Synthesis, reactivity, and properties of N-fused porphyrin rhenium(I) tricarbonyl complexes.

Science.gov (United States)

Toganoh, Motoki; Ikeda, Shinya; Furuta, Hiroyuki

2007-11-12

The thermal reactions of N-fused tetraarylporphyrins or N-confused tetraarylporphyrins with Re2(CO)10 gave the rhenium(I) tricarbonyl complexes bearing N-fused porphyrinato ligands (4) in moderate to good yields. The rhenium complexes 4 are characterized by mass, IR, 1H, and 13C NMR spectroscopy, and the structures of tetraphenylporphynato complex 4a and its nitro derivative 15 are determined by X-ray single crystal analysis. The rhenium complexes 4 show excellent stability against heat, light, acids, bases, and oxidants. The aromatic substitution reactions of 4 proceed without a loss of the center metal to give the nitro (15), formyl (16), benzoyl (17), and cyano derivatives (19), regioselectively. In the electrochemical measurements for 4, one reversible oxidation wave and two reversible reduction waves are observed. Their redox potentials imply narrow HOMO-LUMO band gaps of 4 and are consistent with their electronic absorption spectra, in which the absorption edges exceed 1000 nm. Theoretical study reveals that the HOMO and LUMO of the rhenium complexes are exclusively composed of the N-fused porphyrin skeleton. Protonation of 4 takes place at the 21-position regioselectively, reflecting the high coefficient of the C21 atom in the HOMO orbital. The skeletal rearrangement reaction from N-confused porphyrin Re(I) complex (8) to N-fused porphyrin Re(I) complex (4) is suggested from the mechanistic study as well as DFT calculations.

Spherical rhenium metal powder

International Nuclear Information System (INIS)

Leonhardt, T.; Moore, N.; Hamister, M.

2001-01-01

The development of a high-density, spherical rhenium powder (SReP) possessing excellent flow characteristics has enabled the use of advanced processing techniques for the manufacture of rhenium components. The techniques that were investigated were vacuum plasma spraying (VPS), direct-hot isostatic pressing (D-HIP), and various other traditional powder metallurgy processing methods of forming rhenium powder into near-net shaped components. The principal disadvantages of standard rhenium metal powder (RMP) for advanced consolidation applications include: poor flow characteristics; high oxygen content; and low and varying packing densities. SReP will lower costs, reduce processing times, and improve yields when manufacturing powder metallurgy rhenium components. The results of the powder characterization of spherical rhenium powder and the consolidation of the SReP are further discussed. (author)

The oxidation of ReCl_5 with oleum: synthesis and crystal structure of Re_2O_4Cl_4(SO_4)

International Nuclear Information System (INIS)

Betke, Ulf; Wickleder, Mathias S.

2012-01-01

The reaction of ReCl_5 and fuming sulfuric acid (25 % SO_3) in a sealed glass tube at 200 C led to red, needle shaped single crystals of Re_2O_4Cl_4(SO_4) (monoclinic, C2/c, a = 1501.8(2) pm, b = 1545.9(2) pm, c = 945.18(8) pm, β = 98.761(9) , Z = 8). In the crystal structure the [ReO_2] moieties are linked by [SO_4]"2"- tetrahedra to chains along the [101] direction. Each sulfate ion connects four rhenium atoms, additional two chloride ions complete the octahedral coordination sphere of each rhenium atom according to "1_∞[ReO_2_/_1Cl_2_/_1(SO_4)_2_/_4]. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Rhenium: a rare metal critical in modern transportation

Science.gov (United States)

John, David A.

2015-01-01

Rhenium is a silvery-white, metallic element with an extremely high melting point (3,180 degrees Celsius) and a heat-stable crystalline structure, making it exceptionally resistant to heat and wear. Since the late 1980s, rhenium has been critical for superalloys used in turbine blades and in catalysts used to produce lead-free gasoline.

The kinetics of anodic dissolution of rhenium in aqueous electrolyte solutions

International Nuclear Information System (INIS)

Atanasyants, A.G.; Kornienko, V.A.

1986-01-01

The kinetics of anodic rhenium dissolution was investigated by means of potentiodynamic and potentiostatic polarization curves recorded at temperature from 293 to 333 K in different media (NaOH, KOH, NaCl, NaBr, HCl, H 2 SO 4 ) using the rotating disc technique. It is shown that the kinetics of anodic rhenium dissolution and effective activation energy depend not only on the composition and pH value of the solutions but also on the structure of the dissolving rhenium surface. The investigation of the anodic behaviour of the rhenium monocrystal revealed the existence of anisotropy of the monocrystal electrochemical properties. The experimental results point to an important role of adsorption processes in anodic rhenium dissolution. Rhenium dissolution proceeds with formation of intermediate surface adsorption complexes between the metal and the components of the solution

Synthesis, characterization, and photophysical properties of a thiophene-functionalized bis(pyrazolyl) pyridine (BPP) tricarbonyl rhenium(I) complex.

Science.gov (United States)

Lytwak, Lauren A; Stanley, Julie M; Mejía, Michelle L; Holliday, Bradley J

2010-09-07

A bromo tricarbonyl rhenium(I) complex with a thiophene-functionalized bis(pyrazolyl) pyridine ligand (L), ReBr(L)(CO)(3) (1), has been synthesized and characterized by variable temperature and COSY 2-D (1)H NMR spectroscopy, single-crystal X-ray diffraction, and photophysical methods. Complex 1 is highly luminescent in both solution and solid-state, consistent with phosphorescence from an emissive (3)MLCT excited state with an additional contribution from a LC (3)(pi-->pi*) transition. The single-crystal X-ray diffraction structure of the title ligand is also reported.

Rhenium radioisotopes for therapeutic radiopharmaceutical development

International Nuclear Information System (INIS)

Knapp, F.F. Jr.; Beets, A.L.; Pinkert, J.; Kropp, J.; Lin, W.Y.; Wang, S.Y.

2001-01-01

Rhenium-186 and rhenium-188 represent two important radioisotopes which are of interest for a variety of therapeutic applications in oncology, nuclear medicine and interventional cardiology. Rhenium-186 is directly produced in a nuclear reactor and the 90 hour half-life allows distribution to distant sites. The relatively low specific activity of rhenium-186 produced in most reactors, however, permits use of phosphonates, but limits use for labelled peptides and antibodies. Rhenium-188 has a much shorter 16.9 hour half-life which makes distribution from direct reactor production difficult. However, rhenium-188 can be obtained carrier-free from a tungsten-188/rhenium-188 generator, which has a long useful shelf-life of several months which is cost-effective, especially for developing regions. In this paper we discuss the issues associated with the production of rhenium-186- and rhenium-188 and the development and use of various radiopharmaceuticals and devices labelled with these radioisotopes for bone pain palliation, endoradiotherapy of tumours by selective catheterization and tumour therapy using radiolabelled peptides and antibodies, radionuclide synovectomy and the new field of vascular radiation therapy. (author)

Rhenium Re

International Nuclear Information System (INIS)

Busev, A.I.; Tiptsova, V.G.; Ivanov, V.M.

1978-01-01

The basic methods for determining rhenium in various objects are presented. The gravimetric determination of rhenium is based on a quantitative precipitation of ReO 4 - ions with tetraphenylarsonium chloride. The determination is not hindered by tungstates and molybdates. The potentiometric determination of rhenium in alloys (>=0.5% Re) is based on perrhenate ion reduction to Re(4) with the titrated solution of the Cr(2) salt. Re(7) is titrated in a hot sulfuric acid solution in the presence of KJ. The relative error of the method is 1 to 3%. The photometric determination of rhenium is performed by the rhodamide method in molybdenum-and tungsten-containing alloys and catalytically, in rocks, after it has been separated in the form of sulfide. The extraction-photometric determination of rhenium is carried out with the aid of methyl violet (analysis of a stock with a high content of Mo, W, Ta, Nb, Ti ahd Zr) and thio-oxine (the determination of Re is hindered by Au, Pt, Pd, Ru, Os, Rh, Ir). Also described are methods for differential-spectrophotometric determination of Re with the aid of thiocarbamide, as well as with the aid of dimethylglyoxime in the presence of SnCl 2 in an acid medium when Re is determined in its alloys with niobium and hafnium. It takes 2 hours to analyze the Hf-Re alloy and 3 hours to analyze the Nb-Re alloy, the standard deviation being 0.005 at 30-50% Re and 0.027 to 0.019 at 10-50% Re

Synthesis, structural characterization and photoluminescence properties of rhenium(I) complexes based on bipyridine derivatives with carbazole moieties.

Science.gov (United States)

Li, Hong-Yan; Wu, Jing; Zhou, Xin-Hui; Kang, Ling-Chen; Li, Dong-Ping; Sui, Yan; Zhou, Yong-Hui; Zheng, You-Xuan; Zuo, Jing-Lin; You, Xiao-Zeng

2009-12-21

Three N,N-bidentate ligands, 5,5'-dibromo-2,2-bipyridine (L1) and two carbazole containing ligands of 5-bromo-5'-carbazolyl-2,2-bipyridine (L2), 5,5'-dicarbazolyl-2,2'-bipyridine (L3), and their corresponding rhenium Re(CO)3Cl(L) complexes (ReL1-ReL3) have been successfully synthesized and characterized by elemental analysis, 1H NMR and IR spectra. Their photophysical properties and thermal analysis, along with the X-ray crystal structure analysis of L3 and complexes ReL1 and ReL3 are also described. In CH2Cl2 solution at room temperature, all complexes display intense absorption bands at ca. 220-350 nm, which can be assigned to spin-allowed intraligand (pi-->pi*) transitions, and the low energy broad bands in the 360-480 nm region are attributed to the metal to ligand charge-transfer d(Re)-->pi* (diimine) (MLCT). The introduction of carbazole moieties improves the MLCT absorption and molar extinction coefficient of these complexes. Upon excitation at the peak maxima, all complexes show strong emissions around 620 nm, which are assigned to d(Re)-->pi* (diimine) MLCT phosphorescence. The photoluminescence lifetime decay of Re(I) complexes were measured and the quantum efficiencies of the rhenium(I) complexes were calculated by using air-equilibrated [Ru(bpy)3]2+ x 2 Cl- aqueous solution as standard (phi(std) = 0.028). The complexes with appended carbazole moieties exhibit enhanced luminescence performances relative to ReL1.

Electrodeposition of rhenium-tin nanowires

International Nuclear Information System (INIS)

Naor-Pomerantz, Adi; Eliaz, Noam; Gileadi, Eliezer

2011-01-01

Highlights: → Rhenium-tin nanowires were formed electrochemically, without using a template. → The nanowires consisted of a crystalline-Sn-core/amorphous-Re-shell structure. → The effects of bath composition and operating conditions were investigated. → A mechanism is suggested for the formation of the core/shell structure. → The nanowires may be attractive for a variety of applications. - Abstract: Rhenium (Re) is a refractory metal which exhibits an extraordinary combination of properties. Thus, nanowires and other nanostructures of Re-alloys may possess unique properties resulting from both Re chemistry and the nanometer scale, and become attractive for a variety of applications, such as in catalysis, photovoltaic cells, and microelectronics. Rhenium-tin coatings, consisting of nanowires with a core/shell structure, were electrodeposited on copper substrates under galvanostatic or potentiostatic conditions. The effects of bath composition and operating conditions were investigated, and the chemistry and structure of the coatings were studied by a variety of analytical tools. A Re-content as high as 77 at.% or a Faradaic efficiency as high as 46% were attained. Ranges of Sn-to-Re in the plating bath, applied current density and applied potential, within which the nanowires could be formed, were determined. A mechanism was suggested, according to which Sn nanowires were first grown on top of Sn micro-particles, and then the Sn nanowires reduced the perrhenate chemically, thus forming a core made of crystalline Sn-rich phase, and a shell made of amorphous Re-rich phase. The absence of mutual solubility of Re and Sn may be the driving force for this phase separation.

