mo3O12 shows anisotropic negative thermal expansion property,induced by the reductions in average Yb-O-Mo angle and average apparent Mo2-O bond length with increasing temperatures.As more Yb^3＋ substituted by Fe^3＋,the linear thermal expansion coefficients of Yb2-xFexMo3O12 increase from negative to positive.A near-zero thermal expansion coefficient of 0.55×10^-6K^-1 for Yb0.6Fe1.4Mo3O12 is observed in the temperature range of 573-873 K.
基金Project supported by the Science and Technology Programs of the Educational Committee of Heilongjiang Province,China(Grant No.12541730)the National Natural Science Foundation of China(Grant No.61405057)
文摘A new scheme for recording a dynamic phase grating with an asymmetric profile in C60-doped homeotropically aligned nematic liquid crystal（NLC） was presented.An oblique incidence beam was used to record the thin asymmetric dynamic phase holographic grating.The diffraction efficiency we achieved is more than 40%,exceeding the theoretical limit for symmetric profile gratings.Both facts can be explained by assuming that a grating with an asymmetric saw-tooth profile is formed in the NLC.Finally,physical mechanism and mathematical model for characterizing the asymmetric phase holographic grating were presented,based on the photo-refractive-like（PR-like） effect.
文摘Lanthanum malonate crystals were grown by single tube ionic diffusion through silica gel. The crystallinity of the grown crystals was analyzed by powder X-ray diffraction studies. Fourier transform infrared spectroscopy （FTIR） and fourier transform （FT） Raman studies confirmed the presence of functional groups in the title compound. The optical band gap energy of the material was extracted from diffuse reflectance spectrum.
基金Supported by the National Natural Science Foundation of China for Young Scholars(No.21201087)Natural Science Foundation of Jiangsu Province(Nos.BK20131244)a start-up grant from Jiangsu University of Science and Technology
文摘A new series of 11-pyridyl substituted dibenzo-diazepin-l-one derivatives 1 was synthesized by a two step cyclocondensation reaction. All the compounds were characterized by IR, MS, and H NMR. And crystals of la and lb were obtained and determined by X-ray single-crystal diffraction. Crystal data of la： C48H52N607, monoclinic system, space group C2/c, a = 28.39（4）, b = 9.275（12）, c = 16.84（2） A, β = 104.98（3）°, V= 4284（10） A3, Z= 4, F（000） = 1752, Dc = 1.279 g/cm3, R = 0.0603, and wR = 0.1314. Crystal data of 1b： C24H21N30, monoclinic system, space group P21/c, a = 11.625（5）, b = 19.055（9）, c = 8.741（4） A, fl = 95.547（6）°, V= 1927.2（15） A3, Z = 4, F（000） = 776, Dc = 1.266 g/cm3, R = 0.0494, and wR = 0.1287.
基金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)
文摘A novel thiocyanate-controlled copper（Ⅱ）-L-arginine complex with the formula of Cu（Arg）（SCN）2（1,Arg：L-arginine） has been obtained from aqueous solution and structurally characterized by single-crystal X-ray diffraction method.Crystal data：orthorhombic,space group P212121,a = 6.0156（5）,b = 12.1905（11）,c = 18.4203（16） A°,V = 1350.8（2） A°3,Z = 4,μ = 1.933mm^（-1）,F（000） = 724,S = 1.084,the final R = 0.0410,wR = 0.0754 for 1893 observed reflections with I 〉 2σ（I）,and R = 0.0559,wR = 0.0820 for all reflections.In addition,elemental analysis,IR,TG-DTG and magnetism characterization are presented.
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.
基金supported by the 973 Program(Nos.2010CB833802 and 2012CB721005)the National Science Fund for Distinguished Young Scholars(No.30325044)the Natural Science Foundation of China(No.81373304)
文摘Three new compounds, namely siderochelins D （2）, E （3）, and F （4）, together with one known siderochelin A （1）, were isolated from Amycolatopsis sp. LZ149 and elucidated by spectroscopic analyses includinglD- and 2D-NMR and X-ray single crystal diffraction. Compounds 1-3 showed antibacterial activity against Mycobacterium smegmatis.
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An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-of-fight mass spectrometer. Taking advantage of the nano-electrospray ionization source, polyvalent ions are usually produced in the ＂ionization＂ process and the obtained mass resolution of the equipment is over 8000. The molecular ion peaks of metal cluster compounds [Au20（PPhpy2）10Cl2]（SbF6）4, where PPhpy2=bis（2- pyridyl）phenylphosphine, and [AuaAg2（C）L6]（BF4）4, where L=2-（diphenylphosphino）-5- methylpyridine, are distinguished in the respective mass spectrum, accompanied by some fragment ion peaks. In addition, the mass-to-charge ratios of the parent ions are determi- nated. Preliminary results suggest that the device is a powerful tool for the study of metal cluster compounds. It turns out that the information obtained by the instrumentation serves as an essential supplement to single crystal X-ray diffraction for structure characterization of metal cluster compounds.
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Thin films of zinc-doped cadmium oxide with different Zn-doping levels（0, 2, 4, 6, and 8 at%） were deposited on glass substrates by employing an inexpensive, simplified spray technique using perfume atomizer at relatively low substrate temperature（375 °C） compared with the conventional spray method. The effect of Zn doping on the structural,morphological, optical, and electrical properties of the films was investigated. XRD patterns revealed that all the films are polycrystalline in nature having cubic crystal structure with a preferential orientation along the（1 1 1） plane irrespective of Zn-doping level. Zn-doping level causes a slight shift in the（1 1 1） diffraction peak toward higher angle. The crystallite size of the films was found to be in the range of 28–37 nm. The band gap value increases with Zn doping and reaches a maximum of 2.65 eV for the film coated with 6 at% Zn doping and for further higher doping concentration it decreases.Electrical studies indicate that Zn doping causes a reduction in the resistivity of the films and a minimum resistivity of15.69 X cm is observed for the film coated with 6 at% Zn.
