Analytical solution of crystal diffraction intensity

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.

Comparison between Double Crystals X-ray Diffraction and Micro-Raman Measurement on Composition Determination of High Ge Content Si_(1-x)Ge_(x) Layer Epitaxied on Si Substrate

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.

Synthesis and Crystal Structures of Schiff Bases Bearing Ferrocenylphenyl Groups

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.

Crystal Type Iof Azilsartan Polymorphs: Preparation and Analysis

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.

Solvent-free Synthesis and Crystal Structure of 2,2＇-Dialkyl Bis(3-methyl-6,7- dihydrobenzofuran-4(5H)-one) Derivatives

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））.

Synthesis,Crystal Structure and Cytotoxic Activities of 1-(Prop-2-yn-1-yl)-7,8-dihydro-1H-benzo[d][1,3]-thiazine-2,5(4H,6H)-dione Derivatives

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））.

Synthesis, Characterization and Crystal Structure of Bis[1 -meth oxy-2,2,2-tris-（pyrazol-1 -yl-KN2）ethane]-coppe r（Ⅱ） Bis-perchlorate

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.

Asymmetric dynamic phase holographic grating in nematic liquid crystal

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.

Syntheses and Crystal Structures of Pyridyl Substituted Dibenzo[b,e]-[1,4]diazepin-1-one Derivatives

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.

Thiocyanate-controlled Copper(Ⅱ)-L-arginine Complex:Synthesis,Crystal Structure and Characterization

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.

Synthesis, characterization, spectroscopic and crystallographic investigation of Cobalt(Ⅲ) schiff base complex with two perpendicular diamine coumarin ligands

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.

On the Mechanism of Condensation between 5-Amino-4, 6-dichloro- 2-methylpyrimidine and 1-Acetyl-2-imidazolin-2-one

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.

A Reflectron Time-of-Flight Mass Spectrometer with a Nano-Electrospray Ionization Source for Study of Metal Cluster Compounds

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.

New Iboga‑Type Indole Alkaloids from Tabernaemontana divaricata

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.

Synthesis and Properties of a Heteronuclear Ag(Ⅰ)/Ni(Ⅱ) Complex

A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crystal X-ray diffraction. It is indicated that the complex has a 3D architecture through the silver-silver interactions and the bridging eyano groups. This complex displays interesting luminescent properties caused by argentophilieity at room temperature in solid state.

Synthesis and Structure of Dibenzoyl-bissemicarbazone Neodymium(Ⅲ) Perchlorate

A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.

SAW diffraction field generated by source with finite aperture piezoelectric crystal surfaces

So far, the diffracted SAW field generated by an IDT with finite aperture on piezoelectric crystal surfaces is usually analyzed phenomenologically with the angular spectrum theory. A major approximation of this theory is to ignore the vector nature of the field by assuming that the wave field can be represented by a scalar as in optics. In this paper, a rigorous vector field theory of the surface excitation of elastic wave field in piezoelectric crystal developed by the authors is used to evaluate the SAW diffraction field adepately and precisely. As an example, numerical results for YZ-LiNbO3 are presented and compared with those obtained form the angular spectrum theory.

The determination of the crystal struoure of tetra-potassium uranyl tricarbonate by powder X-ray diffraction method

A uranyl compound, K_4UO_2(CO_3)_3 has been characterized by powder X-ray diffraction method. M. W.=606.46, monoclinic, C2/c (No. 15), a=1.0240(7), b=0.9198(4), c=1.2222(12)nm, β=95.12(4)°,V=1.1466(5)nm^3, Z=4, D_m=3.468g/cm^3, D_c=3.513g/cm~, λ(Cu Kα_1)=O.1540598nm, T=298K. The structure was solved by heavy atom method and Fourier synthesis, and refined by full- matrix least-squares method to R=0.1185 for 275 reflections. The uranium (Ⅵ) atom is in an eight-coordinate distorted hexagonal-bipyramidal environment with creasy fan shape. The linear uranyl group approaches to perpendicular to the equatorial plane in which three carbonate groups are chelated. U(Ⅵ) has two linear oxygen atoms closer to it (U-O=0.1767 (5) nm) than six other neighbours (U-O ranging from 0.2516 to 0.2568nm). The distances between carbon atoms and uncoordinated oxygen atoms are 0.122 (1) and 0.123(1) nm, which are distinctly different from those between carbon and coordinated oxygen atoms (mean 0.134(6) nm). This fact reveals the non-eq- uivalence of one oxygen atom to the other two in each carbonate. In K_4UO_2(CO_3)_3, the O-O dis- tance for the adjacent carbonate groups is 0.2794(4)nm approaching to the sum of Van der Waals radii of two oxygen atoms. The K-O distances vary between 0.2667 and 0.3131nm, and each anion is immediately surrounded by six potassium ions, only four of which can be considered to belong to the same structural formula unit, and they are symmetrically located above and below the equatorial plane.

Growth and characterizations of CdGeAs2single crystal by descending crucible with rotation method

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.

Synthesis, crystal structure and thermal analysis of a new stilbazolium salt crystal

A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium tosylate （DAST） with the benzene sulfonate replacing p-toluenesulfonate. Single crystal XRD demonstrated that the crystal structure of DASBS. H20 was triclinic. The thermal analysis of this new crystal was also conducted, and the melting point was obtained to be 232℃.