Electrochemical behaviour of rhenium-graphite electrode

International Nuclear Information System (INIS)

Varypaev, V.N.; Krasikov, V.L.

1980-01-01

Electrochemical behaviour of combination electrode from graphite with electrodeposited thin coating of electrolytic rhenium is studied. Solution of 0.5 m NaCl+0.04 m AlCl 3 served as an electrolite. Polarization galvanostatic curves of hydrogen evolution upon electrodes with conditional rhenium thickness of 3.5 and 0.35 μm, 35 and 3.5 nm are obtained. Possibility of preparation of rhenium-graphite cathode with extremely low rhenium consume, electro-chemical properties of which are simu-lar to purely rhenium cathode is shown. Such electrode is characterized with stable in time low cathode potential of hydrogen evolution in chloride electrolyte and during cathode polarization it is not affected by corrosion

The oxidation of ReCl{sub 5} with oleum: synthesis and crystal structure of Re{sub 2}O{sub 4}Cl{sub 4}(SO{sub 4})

Energy Technology Data Exchange (ETDEWEB)

Betke, Ulf; Wickleder, Mathias S. [Carl von Ossietzky University of Oldenburg, Institute of Pure and Applied Chemistry (Germany)

2012-01-15

The reaction of ReCl{sub 5} and fuming sulfuric acid (25 % SO{sub 3}) in a sealed glass tube at 200 C led to red, needle shaped single crystals of Re{sub 2}O{sub 4}Cl{sub 4}(SO{sub 4}) (monoclinic, C2/c, a = 1501.8(2) pm, b = 1545.9(2) pm, c = 945.18(8) pm, β = 98.761(9) , Z = 8). In the crystal structure the [ReO{sub 2}] moieties are linked by [SO{sub 4}]{sup 2-} tetrahedra to chains along the [101] direction. Each sulfate ion connects four rhenium atoms, additional two chloride ions complete the octahedral coordination sphere of each rhenium atom according to {sup 1}{sub ∞}[ReO{sub 2/1}Cl{sub 2/1}(SO{sub 4}){sub 2/4}]. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Studies of the structures of rhenium complexes with sulphur-containing amino acids: cysteine and homocysteine

International Nuclear Information System (INIS)

Arkowska, A.; Wojciechowski, W.

1979-01-01

Two rhenium compounds have been synthesized: compound 1 with cysteine HS-CH 2 -CH-NH 2 -COOH and compound 2 with homocysteine HS-CH 2 -CH 2 -CH-NH 2 -COOH. On the basis of spectroscopic measurements (IR, far IR, Raman, VIS and UV spectra) and magnetic susceptibility measurements their probable electronic and molecular structures have been determined. (author)

Near-Net Shape Powder Metallurgy Rhenium Thruster

Science.gov (United States)

Leonhardt, Todd; Hamister, Mark; Carlen, Jan C.; Biaglow, James; Reed, Brian

2001-01-01

This paper describes the development of a method to produce a near-net shape (NNS) powder metallurgy (PM) rhenium combustion chamber of the size 445 N (100 lbf) used in a high performance liquid apogee engine. These engines are used in low earth Orbit and geostationary orbit for satellite positioning systems. The developments in near-net shape powder metallurgy rhenium combustion chambers reported in this paper will reduce manufacturing cost of the rhenium chambers by 25 percent, and reduce the manufacturing time by 30 to 40 percent. The quantity of rhenium metal powder used to produce a rhenium chamber is reduced by approximately 70 percent and the subsequent reduction in machining schedule and costs is nearly 50 percent.

Clustering of transmutation elements tantalum, rhenium and osmium in tungsten in a fusion environment

Science.gov (United States)

You, Yu-Wei; Kong, Xiang-Shan; Wu, Xuebang; Liu, C. S.; Fang, Q. F.; Chen, J. L.; Luo, G.-N.

2017-08-01

The formation of transmutation solute-rich precipitates has been reported to seriously degrade the mechanical properties of tungsten in a fusion environment. However, the underlying mechanisms controlling the formation of the precipitates are still unknown. In this study, first-principles calculations are therefore performed to systemically determine the stable structures and binding energies of solute clusters in tungsten consisting of tantalum, rhenium and osmium atoms as well as irradiation-induced vacancies. These clusters are known to act as precursors for the formation of precipitates. We find that osmium can easily segregate to form clusters even in defect-free tungsten alloys, whereas extremely high tantalum and rhenium concentrations are required for the formation of clusters. Vacancies greatly facilitate the clustering of rhenium and osmium, while tantalum is an exception. The binding energies of vacancy-osmium clusters are found to be much higher than those of vacancy-tantalum and vacancy-rhenium clusters. Osmium is observed to strongly promote the formation of vacancy-rhenium clusters, while tantalum can suppress the formation of vacancy-rhenium and vacancy-osmium clusters. The local strain and electronic structure are analyzed to reveal the underlying mechanisms governing the cluster formation. Employing the law of mass action, we predict the evolution of the relative concentration of vacancy-rhenium clusters. This work presents a microscopic picture describing the nucleation and growth of solute clusters in tungsten alloys in a fusion reactor environment, and thereby explains recent experimental phenomena.

Directed light fabrication of rhenium components

Energy Technology Data Exchange (ETDEWEB)

Milewski, J.O.; Thoma, D.J.; Lewis, G.K.

1997-02-01

Directed Light Fabrication (DLF) is a direct metal deposition process that fuses powder, delivered by gas into the focal zone of a high powered laser beam to form fully dense near-net shaped components. This is accomplished in one step without the use of molds, dies, forming, pressing, sintering or forging equipment. DLF is performed in a high purity inert environment free from the contaminants associated with conventional processing such as oxide and carbon pickup, lubricants, binding agents, cooling or cleaning agents. Applications using rhenium have historically been limited in part by its workability and cost. This study demonstrates the ability to fuse rhenium metal powder, using a DLF machine, into free standing rods and describes the associated parameter study. Microstructural comparisons between DLF deposited rhenium and commercial rhenium sheet product is performed. This research combined with existing DLF technology demonstrates the feasibility of forming complex rhenium, metal shapes directly from powder.

Thermal conduction and linear expansion of sintered rhenium and tungsten-rhenium alloys at a temperature up to 1000 K

International Nuclear Information System (INIS)

Pozdnyak, N.Z.; Belyaev, R.A.; Vavilov, Yu.V.; Vinogradov, Yu.G.; Serykh, G.M.

1978-01-01

Preparation technology (by powder metallurgy methods) of sintered rhenium and tungsten-rhenium VR-5, VR-10, and VR-20 alloys is described. Thermal conduction of rhenium and VR-20 alloy has been measured in the temperature range from 300 to 1000 K. The value obtained turned out to be considerably less than those published elsewhere, this testifies to the great thermal contact resistance between the material grains. Also measured is the mean linear expansion coefficient for the mentioned above materials in the same temperature range. Linear expansion increases with rhenium content increase

Rhenium-osmium geochemistry: method and applications

International Nuclear Information System (INIS)

Luck, J.M.

1982-03-01

Experimental methods for chemical separation and isotopic analysis of rhenium-osmium are described. Accurate determinations are obtained for a quantity ratio around 10 -6 -10 -7 g. Development as a geochemical tracer is examined. Study of rhenium-osmium in meteorites allows the determination of solar system chronology and age of the galaxy. Rhenium-osmium chronology in meteorites is improved and osmium isotopes are used as petrogenetic and geological tracers. Molybdenites are studied through 187 Re- 187 Os dating [fr

Rhenium complexes of chromophore-appended dipicolylamine ligands: syntheses, spectroscopic properties, DNA binding and X-ray crystal structure

International Nuclear Information System (INIS)

Mullice, L.A.; Buurma, N.J.; Pope, S.J.A.; Laye, R.H.; Harding, L.P.

2008-01-01

The syntheses of two chromophore-appended dipicolylamine-derived ligands and their reactivity with penta-carbonyl-chloro-rhenium have been studied. The resultant complexes each possess the fac-Re(CO) 3 core. The ligands L 1 1-[bis(pyridine-2-yl-methyl)amino]methyl-pyrene and L 2 2-[bis(pyridine-2-yl-methyl)amino]methyl-quinoxaline were isolated via a one-pot reductive amination in moderate yield. The corresponding rhenium complexes were isolated in good yields and characterised by 1 H NMR, MS, IR and UV-Vis studies. X-Ray crystallographic data were obtained for fac-{Re(CO) 3 (L 1 )}(BF 4 ), C 34 H 26 BF 4 N 4 O 3 Re: monoclinic, P2(1)/c, a 18.327(2) Angstroms, α = 90.00 degrees, b 14.1537(14) Angstroms, β96.263(6) degrees, c = 23.511(3) Angstroms, γ 90.00 Angstroms, 6062.4(11) (Angstroms) 3 , Z=8. The luminescence properties of the ligands and complexes were also investigated, with the emission attributed to the appended chromophore in each case. Isothermal titration calorimetry suggests that fac-{Re(CO) 3 (L 1 )}(BF 4 ) self-aggregates cooperatively in aqueous solution, probably forming micelle-like aggregates with a cmc of 0.18 mM. Investigations into the DNA-binding properties of fac-{Re(CO) 3 (L 1 )}(BF 4 ) were undertaken and revealed that fac-{Re(CO) 3 (L 1 )}(BF 4 ) binding to fish sperm DNA (binding constant 1.5 ± 0.2 * 10 5 M -1 , binding site size 3.2 ± 0.3 base pairs) is accompanied by changes in the UV-Vis spectrum as typically observed for pyrene-based intercalators while the calorimetrically determined binding enthalpy (-14 ± 2 kcal mol -1 ) also agrees favourably with values as typically found for intercalators. (authors)

Preparation and crystal structure of carbonyltris (diethyldithiocarbamato) technetium (III): an unexpected source of co-ordinated carbon monoxide

International Nuclear Information System (INIS)

Baldas, J.; Bonnyman, J.; Pojer, P.M.; Williams, G.A.

1981-10-01

Tc(S 2 CNEt 2 ) 3 CO has been prepared by the reduction of NH 4 TcO 4 with formamidinesulphinic acid in the presence of NaS 2 CNEt 2 . It is suggested that the co-ordinated carbon monoxide is formed after co-ordination of formamidinesulphinic acid, or some decomposition product, with technetium. The crystal structure of Tc(S 2 CNEt 2 ) 3 CO has been determined by single-crystal X-ray diffraction methods at 17 deg. C. Diffractometry has provided significant Bragg intensities for 2045 independent reflections and the structure has been refined by full-matrix least-squares methods to R 0.049. The compound is isostructural with the rhenium analogue and consists of discrete Tc(S 2 CNEt 2 ) 3 CO molecules, each containing a terminal linear CO group. The technetium atom has a seven co-ordinate environment which is best described as a distorted pentagonal bipyramid

Rhenium corrosion in chloride melts

International Nuclear Information System (INIS)

Stepanov, A.D.; Shkol'nikov, S.N.; Vetyukov, M.M.

1989-01-01

The results investigating rhenium corrosion in chloride melts containing sodium, potassium and chromium ions by a gravimetry potentials in argon atmosphere in a sealing quarth cell are described. Rhenium corrosion is shown to be rather considerable in melts containing CrCl 2 . The value of corrosion rate depending on temperature is determined

Near net shape of powder metallurgy rhenium parts

International Nuclear Information System (INIS)

Leonhardt, T.; Downs, J.

2001-01-01

In this paper, a description of the stages of processing necessary to produce a near-net shape (NNS) powder metallurgy (PM) rhenium component through the use of cold isostatic pressing (CIP) to form a complex shape will be explained. This method was primarily developed for the production of the 440 N and 490 N liquid apogee engine combustion chambers used in satellite positioning systems. The CIP to NNS process has been used in the manufacture and production of other rhenium aerospace components as well. Cold isostatic pressing (CIP) to a near net shape utilizing a one or two-part mandrel greatly reduces the quantity of rhenium required to produce the component, and also significantly reduces the number of secondary machining operations necessary to complete the manufacturing process. Further, the developments in near-net shape powder metallurgy rhenium manufacturing techniques have generated significant savings in the area of both time and budget. Overall, cost declined by as much as 35 % for the quantity of rhenium chambers, and manufacturing time was decreased by 30-40 %. The quantity of rhenium metal powder used to produce a rhenium chamber was reduced by approximately 70 %, with a subsequent reduction of nearly 50 % in secondary machining operation schedules. Thus, it is apparent that the overall savings provided by the production of near-net shape powder metallurgy rhenium components will be more than merely another aspect of any project involving high temperature applications, it will constitute significant benefit. (author)

Development of industrial hydrogenating catalyst on rhenium base

International Nuclear Information System (INIS)

Chistyakova, G.A.; Bat', I.I.; Rebrova, V.V.

1975-01-01

Processes for forming rhenium catalysts on carbon carrier and their catalytic properties in nitrobenzene (NB) reduction were studied. Application of an ammonia preparation to the carbon surface produced impregnated carbon saturated at room temperature with a water solution of the ammonia preparation, taken in a volume equal to the volumetric capacity of the carbon. With one impregnation, 2% rhenium was taken up. Catalysts containing more than 5% rhenium were obtained by impregnating the carbon with heating and use of more concentrated solutions. Catalysts made in this way and dried at 100 0 C had the composition Re 2 OH/carbon/. The most active catalysts were those reduced at 200-250 0 C; higher temperatures, up to 300-500 0 C, decreased the activity. Study of the catalytic properties of the rhenium catalysts in a liquid phase reduction of NB showed that the specific activity of rhenium depends only slightly on the content of the active component in the catalyst and is close to the specific activity of palladium and considerably exceeds that of nickel. Study of the effect of the NB concentration and hydrogen pressure on the activity and stability of the 5% rhenium catalyst indicated that with NB concentrations from 50 to 10% the process takes place at an essentially constant rate; the order of the reaction was close to zero with an apparent activation energy of about 7000 cal/mole. At pressures of 15-200 atm the yield with the 5% catalyst was proportional to the hydrogen pressure. A big advantage of the rhenium catalysts in the reduction of NB is their high selectivity. With a higher activity than palladium and nickel catalysts, 5% rhenium catalyst produces a high operating capacity in a wide range of contact charges, which has considerable significance for industrial use in contact apparatus of the column type. Comparison of the costs of rhenium catalysts and granular carbon carrier with those of nickel, platinum, and palladium showed that 5% rhenium catalyst can

THE SYNTHESIS OF BIOCONJUGATE BASED ON RHENIUM(I CARBONYL COMPLEX FOR VISUALIZATION OF PATHOLOGICAL PROCESS

Directory of Open Access Journals (Sweden)

K. O. Piletska

2017-03-01

Full Text Available Tricarbonyl rhenium(I complexes have a great potential like biomarkers. It is caused their biological stability, low toxicity, large Stokes shifts, and long luminescence lifetimes. Rhenium tricarbonyl complexes fac-[Re(CO3(N^N], where N^N is a ligand with low π* orbitals are excellent candidates as imaging dyes. The method of obtaining potential biomarkers based on tricarbonyl rhenium(I complex with a 4-methyl-2,2’-bipyridine-4’-carboxylate by the addition of biomolecules by peptide synthesis was developed. The new complex [Re(CO3MebpyCOOHBr] was synthesized, composition and structure of which were established by mass spectrometry, IR and NMR spectroscopy. A selective attachment of receptor peptide enkephalin to complex [Re(CO3(MebpyCOOHBr] was performed. The formation of a new compound and its structure has been confirmed by HPLC and mass spectral analysis. The method which has been developed allows to connect various peptides to rhenium(I complex in the solution.

Extraction of rhenium(VII) by phosphorylated podands

International Nuclear Information System (INIS)

Turanov, A.N.; Karandashev, V.K.; Baulin, V.E.

2006-01-01

Interphase distribution of ReO 4 - between aqueous solutions of H 2 SO 4 and solutions of phosphoryl-containing podands in organic solvents is studied. Stoichiometry of the complexes extracted is determined. Effect of extractant structure and nature of organic solvent on efficiency of rhenium extraction into organic phase is determined [ru

Design criteria for rhenium-reduced nickel-based single-crystal alloys. Identification and computer-assisted conversion; Designkriterien fuer rheniumreduzierte Nickelbasis-Einkristalllegierungen. Identifikation und rechnergestuetzte Umsetzung

Energy Technology Data Exchange (ETDEWEB)

Goehler, Thomas

2016-06-17

In the present work, design criteria and property models for the creep strength optimization of rhenium-free nickel based single crystal Superalloys are investigated. The study focuses on a typical load condition of 1050 C and 150 MPa, which is representative for flight engine applications. Thereby the key aspect is to link chemical composition, manufacturing processes, microstructure formation and mechanistic understanding of dislocation creep through a computational materials engineering approach. Beside the positive effect of rhenium on solid solution hardening, a second mechanism in which rhenium increases high temperature creep strength is identified. It indirectly stabilizes precipitation hardening by reducing the coarsening kinetics of γ'-rafting. Five 1st and 2nd generation technical Superalloys show a comparable microstructure evolution for up to 2 % plastic elongation, while creep times differ by a factor of five. The application of a microstructure sensitive creep model shows that these coarsening processes can activate γ-cutting and thus lead to an increasing creep rate. Based on these calculations a threshold value of φ{sub γ/γ'} > 2,5 at 150 MPa is estimated. This ratio of matrix channel to raft thickness has been proofed for multiple positions by microstructure analysis of interrupted creep tests. The mechanism described previously can be decelerated by the enrichment of the γ-matrix with slow diffusing elements. The same principle also increases the solid solution strength of the γ-matrix. Therefore, the present work delivers an additional mechanistic explanation why creep properties of single phase nickel based alloys can be transferred to two phase technical Superalloys with rafted γ'-structure. Following, the best way to substitute both rhenium fundamental properties, namely a slow diffusion coefficient and a small solubility in g', has been investigated by means of CALPHAD-modeling. Only molybdenum and especially

Concentration of rhenium from dilute sodium chloride solutions

Directory of Open Access Journals (Sweden)

DRAGOLJUB M. LUKIC

2008-03-01

Full Text Available The conditions for the desorption of rhenium from the anion exchange resin Dowex 1-x8 by HNO3, HCl, H2SO4 and NaOH were determined. The solution (5.0´10-3 mol dm-3 Re in 0.15 mol dm-3 NaCl was passed through a column containing 0.10 g of the resin. The total sorbed amount of rhenium was 0.20 g/g of the resin. It was then eluted by the corresponding eluent in the concentration range up to about 3.0 mol dm-3. The highest elution efficiency and the most favourable elution profile were found with 3.0 mol dm-3 HNO3. Over 77 % of the sorbed rhenium was found in the first 5 ml of the eluate. Practically all the rhenium was recovered with 20 ml of the acid. Under the given experimental conditions, HCl and H2SO4 were less favourable while NaOH was not applicable, due to very low efficiency of rhenium elution.

Ambient aging of rhenium filaments used in thermal ionization mass spectrometry: Growth of oxo-rhenium crystallites and anti-aging strategies

Directory of Open Access Journals (Sweden)

Joseph M. Mannion

2017-01-01

Full Text Available Degassing is a common preparation technique for rhenium filaments used for thermal ionization mass spectrometric analysis of actinides, including plutonium. Although optimization studies regarding degassing conditions have been reported, little work has been done to characterize filament aging after degassing. In this study, the effects of filament aging after degassing were explored to determine a “shelf-life” for degassed rhenium filaments, and methods to limit filament aging were investigated. Zone-refined rhenium filaments were degassed by resistance heating under high vacuum before exposure to ambient atmosphere for up to 2 months. After degassing the nucleation and preferential growth of oxo-rhenium crystallites on the surface of polycrystalline rhenium filaments was observed by atomic force microscopy and scanning electron microscopy (SEM. Compositional analysis of the crystallites was conducted using SEM-Raman spectroscopy and SEM energy dispersive X-ray spectroscopy, and grain orientation at the metal surface was investigated by electron back-scatter diffraction mapping. Spectra collected by SEM-Raman suggest crystallites are composed primarily of perrhenic acid. The relative extent of growth and crystallite morphology were found to be grain dependent and affected by the dissolution of carbon into filaments during annealing (often referred to as carbonization or carburization. Crystallites were observed to nucleate in region specific modes and grow over time through transfer of material from the surface. Factors most likely to affect the rates of crystallite growth include rhenium substrate properties such as grain size, orientation, levels of dissolved carbon, and relative abundance of defect sites; as well as environmental factors such as length of exposure to oxygen and relative humidity. Thin (∼180 nm hydrophobic films of poly(vinylbenzyl chloride were found to slow the growth of oxo-rhenium crystallites on the filament

Studies of technetium chemistry. Pt.8. The regularities of the bond length and configuration of rhenium and technetium complexes in crystals

International Nuclear Information System (INIS)

Liu Guozheng; Liu Boli

1995-01-01

Some bond length regularities in MO 6 , MO-4, MX 5 α and MX 4 αβ moieties of technetium and rhenium compounds are summarized and rationalized by cavity model. The chemical properties of technetium and rhenium are so similar that their corresponding complexes have almost the same configuration and M-X bond lengths when they are in cavity-controlled state. Technetium and Rhenium combine preferably with N, O, F, S, Cl and Br when they are in higher oxidation states (>3), but preferably with P, Se etc. when they are in lower oxidation states ( 4 αβ is approximately constant; (2) the average M-X bond length of MX 6 varies moderately with the oxidation state of M; (3) the bond length of M-X trans to M-α in MX 5 α has a linear relationship with the angle

Characterization of rhenium compounds obtained by electrochemical synthesis after aging process

Energy Technology Data Exchange (ETDEWEB)

Vargas-Uscategui, Alejandro, E-mail: avargasuscat@ing.uchile.cl [Departamento de Ingeniería de Minas, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile); Mosquera, Edgar [Laboratorio de Materiales a Nanoescala, Departamento de Ciencia de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile); López-Encarnación, Juan M. [Department of Mathematics-Physics and Department of Chemistry, University of Puerto Rico at Cayey, 205 Ave. Antonio R. Barceló, Cayey, PR 00736, USA. (Puerto Rico); Chornik, Boris [Departamento de Física, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Blanco Encalada Av. 2008, Santiago (Chile); Katiyar, Ram S. [Department of Physics and Institute for Functional Nanomaterials, University of Puerto Rico San Juan, San Juan, PR 00931-3343 (United States); Cifuentes, Luis [Departamento de Ingeniería de Minas, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile)

2014-12-15

The proper identification of the molecular nature of the aged rhenium compound obtained by means of electrodeposition from an alkaline aqueous electrolyte was determined. Chemical, structural and vibrational experimental characterization of the aged Re compound showed agreement with quantum-computations, thereby allowing the unambiguous identification of the Re compound as H(ReO{sub 4})H{sub 2}O. - Graphical abstract: Rhenium oxides were electrodeposited on a copper surface and after environmental aging was formed the H(ReO{sub 4})H{sub 2}O compound. The characterization of the synthesized material was made through the comparison of experimental evidence with quantum mechanical computations carried out by means of density functional theory (DFT). - Highlights: • Aged rhenium compound obtained by means of electrodeposition was studied. • The study was made by combining experimental and DFT-computational information. • The aged electrodeposited material is consistent with the H(ReO{sub 4})H{sub 2}O compound.

Linkable thiocarbamoylbenzamidines as ligands for bioconjugation of Rhenium and Technetium; Kopplungsfaehige Thiocarbamoylbenzamidine als Liganden zur Biokonjugation von Rhenium und Technetium

Energy Technology Data Exchange (ETDEWEB)

Castillo Gomez, Juan Daniel

2015-04-27

Bioconjugation reactions with Rhenium and Technetium are of high importance for the development of novel radiopharmaceuticals for nuclear medicine. In this thesis the possibilities for bioconjugation using linkable Thiocarmbamoylbenzamidines as ligands for the complexation of Rhenium and Technetium were examined.

Thermophysical measurements on solid and liquid rhenium

International Nuclear Information System (INIS)

Pottlacher, G.; Jager, H.; Neger, T.

1986-01-01

A fast resistive heating technique was used to measure such thermophysical data of solid and liquid rhenium as enthalpy, specific heat, thermal volume expansion, and electrical resistivity. The measurements are performed with heating rates of slightly more than 10 9 K s -1 up to states of superheated liquid rhenium (7500 K)

Effect of Temperature and Mole Ratio on the Synthesis Yield of Rhenium-Tetrofosmin

Directory of Open Access Journals (Sweden)

Widyastuti

2015-08-01

Full Text Available Technetium-99m (99mTc tetrofosmin is widely used in nuclear medicine as a diagnostic agent for myocardial perfusion and as a tumor imaging agent. As a parenteral preparation it requires an evaluation of its pharmacokinetics and stability in-vivo. Since 99mTc has a short half-life and is only available in very low concentrations, it is impossible to characterize its chemical properties and presence in the body. Due to this reason, only technetium-99 (T1/2 = 5 × 105 years, which is available in macro quantities, or natural rhenium can be used for this purpose. In this study rhenium-188 (188Re tetrofosmin will be synthesized and applied, because non-radioactive Re can be easily obtained. Synthesis and radiochemical purity analysis of carrier-added 188Re-tetrofosmin were carried out as a model to study the in-vivo stability of technetium-99m tetrofosmin. Rhenium-188 was used as a tracer to identify the formation of rhenium tetrofosmin. Rhenium gluconate was synthesized first prior to the formation of rhenium tetrofosmin. The quality of labeling for both rhenium gluconate and rhenium tetrofosmin was analyzed using paper- and thin-layer chromatography, respectively. Rhenium gluconate can be synthesized with high labeling yield within 1 hour, whereas rhenium tetrofosmin was synthesized both in room temperature and in an elevated temperature with various tetrofosmin-to-rhenium mole ratios.The results showed that heating at 95oC led to a higher yield of more than 90% within 30 minutes. Rhenium tetrofosmin could be produced in high radiochemical purity using an excess of tetrofosmin with mole ratio of 2000. It is concluded that rhenium tetrofosmin could be synthesized through the formation of rhenium gluconate, and a higher yield could be obtained in a shorter time by heating process.

Synthesis and investigation of CrB{sub 4}, MnB{sub 4} and new ternary chromium and rhenium manganese borides; Synthese und Untersuchung von CrB{sub 4}, MnB{sub 4} sowie neuen ternaeren Chrom- und Rheniummanganboriden

Energy Technology Data Exchange (ETDEWEB)

Knappschneider, Arno

2014-10-13

In the present work single crystals of the tetraborides of chromium and manganese have been grown and allowed a structure refinement of the compounds. Furthermore the physical characteristics for example hardness, electronic properties and magnetism were been determined. Also the ternary tetraboride phase of chromium and manganese was synthesized and a new ternary rhenium manganese diboride could be obtained.

Determination of rhenium in geologic samples of sandstone-type uranium deposit

International Nuclear Information System (INIS)

Li Yanan; Wang Xiuqin; Yin Jinshuang

1997-01-01

The thiourea colorimetry method suitable for the determination of samples with rhenium content higher than 5 μg/g is described. The method is characterized by many advantages: stability of analytical results, simplicity and cheapness of reagent, and wide range of analysed samples. The catalytic colorimetry is also applied to determine trace rhenium meeting the demand for comprehensive appraisal of prospecting and exploration, recovery and utilization of rhenium. This method can also be applied to analyse rhenium of other samples

Work function of carburized rhenium

International Nuclear Information System (INIS)

Pallmer, P.G. Jr.; Gordon, R.L.; Dresser, M.J.

1980-01-01

Variations of the electronic work function of carburized rhenium foils containing approximately 5 at.% carbon have been observed using the contact potential difference technique. Surface work function was observed to vary between 5.25 and 4.1 eV, with the work function of pure rhenium taken as 5.0 eV. Decrease in work function has been ascribed to the formation of graphitic layers on the surface at temperatures below the temperature of saturated solubility. The high work function surface was observed with all carbon in solution and has been ascribed to the presence of amorphous carbon near the surface

Diverse roles of hydrogen in rhenium carbonyl chemistry: hydrides, dihydrogen complexes, and a formyl derivative.

Science.gov (United States)

Li, Nan; Xie, Yaoming; King, R Bruce; Schaefer, Henry F

2010-11-04

Rhenium carbonyl hydride chemistry dates back to the 1959 synthesis of HRe(CO)₅ by Hieber and Braun. The binuclear H₂Re₂(CO)₈ was subsequently synthesized as a stable compound with a central Re₂(μ-H)₂ unit analogous to the B₂(μ-H)₂ unit in diborane. The complete series of HRe(CO)(n) (n = 5, 4, 3) and H₂Re₂(CO)(n) (n = 9, 8, 7, 6) derivatives have now been investigated by density functional theory. In contrast to the corresponding manganese derivatives, all of the triplet rhenium structures are found to lie at relatively high energies compared with the corresponding singlet structures consistent with the higher ligand field splitting of rhenium relative to manganese. The lowest energy HRe(CO)₅ structure is the expected octahedral structure. Low-energy structures for HRe(CO)(n) (n = 4, 3) are singlet structures derived from the octahedral HRe(CO)₅ structure by removal of one or two carbonyl groups. For H₂Re₂(CO)₉ a structure HRe₂(CO)₉(μ-H), with one terminal and one bridging hydrogen atom, lies within 3 kcal/mol of the structure Re₂(CO)₉(η²-H₂), similar to that of Re₂(CO)₁₀. For H₂Re₂(CO)(n) (n = 8, 7, 6) the only low-energy structures are doubly bridged singlet Re₂(μ-H)₂(CO)(n) structures. Higher energy dihydrogen complex structures are also found.

Accelerator Production and Separations for High Specific Activity Rhenium-186

Energy Technology Data Exchange (ETDEWEB)

Jurisson, Silvia S. [Univ. of Missouri, Columbia, MO (United States); Wilbur, D. Scott [Univ. of Washington, Seattle, WA (United States)

2016-04-01

Tungsten and osmium targets were evaluated for the production of high specific activity rhenium-186. Rhenium-186 has potential applications in radiotherapy for the treatment of a variety of diseases, including targeting with monoclonal antibodies and peptides. Methods were evaluated using tungsten metal, tungsten dioxide, tungsten disulfide and osmium disulfide. Separation of the rhenium-186 produced and recycling of the enriched tungsten-186 and osmium-189 enriched targets were developed.

Electrocatalysis of the hydrogen evolution reaction by rhenium oxides electrodeposited by pulsed-current

International Nuclear Information System (INIS)

Vargas-Uscategui, Alejandro; Mosquera, Edgar; Chornik, Boris; Cifuentes, Luis

2015-01-01

Highlights: • Rhenium oxides were produced by means of pulsed current electrodeposition over ITO. • The electrocatalytic behavior of rhenium oxides electrodeposited over ITO was studied. • Electrodeposited rhenium oxides showed electrocatalytic behavior increasing the rate of the hydrogen evolution reaction. • The electrocatalysis behavior was explained considering the relative abundance of Re species on the surface of the electrodeposited material. - Abstract: Rhenium oxides are materials of interest for applications in the catalysis of reactions such as those occurring in fuel cells and photoelectrochemical cells. This research work was devoted to the production of rhenium oxide by means of pulsed current electrodeposition for the electrocatalysis of the hydrogen evolution reaction (HER). Rhenium oxides were electrodeposited over a transparent conductive oxide substrate (Indium Tin-doped Oxide – ITO) in an alkaline aqueous electrolyte. The electrodeposition process allowed the production of rhenium oxides islands (200–600 nm) with the presence of three oxidized rhenium species: Re"I"V associated to ReO_2, Re"V"I associated to ReO_3 and Re"V"I"I associated to H(ReO_4)H_2O. Electrodeposited rhenium oxides showed electrocatalytic behavior over the HER and an increase of one order of magnitude of the exchange current density was observed compared to the reaction taking place on the bare substrate. The electrocatalytic behavior varied with the morphology and relative abundance of oxidized rhenium species in the electrodeposits. Finally, two mechanisms of electrocatalysis were proposed to explain experimental results.

Tungsten - rhenium alloys wire: overview of thermomechanical processing and properties data

International Nuclear Information System (INIS)

Bryskin, B.

2001-01-01

The scope of this study encompasses the compositional modifications of the tungsten-rhenium dual system (W-3/5 Re up to W-27 Re) as well as some of the tungsten-molybdenum-rhenium ternary system. The alloys of interest are considered with a specific representation of powder metallurgy route based on doped or undoped tungsten vs. vacuum melted materials. This paper constitutes an in-depth review of structural and mechanical properties and systematic compilation of challenges necessary to provide the quality consistency of severely drawn filaments. The issue of thermomechanical processing trends is addressed as an important part of W-Re fabrication technology to achieve further improvement in design properties of rod and wire. (author)

Phase stability, physical properties of rhenium diboride under high pressure and the effect of metallic bonding on its hardness

International Nuclear Information System (INIS)

Zhong, Ming-Min; Kuang, Xiao-Yu; Wang, Zhen-Hua; Shao, Peng; Ding, Li-Ping; Huang, Xiao-Fen

2013-01-01

Highlights: •The transition pressure P t between the ReB 2 –ReB 2 and MoB 2 –ReB 2 phases is firstly determinate. •The single-bonded B–B feather remains in ReB 2 compounds. •A semiempirical method to evaluate the hardness of crystals with partial metallic bond is presented. •The large hardness (39.1 GPa) of ReB 2 –ReB 2 indicate that it is a superhard material. •The zigzag interconnected B–Re and B–B covalent bonds underlie the ultraincompressibilities. -- Abstract: Using first-principles calculations, the elastic constants, thermodynamic property and structural phase transition of rhenium diboride under pressure are investigated by means of the pseudopotential plane-waves method, as well as the effect of metallic bond on its hardness. Eight candidate structures of known transition-metal compounds are chosen to probe for rhenium diboride ReB 2 . The calculated lattice parameters are consistent with the experimental and theoretical values. Based on the third order Birch–Murnaghan equation of states, the transition pressure P t between the ReB 2 –ReB 2 and MoB 2 –ReB 2 phases is firstly determinate. Elastic constants, shear modulus, Young’s modulus, Poisson’s ratio and Debye temperature are derived. The single-bonded B–B feather remains in ReB 2 compounds. Furthermore, according to Mulliken overlap population analysis, a semiempirical method to evaluate the hardness of multicomponent crystals with partial metallic bond is presented. Both strong covalency and a zigzag topology of interconnected bonds underlie the ultraincompressibilities. In addition, the superior performance and large hardness (39.1 GPa) of ReB 2 –ReB 2 indicate that it is a superhard material

Effect of rhenium addition on tungsten fuzz formation in helium plasmas

Energy Technology Data Exchange (ETDEWEB)

Khan, Aneeqa, E-mail: aneeqa.khan-3@postgrad.manchester.ac.uk [School of Mechanical, Aerospace and Civil Engineering, The University of Manchester, M13 9PL (United Kingdom); De Temmerman, Gregory [ITER Organization, Route de Vinon-sur-Verdon, CS 90 046 - 13067 St Paul Lez Durance Cedex (France); Morgan, Thomas W. [FOM Institute DIFFER – Dutch Institute for Fundamental Energy Research, Partner in the Trilateral Euregio Cluster, Eindhoven (Netherlands); Ward, Michael B. [Institute for Materials Research, School of Chemical Process Engineering, University of Leeds, Leeds, LS2 9JT (United Kingdom)

2016-06-15

The effect of the addition of rhenium to tungsten on the formation of a nanostructure referred to as ‘fuzz’ when exposed to helium plasmas at fusion relevant ion fluxes was investigated in the Magnum and Pilot PSI devices at the FOM Institute DIFFER. The effect rhenium had on fuzz growth was seen to be dependent on time, temperature and flux. Initial fuzz growth was seen to be highly dependent on grain orientation, with rhenium having little effect. Once the fuzz was fully developed, the effect of grain orientation disappeared and the rhenium had an inhibiting effect on growth. This could be beneficial for inhibiting fuzz growth in a future fusion reactor, where transmutation of tungsten to rhenium is expected. It also appears that erosion or annealing of the fuzz is limiting growth of fuzz at higher temperatures in the range of ∼1340 °C.

Effect of rhenium addition on tungsten fuzz formation in helium plasmas

International Nuclear Information System (INIS)

Khan, Aneeqa; De Temmerman, Gregory; Morgan, Thomas W.; Ward, Michael B.

2016-01-01

The effect of the addition of rhenium to tungsten on the formation of a nanostructure referred to as ‘fuzz’ when exposed to helium plasmas at fusion relevant ion fluxes was investigated in the Magnum and Pilot PSI devices at the FOM Institute DIFFER. The effect rhenium had on fuzz growth was seen to be dependent on time, temperature and flux. Initial fuzz growth was seen to be highly dependent on grain orientation, with rhenium having little effect. Once the fuzz was fully developed, the effect of grain orientation disappeared and the rhenium had an inhibiting effect on growth. This could be beneficial for inhibiting fuzz growth in a future fusion reactor, where transmutation of tungsten to rhenium is expected. It also appears that erosion or annealing of the fuzz is limiting growth of fuzz at higher temperatures in the range of ∼1340 °C.

Analysis of the Nuclear Structure of Rhenium-186 Using Neutron-Induced Reactions

Science.gov (United States)

2015-03-26

5 1.5 Methods ... radioisotope power source for use on the battlefield. 1 Re-Os Cosmochronometer. The isotope 187Re has a half-life in its ground state of 4.35⇥ 1010 years [2...187Os in meteorites permits one to date the nucleosynthesis of rhenium and osmium by high neutron flux events such as supernovae. The Re-Os radioactive

Determination of rhenium in ores of complex composition by the kinetic method

Energy Technology Data Exchange (ETDEWEB)

Pavlova, L G; Gurkina, T V [Kazakhskij Gosudarstvennyj Univ., Alma-Ata (USSR); Tsentral' naya Lab. Yuzhno-Kazakhstanskogo Geologicheskogo Upravleniya, Alma-Ata (USSR))

1979-09-01

The kinetic rhenium determination method is proposed based on rhenium catalytic effect in the reaction of malachite green with thiourea. The accompanying elements, excluding molybdenum, do not interfere with the rhenium determination at their concentration of up to 0.1 M. The interfering influence of molybdenum can be eliminated by addition of tartaric acid to the solution up to the concentration of 0.1 M. This enables to determine rhenium in presence of 1000-fold quantity of molybdenum. The method is applicable for the analysis of complex copper-zinc sulphide ores.

Nipponium, the element ascribable to rhenium from the modern chemical viewpoint

Energy Technology Data Exchange (ETDEWEB)

Yoshihara, H.K. [Japan Isotope Data Inst., Sendai (Japan)

1997-11-01

Though the discovery of nipponium by Ogawa in 1908 was judged to be false and his work was forgotten for many years, the new element he believed to have found should be ascribed to rhenium (z = 75) by the following reasons: (1) the spectral line of 4882 A agrees well with the present data of rhenium, (2) recalculation of the atomic weight of the element supports the value in the neighbourhood of 185 which is very close to the present value 186.2 of rhenium, and (3) rhenium is actually present in Japanese molybdenite he studied. Therefore, it is concluded that his discovery of the `new` element was correct, but assignment of z = 43 was wrong. (orig.)

Method of stably radiolabeling antibodies with technetium and rhenium

International Nuclear Information System (INIS)

Paik, C.H.; Reba, R.C.; Eckelman, W.C.

1987-01-01

A method is described for labeling antibodies or antibody fragments with radionuclides of technetium or rhenium to obtain stable labeling, comprising: reacting a reduced radioisotope of technetium or rhenium with an antibody or antibody fragment, or a diethylenetriaminepentaacetic acid conjugated antibody or antibody fragment, in the presence of free or carrier-bound diethylenetriaminepentaacetic acid (DTPA). The amount of DTPA is sufficient to substantially completely inhibit binding of the reduced technetium or rhenium to nonstable binding sites of the antibody or antibody fragment, or the DTPA-conjugated antibody or antibody fragment. The resultant stably labeled antibody or antibody fragment, or DTPA[conjugated antibody or antibody fragment is recovered

Lattice strains in gold and rhenium under nonhydrostatic compression to 37 GPa

International Nuclear Information System (INIS)

Duffy, Thomas S.; Shen, Guoyin; Heinz, Dion L.; Shu, Jinfu; Ma, Yanzhang; Mao, Ho-Kwang; Hemley, Russell J.; Singh, Anil K.

1999-01-01

Using energy-dispersive x-ray diffraction techniques together with the theory describing lattice strains under nonhydrostatic compression, the behavior of a layered sample of gold and rhenium has been studied at pressures of 14-37 GPa. For gold, the uniaxial stress component t is consistent with earlier studies and can be described by t=0.06+0.015P where P is the pressure in GPa. The estimated single-crystal elastic moduli are in reasonable agreement with trends based on extrapolated low-pressure data. The degree of elastic anisotropy increases as α, the parameter which characterizes stress-strain continuity across grain boundaries, is reduced from 1.0 to 0.5. For rhenium, the apparent equation of state has been shown to be strongly influenced by nonhydrostatic compression, as evidenced by its dependence on the angle ψ between the diffracting plane normal and the stress axis. The bulk modulus obtained by inversion of nonhydrostatic compression data can differ by nearly a factor of 2 at angles of 0 degree sign and 90 degree sign . On the other hand, by a proper choice of ψ, d spacings corresponding to quasihydrostatic compression can be obtained from data obtained under highly nonhydrostatic conditions. The uniaxial stress in rhenium over the pressure range from 14-37 GPa can be described by t=2.5+0.09P. The large discrepancy between x-ray elastic moduli and ultrasonic data and theoretical calculations indicates that additional factors such as texturing or orientation dependence of t need to be incorporated to more fully describe the strain distribution in hexagonal-close-packed metals. (c) 1999 The American Physical Society

Separation of Rhenium (VII) from Tungsten (VI)

International Nuclear Information System (INIS)

Vucina, J.; Lukic, D.; Stoiljkovic, M.; Milosevic, M.; Orlic, M.

2004-01-01

Examined were the conditions for an effective separation of tungsten (VI) and rhenium (VII) on alumina if the solution of 0.20 mol dm -3 NaCl, ph=2.6 is used as the aqueous phase. Under the given experimental conditions alumina was found to be much better adsorbent for tungsten than for rhenium. The breakthrough and saturation capacities of alumina at pH=2 are 24 and 78 mg W/g Al 2 O 3 , respectively. With the increase of pH these values decrease. So, at pH=6 they are only 4 and 13 mg W/g Al 2 O 3 respectively. The elution volume for rhenium for the given column dimensions and quantity of the adsorbent is about 16 ml. These results were confirmed by the experiments of the radiological separations. Tungsten-187 remains firmly bound to the alumina. The radionuclide purity of the eluted 186'188 Re at pH=2 is very high. (authors)

Determination of rhenium in molybdenite by neutron-activation analysis.

Science.gov (United States)

Terada, K; Yoshimura, Y; Osaki, S; Kiba, T

1967-01-01

A neutron-activation method is described for the determination of rhenium in molybdenite. Radiochemical separation by a carrier technique was carried out very rapidly by means of successive liquid-liquid extraction processes. The recovery of rhenium, which was determined by a spectrophotometric method, was about 93%. About 10 samples could be analysed within 6 hr in parallel runs.

Rhenium solubility in borosilicate nuclear waste glass: implications for the processing and immobilization of technetium-99.

Science.gov (United States)

McCloy, John S; Riley, Brian J; Goel, Ashutosh; Liezers, Martin; Schweiger, Michael J; Rodriguez, Carmen P; Hrma, Pavel; Kim, Dong-Sang; Lukens, Wayne W; Kruger, Albert A

2012-11-20

The immobilization of technetium-99 ((99)Tc) in a suitable host matrix has proven to be a challenging task for researchers in the nuclear waste community around the world. In this context, the present work reports on the solubility and retention of rhenium, a nonradioactive surrogate for (99)Tc, in a sodium borosilicate glass. Glasses containing target Re concentrations from 0 to 10,000 ppm [by mass, added as KReO(4) (Re(7+))] were synthesized in vacuum-sealed quartz ampules to minimize the loss of Re from volatilization during melting at 1000 °C. The rhenium was found as Re(7+) in all of the glasses as observed by X-ray absorption near-edge structure. The solubility of Re in borosilicate glasses was determined to be ~3000 ppm (by mass) using inductively coupled plasma optical emission spectroscopy. At higher rhenium concentrations, additional rhenium was retained in the glasses as crystalline inclusions of alkali perrhenates detected with X-ray diffraction. Since (99)Tc concentrations in a glass waste form are predicted to be wastes, assuming Tc as Tc(7+) and similarities between Re(7+) and Tc(7+) behavior in this glass system.

Rhenium(5) and molybdenum(5) complexes with 4',4(5)-divaleryldibenzo-18-crown-6

International Nuclear Information System (INIS)

Ashurova, N.Kh.; Yakubov, K.G.; Tashmukhamedova, A.K.; Basitova, S.M.

1993-01-01

Methods for synthesizing oxohalide complexes of rhenium and molybdenum with +5 oxidation degree with 4',4 (5) -divaleryldibenzo-18-crown-6 were developed. Content and composition of prepared compounds were investigated by the methods of element analysis, crystal optics, conductometry, IR spectroscopy in the near and far regions, thermogravimetry. Oxidation degree of the complex-forming metal was determined. It was established that composition of the compounds coressponded to the general formula MOLX · H 2 O, where M - Re, Mo; L -4',4 (5) -divaleryldibenzo-18-crown-6; X -Cl - , Br -

A comparative study of electrochemical and optical properties of rhenium deposited on gold and platinum

Energy Technology Data Exchange (ETDEWEB)

Zerbino, Jorge O.; Castro Luna, Ana M.; Martins, M. E. [Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Buenos Aires (Argentina). Inst. de Investigaciones Fisico-Quimicas, Teoricas y Aplicadas (INIFTA)]. E-mail: mmartins@inifta.unlp.edu.ar; Zinola, Carlos F.; Mendez, Eduardo [Universidad de la Republica, Montevideo (Uruguay). Facultad de Ciencias. Lab. de Electroquimica Fundamental

2002-08-01

Rhenium-containing films were grown on gold and platinum after different potentiostatic and potentiodynamic polarizations in the - 0.20 V to 0.70 V range (vs rhe) in aqueous acid perrhenate. Experimental data were obtained using cyclic voltammetry and ellipsometry, from which the thickness and optical indices of the electrodeposited rhenium layer were calculated. Metallic rhenium deposition on gold takes place at potentials within the hydrogen evolution reaction. Rhenium oxide on platinum is formed in the hydrogen adatom potential domain, whereas metallic rhenium is deposited concurrently with the hydrogen adsorption and evolution reactions on the same metal. (author)

A comparative study of electrochemical and optical properties of rhenium deposited on gold and platinum

Directory of Open Access Journals (Sweden)

Zerbino Jorge O.

2002-01-01

Full Text Available Rhenium-containing films were grown on gold and platinum after different potentiostatic and potentiodynamic polarizations in the - 0.20 V to 0.70 V range (vs rhe in aqueous acid perrhenate. Experimental data were obtained using cyclic voltammetry and ellipsometry, from which the thickness and optical indices of the electrodeposited rhenium layer were calculated. Metallic rhenium deposition on gold takes place at potentials within the hydrogen evolution reaction. Rhenium oxide on platinum is formed in the hydrogen adatom potential domain, whereas metallic rhenium is deposited concurrently with the hydrogen adsorption and evolution reactions on the same metal.

Highvalent and organometallic technetium and rhenium compounds

International Nuclear Information System (INIS)

Oehlke, Elisabeth

2010-01-01

Diagnostic methods in nuclear medicine allow a detailed description of morphological organ structures and their function. The beta emitting isotope Tc-99 has optimal physical properties (140 keV gamma rays, half-life 6 h) and is therefore used for radiopharmaceuticals. The thesis is concerned with the search for new technetium complexes and their reproducible production. The (TcO3) core is of main interest. The second part of the thesis deals with organometallic technetium and rhenium complexes with carbonyl ligands and N-heterocyclic carbenes that show stability in aerobic aqueous solutions.

New leads for fragment-based design of rhenium/technetium radiopharmaceutical agents.

Science.gov (United States)

Brink, Alice; Helliwell, John R

2017-05-01

Multiple possibilities for the coordination of fac -[Re(CO) 3 (H 2 O) 3 ] + to a protein have been determined and include binding to Asp, Glu, Arg and His amino-acid residues as well as to the C-terminal carboxylate in the vicinity of Leu and Pro. The large number of rhenium metal complex binding sites that have been identified on specific residues thereby allow increased target identification for the design of future radiopharmaceuticals. The core experimental concept involved the use of state-of-art tuneable synchrotron radiation at the Diamond Light Source to optimize the rhenium anomalous dispersion signal to a large value ( f '' of 12.1 electrons) at its L I absorption edge with a selected X-ray wavelength of 0.9763 Å. At the Cu  K α X-ray wavelength (1.5418 Å) the f '' for rhenium is 5.9 electrons. The expected peak-height increase owing to the optimization of the Re f '' was therefore 2.1. This X-ray wavelength tuning methodology thereby showed the lower occupancy rhenium binding sites as well as the occupancies of the higher occupancy rhenium binding sites.

New leads for fragment-based design of rhenium/technetium radiopharmaceutical agents

Directory of Open Access Journals (Sweden)

Alice Brink

2017-05-01

Full Text Available Multiple possibilities for the coordination of fac-[Re(CO3(H2O3]+ to a protein have been determined and include binding to Asp, Glu, Arg and His amino-acid residues as well as to the C-terminal carboxylate in the vicinity of Leu and Pro. The large number of rhenium metal complex binding sites that have been identified on specific residues thereby allow increased target identification for the design of future radiopharmaceuticals. The core experimental concept involved the use of state-of-art tuneable synchrotron radiation at the Diamond Light Source to optimize the rhenium anomalous dispersion signal to a large value (f′′ of 12.1 electrons at its LI absorption edge with a selected X-ray wavelength of 0.9763 Å. At the Cu Kα X-ray wavelength (1.5418 Å the f′′ for rhenium is 5.9 electrons. The expected peak-height increase owing to the optimization of the Re f′′ was therefore 2.1. This X-ray wavelength tuning methodology thereby showed the lower occupancy rhenium binding sites as well as the occupancies of the higher occupancy rhenium binding sites.

Monoclonal Antibodies Radiolabeling with Rhenium-188 for Radioimmunotherapy

Science.gov (United States)

Martini, Petra; Pasquali, Micol

2017-01-01

Rhenium-188, obtained from an alumina-based tungsten-188/rhenium-188 generator, is actually considered a useful candidate for labeling biomolecules such as antibodies, antibody fragments, peptides, and DNAs for radiotherapy. There is a widespread interest in the availability of labeling procedures that allow obtaining 188Re-labeled radiopharmaceuticals for various therapeutic applications, in particular for the rhenium attachment to tumor-specific monoclonal antibodies (Mo)Abs for immunotherapy. Different approaches have been developed in order to obtain 188Re-radioimmunoconjugates in high radiochemical purity starting from the generator eluted [188Re]ReO4−. The aim of this paper is to provide a short overview on 188Re-labeled (Mo)Abs, focusing in particular on the radiolabeling methods, quality control of radioimmunoconjugates, and their in vitro stability for radioimmunotherapy (RIT), with particular reference to the most important contributions published in literature in this topic. PMID:28951872

Manufacture and properties of molybdenum-rhenium alloys

International Nuclear Information System (INIS)

Fischer, B.; Freund, D.

2001-01-01

It is necessary to measure strength and creep behavior to guarantee the safe and reliable usage of refractory alloys at extremely high temperatures. In the literature there is very little information available about the properties of Mo-Re alloys at temperatures higher than 1000 C. A special test facility has been designed and built for stress-rupture testing at very high temperatures (up to 3000 C) of refractory metals and alloys in inert atmospheres. - The stress-rupture strength as well as the creep behavior of molybdenum-rhenium alloys with rhenium contents between 41 and 51 wt.% have been determined at temperatures ranging from 1200 to 2000 C, and rupture times of up to 10 hours using this facility. Previous measurements of stress-rupture strength and creep behavior of pure rhenium have been compared with the measurement results of Mo-Re alloys. - The discussion of the values measured is based on metallographic test results and scanning electron microscopy (SEM) images of Mo-Re alloy samples after stress-rupture testing. (orig.) [de

Electrodialysis separation of rhenium from silicon

International Nuclear Information System (INIS)

Prasolova, O.D.; Borisova, L.V.; Ermakov, A.N.

1989-01-01

A method of separation of ruthenium from silicon by electrodialysis with heterogenuos ion-exchange membranes is developed. The effeciency of purification of rhenium from silicon depending on the number of dialyzer chambers, temperature and pH value of the dialyzate is studed. It is found that an addditional fourth chamber between the middle and anolytic ones causes the purification coefficient increase 50 times. It is necessary to cool the dialyzate in order to reduce silicon migration into the anolyte and reverse diffusion of perrhenate-ion from the anolyte into the dialyzate. The optimal pH value of diaizate is 5.5-6. The method developed has been used for separating rhenium from industrial solution of lead production with complex composition

Rhenium(V) complexes with sulfur-containing amino acids

International Nuclear Information System (INIS)

Gagieva, S.Ch.; Tautieva, M.A.; Tsaloev, A.T.; Galimov, Yu.B.; Gagieva, L.Ch.; Belyaeva, T.N.

2007-01-01

Rhenium(V) complexes with 2-amino-4-(methylthio)butanoic acid (methionine, Met) and 2-amino-3-sulfopropionic acid (cysteine, Cys) have been synthesized. Depending on the initial reagent ratio, the resulting complexes contain one or two ligand molecules. On heating the compounds with one amino acid molecule, two hydrogen halide molecules are removed at 128-132 deg C to form a molecular complex. The composition, structure, and thermal stability of the complexes have been studied by elemental analysis, conductometry, IR spectroscopy, NMR, and mass spectrometry [ru

Determination of rhenium in molybdenite by X-ray fluorescence: A combined chemical-spectrometric technique.

Science.gov (United States)

Solt, M W; Wahlberg, J S; Myers, A T

1969-01-01

Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 microg of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods.

Determination of rhenium in molybdenite by X-ray fluorescence. A combined chemical-spectrometric technique

Science.gov (United States)

Solt, M.W.; Wahlberg, J.S.; Myers, A.T.

1969-01-01

Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 ??g of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. ?? 1969.

Effect of rhenium addition on tungsten fuzz formation in helium plasmas

NARCIS (Netherlands)

Khan, A.; De Temmerman, G.; Morgan, T. W.; M. B. Ward,

2016-01-01

The effect of the addition of rhenium to tungsten on the formation of a nanostructure referred to as ‘fuzz’ when exposed to helium plasmas at fusion relevant ion fluxes was investigated in the Magnum and Pilot PSI devices at the FOM Institute DIFFER. The effect rhenium had on fuzz growth was seen to

Neutron activation determination of rhenium in shales shales and molybdenites

International Nuclear Information System (INIS)

Zajtsev, E.I.; Radinovich, B.S.

1977-01-01

Described is the technique for neutron activation determination of rhenium in shales and molybdenites with its radiochemical extraction separation by methyl-ethyl ketone. The sensitivity of the analysis is 5x10 -7 %. Experimental checking of the developed technique in reference to the analysis of shales and molybdenites was carried out. Estimated is the possibility of application of X-ray gamma-spectrometer to instrumental determination of rhenium in molybdenites

Synthesis and study of rhenium (5) complexes with benzimidazole and rubeanic acid

Energy Technology Data Exchange (ETDEWEB)

Basitova, S M; Yurina, R D; Kotegov, K V; Amindzhanov, A A

1986-01-01

Mixed rhenium (5) oxohalide complex compounds with benzimidazole and rubeanic acid are synthesized. Composition of the compounds obtained is established by IR spectroscpy thermal and chemical analyses. It is shown that rhenium (5) chloride compound stability to pyrolysis is rather lower than that of the corresponding bromide derivatives.

Synthesis and study of rhenium (5) complexes with benzimidazole and rubeanic acid

International Nuclear Information System (INIS)

Basitova, S.M.; Yurina, R.D.; Kotegov, K.V.; Amindzhanov, A.A.

1986-01-01

Mixed rhenium (5) oxohalide complex compounds with benzimidazole and rubeanic acid are synthesized. Composition of the compounds obtained is established by IR spectroscpy thermal and chemical analyses. It is shown that rhenium (5) chloride compound stability to pyrolysis is rather lower than that of the corresponding bromide derivatives

Cermets based on rhenium and rare earth element oxides

International Nuclear Information System (INIS)

Varfolomeev, M.B.; Velichko, A.V.; Zajtseva, L.L.; Shishkov, N.V.

1977-01-01

The reduction of perrhenates of rare earth elements and of yttrium by hydrogen and the subsequent sintering have yielded cermets based on rhenium and rare earth element oxides inherent in which are more disperse and homogeneous structures than those of the ''molecular'' rare earth element-Tc cermets. The dispersity of cermets increases in the rare earth elements series from La to Lu. The microhardness of the Re phase in cermets is 490 kgf/mm 2 ; the total microhardness of a cermet is substantially higher

Rhenium Mechanical Properties and Joining Technology

Science.gov (United States)

Reed, Brian D.; Biaglow, James A.

1996-01-01

Iridium-coated rhenium (Ir/Re) provides thermal margin for high performance and long life radiation cooled rockets. Two issues that have arisen in the development of flight Ir/Re engines are the sparsity of rhenium (Re) mechanical property data (particularly at high temperatures) required for engineering design, and the inability to directly electron beam weld Re chambers to C103 nozzle skirts. To address these issues, a Re mechanical property database is being established and techniques for creating Re/C103 transition joints are being investigated. This paper discusses the tensile testing results of powder metallurgy Re samples at temperatures from 1370 to 2090 C. Also discussed is the evaluation of Re/C103 transition pieces joined by both, explosive and diffusion bonding. Finally, the evaluation of full size Re transition pieces, joined by inertia welding, as well as explosive and diffusion bonding, is detailed.

Crystal structure and magnetic susceptibility of UOSe single crystals

International Nuclear Information System (INIS)

Kaczorowski, D.; Muenster Univ.; Poettgen, R.; Jeitschko, W.; Gajek, Z.; Zygmunt, A.

1993-01-01

The crystal structure and magnetic susceptibility behaviour of UOSe single crystals have been studied. UOSe crystalizes in the tetragonal PbFC1-type structure (space group P4/nmm) with the lattice parameters: a = 390.38(5) pm and c = 698.05(9) pm. It orders antiferromagnetically at T N =100±2 K and exhibits a very strong anisotropy in the susceptibility vs temperature variation. The magnetic and thermodynamic properties of UOSe are successfully interpreted in the framework of a perturbative ab initio crystal field approach. (Author)

Crystal structure and magnetic susceptibility of UOSe single crystals

Energy Technology Data Exchange (ETDEWEB)

Kaczorowski, D. (Polish Academy of Sciences, Wroclaw (Poland). Inst. for Low Temperature and Structure Research Muenster Univ. (Germany). Anorganisch-Chemisches Inst.); Poettgen, R.; Jeitschko, W. (Muenster Univ. (Germany). Anorganisch-Chemisches Inst.); Gajek, Z.; Zygmunt, A. (Polish Academy of Sciences, Wroclaw (Poland). Inst. for Low Temperature and Structure Research)

1993-01-01

The crystal structure and magnetic susceptibility behaviour of UOSe single crystals have been studied. UOSe crystalizes in the tetragonal PbFC1-type structure (space group P4/nmm) with the lattice parameters: a = 390.38(5) pm and c = 698.05(9) pm. It orders antiferromagnetically at T[sub N]=100[+-]2 K and exhibits a very strong anisotropy in the susceptibility vs temperature variation. The magnetic and thermodynamic properties of UOSe are successfully interpreted in the framework of a perturbative ab initio crystal field approach. (Author).

Mew organometallic complexes of technetium in different oxidation states

International Nuclear Information System (INIS)

Joachim, J.E.

1993-09-01

New organometallic compounds of Tc(I), Tc(III) and Tc(VII) were synthesized and their properties examined. These compounds were correlated with their homologous compounds of manganese and rhenium, which were also synthesized by the same route. The molecular and crystal structures of most technetium complexes and of the homologous complexes of manganese and rhenium were determined by single crystal X-ray diffraction. (orig.) [de

Lymph node scintigraphy with sup(99m)Tc-rhenium colloid

International Nuclear Information System (INIS)

Mitsuhata, Naoki; Suyama, Bunzo; Matsumura, Yosuke; Ohmori, Hiroyuki

1981-01-01

Lymph node scintigraphy with sup(99m)Tc-rhenium colloid in evaluation of nodal involvement by urological malignancy were performed on twelve cases (4 bladder cancer, 3 prostatic cancer, 2 penile cancer and 3 testicular tumor). These cases had been examined the extent of disease on the basis of findings at pedal lymphangiography, urography, computed tomography or laparotomy. sup(99m)Tc-rhenium colloid in a volume of 0.2 ml (2 mCi) was injected into the first interdigital webs of each foot without local anesthesia. In one case of penile cancer radioactive colloid was directly injected into the glans penis and prepuce including tumor area. Our clinical experience reported here reveals that lymph node scintigraphy with sup(99m)Tc-rhenium colloid can provide a useful method of investigating the lymphatic system. This technique is reproducible and can be performed in poor risk patients or pediatric patients readily and safely. (author)

Prediction of molecular crystal structures

International Nuclear Information System (INIS)

Beyer, Theresa

2001-01-01

The ab initio prediction of molecular crystal structures is a scientific challenge. Reliability of first-principle prediction calculations would show a fundamental understanding of crystallisation. Crystal structure prediction is also of considerable practical importance as different crystalline arrangements of the same molecule in the solid state (polymorphs)are likely to have different physical properties. A method of crystal structure prediction based on lattice energy minimisation has been developed in this work. The choice of the intermolecular potential and of the molecular model is crucial for the results of such studies and both of these criteria have been investigated. An empirical atom-atom repulsion-dispersion potential for carboxylic acids has been derived and applied in a crystal structure prediction study of formic, benzoic and the polymorphic system of tetrolic acid. As many experimental crystal structure determinations at different temperatures are available for the polymorphic system of paracetamol (acetaminophen), the influence of the variations of the molecular model on the crystal structure lattice energy minima, has also been studied. The general problem of prediction methods based on the assumption that the experimental thermodynamically stable polymorph corresponds to the global lattice energy minimum, is that more hypothetical low lattice energy structures are found within a few kJ mol -1 of the global minimum than are likely to be experimentally observed polymorphs. This is illustrated by the results for molecule I, 3-oxabicyclo(3.2.0)hepta-1,4-diene, studied for the first international blindtest for small organic crystal structures organised by the Cambridge Crystallographic Data Centre (CCDC) in May 1999. To reduce the number of predicted polymorphs, additional factors to thermodynamic criteria have to be considered. Therefore the elastic constants and vapour growth morphologies have been calculated for the lowest lattice energy

Prediction of molecular crystal structures

Energy Technology Data Exchange (ETDEWEB)

Beyer, Theresa

2001-07-01

The ab initio prediction of molecular crystal structures is a scientific challenge. Reliability of first-principle prediction calculations would show a fundamental understanding of crystallisation. Crystal structure prediction is also of considerable practical importance as different crystalline arrangements of the same molecule in the solid state (polymorphs)are likely to have different physical properties. A method of crystal structure prediction based on lattice energy minimisation has been developed in this work. The choice of the intermolecular potential and of the molecular model is crucial for the results of such studies and both of these criteria have been investigated. An empirical atom-atom repulsion-dispersion potential for carboxylic acids has been derived and applied in a crystal structure prediction study of formic, benzoic and the polymorphic system of tetrolic acid. As many experimental crystal structure determinations at different temperatures are available for the polymorphic system of paracetamol (acetaminophen), the influence of the variations of the molecular model on the crystal structure lattice energy minima, has also been studied. The general problem of prediction methods based on the assumption that the experimental thermodynamically stable polymorph corresponds to the global lattice energy minimum, is that more hypothetical low lattice energy structures are found within a few kJ mol{sup -1} of the global minimum than are likely to be experimentally observed polymorphs. This is illustrated by the results for molecule I, 3-oxabicyclo(3.2.0)hepta-1,4-diene, studied for the first international blindtest for small organic crystal structures organised by the Cambridge Crystallographic Data Centre (CCDC) in May 1999. To reduce the number of predicted polymorphs, additional factors to thermodynamic criteria have to be considered. Therefore the elastic constants and vapour growth morphologies have been calculated for the lowest lattice energy

Study of the electrodeposition of rhenium thin films by electrochemical quartz microbalance and X-ray photoelectron spectroscopy

International Nuclear Information System (INIS)

Schrebler, R.; Cury, P.; Suarez, C.; Munoz, E.; Vera, F.; Cordova, R.; Gomez, H.; Ramos-Barrado, J.R.; Leinen, D.; Dalchiele, E.A.

2005-01-01

Rhenium thin films were prepared by electrodeposition from an aqueous solution containing 0.1 M Na 2 SO 4 +H 2 SO 4 , pH 2 in presence of y mM HReO 4 . As substrates polycrystalline gold (y=0.75 mM HReO 4 ) and monocrystalline n-Si(100) (y=40 mM HReO 4 ) were used. The electrochemical growth of rhenium was studied by cyclic voltammetry and electrochemical quartz microbalance on gold electrodes. The results found in the potential region before the hydrogen evolution reaction (her) showed that ReO 3 , ReO 2 and Re 2 O 3 with different hydration grades can be formed. In the potential region where the her is occurring, either on gold or n-Si(100) the electrodeposition of metallic rhenium takes place. On both substrates, rhenium films were formed by electrolysis at constant potential and X-ray photoelectron spectroscopy technique was used to characterise these deposits. It was concluded that the electrodeposited films were of metallic rhenium and only the uppermost atomic layer contained rhenium oxide species

High-temperature extraction of rhenium from sulfuric acid solutions with trialkylamines

International Nuclear Information System (INIS)

Gladyhev, V.P.; Andreeva, N.N.; Kim, E.M.; Kovaleva, S.V.

1985-01-01

This paper attempts to determine the possibility of conducting high-temperature extraction of rhenium from sulfuric acid solutions with trialkylamines (TAA) using higher hydrocarbon-paraffin mixtures as the diluent of the extraction system. Substitution of kerosene by paraffin in the extraction system would permit decreasing the danger of fire and explosions during he extraction process. In extracting rhenium from industrial solutions with a melt of higher paraffins containing TAA and alcohols, the extraction system can be continously heated in heat exchangers through which washing sulfuric acid passes and then goes to the extractor. This permits utilizing the heat and decreases the temperature of the solutions for extraction to the optimum temperatures. Extraction of rhenium with a melt of trioctylamine in paraffin obeys the same mechanisms as high-temperature extraction of ruthenium (IV) by amines in kerosene and aromatic hydrocarbons

3.3.1. Synthesis, Spectroscopy and Structural Analysis of Technetium and Rhenium Nitrosyl Complexes

Directory of Open Access Journals (Sweden)

Terrence\tNicholson*,\tEsther\tChunb, Ashfaq\tMahmood,\tPeter\tMueller,\tAlan\tDavisona\tand\tAlun\tG.\tJones

2015-11-01

Full Text Available Here we report an overview of our synthetic, spectroscopic and structural studies of technetium and rhenium nitrosyl complexes. We review the results from various notes and short papers reported over the past 15 years and discuss their significance in terms of radiopharmaceutical design.A single new complex is reported, the ReI-NO complex [ReICl2(NO(py-N(Et-py], in which the tridentate ligand di-(2-picolyl(N-ethylamine, (py-N(Et-py, is coordinated in a meridional manner. This complex was synthesized from the reaction of the ReI-nitrosyl complex ReCl2(NO(NCMe3] and the neutral tri-amine ligand py-N(Et-py in methylene chloride under argon. The bright red species was isolated chromatographically and recrystallized from CH2Cl2/MeOH under diethylether.A review of literature values for nitrosyl complexes with various ligands bound to the coordination sitetrans- to the nitrosyl group shows only minor variations in the M-N-O bond angle.

Endocavitary treatment of craniopharyngioma cysts by 186-rhenium. Traitement endocavitaire par le rhenium 186 des kystes de craniopharyngiomes

Energy Technology Data Exchange (ETDEWEB)

Berenger, N.; Lebtahi, R.; Piketty, M.L.; Merienne, L.; Turak, B.; Bok, R.; Askienazy, S. (Hopital Sainte-Anne, 75 - Paris (France)); Munari, C. (Centre Hospitalier Universitaire, 38 - Grenoble (France))

1993-01-01

Forty-three patients with craniopharyngioma cysts were treated by intracystic injection of 186-rhenium. Leakage of colloid isotope into the CSF spaces during the ''test'' or ''therapeutic'' injection was detected by scintigraphic follow-up (15 cases/58 intracystic injections). In fact the physical characteristics of [sup 186]Re are well adapted to the requirements of treatment and, with the gamma emission, also allows early detection of leakage, avoiding irradiation of neighbouring structures. Follow-up studies revealed that craniopharyngioma cysts were effectively treated, with cessation of fluid formation, progressive shrinkage of the cysts leading to total disappearance in 14 cases (10-156 months, mean 52.5) and a considerable decrease in 13 cases (5-53 months, mean 23).

Influence of nano-cluster compounds of rhenium drugs on the activity of liver enzymes in a tumor model

Directory of Open Access Journals (Sweden)

J. V. Suponko

2010-06-01

Full Text Available Enzymes’ level in rat’s hepatocytes under Guerin's carcinoma T8 development as well as after injection of rhenium compounds and cis-platin has been studied. It has been determined that the decrease of enzymatic activity to the level of the animals of control group was observed at the simultaneous injection of cis-platin and cluster rhenium compounds in nanoliposomal and water-soluble forms. That confirms possible hepatoprotective properties of the rhenium compounds. It has been shown that hepatoprotective properties of rhenium cluster compounds mostly don’t depend on the form of their injection and are detected regardless of anticancer properties. Rhenium-platinum system with β-alanine ligand in aqueous solution, has been found. Its injection is accompanied by the hepatoprotective effect.

Synthesis and physicochemical characterization of rhenium (V) complexes with bisbenzoylthiosemicarbazones

International Nuclear Information System (INIS)

Gagieva, S.Ch.; Gutnova, N.A.; Tsaloev, A.T.; Khubulov, A.B.; Arutyunyants, A.A.; Galimov, Yu.B.

2003-01-01

Rhenium (V) complexing with mono- and bis-benzoylthiosemicarbazones is studied in dependence on hydrohalic acids concentration changes. It is determined that in media with high concentration of hydrohalic acids (6 mol/l HCl, 7 mol/l HBr) in dependence on reaction conditions stable complexes with bi- and tridentate coordination of thiosemicarbazone are formed. In the case of hydrohalic acid concentration decreasing stable binuclear and oxohydroxycomplexes are formed. Composition and structure of the compounds obtained are determined by the methods of element analysis, IR spectroscopy, conductometry. Thermal investigations of the compounds obtained are done [ru

Use of cluster rhenium substances with alkyl ligands for inhibition of the Guerin carcinoma Growth

Directory of Open Access Journals (Sweden)

O. S. Voronkova

2007-04-01

Full Text Available Quantity and quality of erythrocytes, blood haemoglobin concentration, glucose levels in the erythrocytes and plasma, content of TBA-active products in blood plasma of rats were studied during development of the Guerin carcinoma, introduction of cis-platinum and cluster rhenium substances with organic ligands. It was shown that rhenium substances had essential antioxidant effects and changed the dynamic of tumour growth. The conclusion on perspectiveness of further investigations of rhenium substances with cluster fragment and organic ligands in experiments in vivo with changed redox-status of an organism was drawn.

A study of scandia and rhenium doped tungsten matrix dispenser cathode

Science.gov (United States)

Wang, Jinshu; Li, Lili; Liu, Wei; Wang, Yanchun; Zhao, Lei; Zhou, Meiling

2007-10-01

Scandia and rhenium doped tungsten powders were prepared by solid-liquid doping combined with two-step reduction method. The experimental results show that scandia was distributed evenly on the surface of tungsten particles. The addition of scandia and rhenium could decrease the particle size of doped tungsten, for example, the tungsten powders doped with Sc 2O 3 and Re had the average size of about 50 nm in diameter. By using this kind of powder, scandia and rhenium doped tungsten matrix with the sub-micrometer sized tungsten grains was obtained. This kind of matrix exhibited good anti-bombardment insensitivity at high temperature. The emission property result showed that high space charge limited current densities of more than 60 A/cm 2 at 900 °C could be obtained for this cathode. A Ba-Sc-O multilayer about 100 nm in thickness formed at the surface of cathode after activation led to the high emission property.

Evaluation of oxide dispersion strengthened (ODS) molybdenum and molybdenum-rhenium alloys

International Nuclear Information System (INIS)

Mueller, A.J.; Bianco, R.; Buckman, R.W. Jr.

1999-01-01

Oxide dispersion strengthened (ODS) molybdenum alloys being developed for high temperature applications possess excellent high temperature strength and creep resistance. In addition they exhibit a ductile-to-brittle transition temperature (DBIT) in the worked and stress-relieved condition under longitudinal tensile load well below room temperature. However, in the recrystallized condition, the DBTT maybe near or above room temperature, depending on the volume fraction of oxide dispersion and the amount of prior work. Dilute rhenium additions (7 and 14 wt.%) to ODS molybdenum were evaluated to determine their effect on low temperature ductility. The addition of 7 wt.% rhenium to the ODS molybdenum did not significantly enhance the mechanical properties. However, the addition of 14 wt.% rhenium to the ODS molybdenum resulted in a DBTT well below room temperature in both the stress-relieved and recrystallized condition. Additionally, the tensile strength of ODS Mo-14Re is greater than the base ODS molybdenum at 1,000 to 1,250 C

Influence of cold rolling and strain rate on plastic response of powder metallurgy and chemical vapor deposition rhenium

International Nuclear Information System (INIS)

Koeppel, B.J.; Subhash, G.

1999-01-01

The plastic response of two kinds of rhenium processed via powder metallurgy (PM) and chemical vapor deposition (CVD) were investigated under uniaxial compression over a range of strain rates. The PM rhenium, further cold rolled to 50 and 80 pct of the original thickness, was also investigated to assess the influence of cold work on the plastic behavior. A strong basal texture was detected in all the preceding materials as a result of processing and cold work. Both CVD and PM rhenium exhibited an increase in yield strength and flow stress with increasing strain rate. In PM rhenium, cold work resulted in an increase in hardness and yield strength and a decrease in the work hardening rate. The deformed microstructures revealed extensive twinning in CVD rhenium. At large strains, inhomogeneous deformation mode in the form of classical cup and cone fracture was noticed

Nanograined Net-Shaped Fabrication of Rhenium Components by EB-PVD

International Nuclear Information System (INIS)

Singh, Jogender; Wolfe, Douglas E.

2004-01-01

Cost-effective net-shaped forming components have brought considerable interest into DoD, NASA and DoE. Electron beam physical vapor deposition (EB-PVD) offers flexibility in forming net-shaped components with tailored microstructure and chemistry. High purity rhenium (Re) components including rhenium-coated graphite balls, Re- plates and tubes have been successfully manufactured by EB-PVD. EB-PVD Re components exhibited sub-micron and nano-sized grains with high hardness and strength as compared to CVD. It is estimated that the cost of Re components manufactured by EB-PVD would be less than the current CVD and powder-HIP Technologies

Amine free crystal structure: The crystal structure of d(CGCGCG)2 and methylamine complex crystal

International Nuclear Information System (INIS)

Ohishi, Hirofumi; Tsukamoto, Koji; Hiyama, Yoichi; Maezaki, Naoyoshi; Tanaka, Tetsuaki; Ishida, Toshimasa

2006-01-01

We succeeded in the crystallization of d(CGCGCG) 2 and methylamine Complex. The crystal was clear and of sufficient size to collect the X-ray crystallographic data up to 1.0 A resolution using synchrotron radiation. As a result of X-ray crystallographic analysis of 2F o - F c map was much clear and easily traced. It is First time monoamine co-crystallizes with d(CGCGCG) 2 . However, methylamine was not found from the complex crystal of d(CGCGCG) 2 and methylamine. Five Mg ions were found around d(CGCGCG) 2 molecules. These Mg ions neutralized the anion of 10 values of the phosphate group of DNA with five Mg 2+ . DNA stabilized only by a metallic ion and there is no example of analyzing the X-ray crystal structure like this. Mg ion stabilizes the conformation of Z-DNA. To use monoamine for crystallization of DNA, we found that we can get only d(CGCGCG) 2 and Mg cation crystal. Only Mg cation can stabilize the conformation of Z-DNA. The method of using the monoamine for the crystallization of DNA can be applied to the crystallization of DNA of long chain of length in the future like this

Syntheses and structures of technetium(V) and rhenium(V) oxo complexes of peptide having KYC-sequence

International Nuclear Information System (INIS)

Takayama, T.; Suzuki, K.; Sekine, T.; Kudo, H.

2000-01-01

Technetium(V) and rhenium(V) oxo complexes of a peptide having a KYC-sequence such as KYCAR (H 3 L 5 ) and KYCAREPPTRTNAYQGQG-NH 2 (H 3 L 18 ) were synthesized, and structures of the complexes were characterized by spectroscopic techniques. All of the complexes were synthesized by the ligand exchange reaction of [(n-C 4 H 9 ) 4 N][MOCl 4 ] (M = 99 Tc, Re) with peptide in methanol or dimethylformamide solution. These complexes have a square pyramidal structure with an oxo ligand at the apical position. The peptide is coordinated to a metal atom through N amine of lysine. S thiol of cysteine, and N amide of tyrosine and cysteine in the equatorial plane. A lysine (CH 2 ) 4 NH 2 group of the L 5 ligand has the syn conformation with respect to metal-oxo bonding in the complex. The syn isomer was selectively formed in the ligand exchange reaction. The conversion of the syn isomer to the anti isomer was observed only for syn-[ReO(L 5 )], in which the coordination of water to the trans position of the oxo ligand was involved. (orig.)

Treatment of liver cancer with Rhenium-188 Lipiodol: Colombian experience

International Nuclear Information System (INIS)

Bernal, P.; Osorio, M.; Mendoza, M.; Esguerra, R.; Ucros, G.; Gutierrez, C.; Velez, O.; Cerquera, A.M.; Padhy, A.K.

2002-01-01

Aim:Trans-arterial Radio-conjugate therapy plays an important role in the palliative treatment of inoperable liver cancer. It also helps in reduction of the tumor to an operable state from an inoperable one. As a part of an IAEA sponsored coordinated research project, a new radiopharmaceutical, Rhenium-188 Lipiodol has been developed. The aim of this study was to establish the safety of the radiopharmaceutical and to find out the efficacy of treatment. Materials and Methods: Eight patients suffering from various forms of liver cancer (Hepatocellular carcinoma-4, Metastases from carcinoma of colon-3 and Carcinoid- 1) were treated with Rhenium -188 Lipiodol. Seven out of the eight patients were classified as ECOG- 1 and one as ECOG- 3. Labelling of Rhenium-188 with Lipiodol was carried out according to a protocol developed under the CRP and standardized in our service. Rhenium-188 Lipiodol was administered through the trans-arterial route by either selective (75%) or ultra selective (25%) hepatic arteriography. Administered therapeutic doses ranged between 170 MBq and 4181 MBq. Dosimetric evaluations were made using the IAEA developed dosimetry spreadsheet. All patients were followed up (1-5 months, average = 2 months) after treatment by clinical examination, liver function tests, haematological examinations and CT scans of liver to determine the size of hepatic tumor. Results: Rhenium-188 Lipiodol treatment was well tolerated by all patients. No immediate systemic complications were noted in any of the patients within 72 hrs. following therapy. Only two patients had mild rise in temperature in the immediate post-therapy period, which subsided subsequently. One patient who was classified as Child B and ECOG 3, developed encephalopathy on the seventh day after treatment. He died of hepatic failure. Another one present depressive syndrome, didn't accept food and died Follow-up CT scans in all the surviving (6/8) patients revealed significant reduction of the tumours

Rhenium (5) and molybdenum (5) complexes with 4',4''(5'')-ditretbutyldibenzo-24-crown-8

International Nuclear Information System (INIS)

Ashurova, N.Kh.; Yakubov, K.G.; Basitova, S.M.; Tashmukhamedova, A.K.; Sajfullina, N.Zh.

1989-01-01

Rhenium and molybdenum complexes in +5 oxidation degree with 4',4''(5'')-ditretbutyldibenzo-24-crown-8 (L) are synthesized with 75-95 % yield. Composition and structure of compounds produced are investigated using element analysis, conductometry, IR spectroscopy, thermogravimetry methods. Oxidation degree of complexer metal is determined. It is ascertained that the compound composition corresponds to the MOLX 3 formula, where M-Re, Mo; X-Cl - , Br -

Photonic Crystal Laser-Driven Accelerator Structures

International Nuclear Information System (INIS)

Cowan, B

2004-01-01

The authors discuss simulated photonic crystal structure designs for laser-driven particle acceleration. They focus on three-dimensional planar structures based on the so-called ''woodpile'' lattice, demonstrating guiding of a speed-of-light accelerating mode by a defect in the photonic crystal lattice. They introduce a candidate geometry and discuss the properties of the accelerating mode. They also discuss the linear beam dynamics in the structure present a novelmethod for focusing the beam. In addition they describe ongoing investigations of photonic crystal fiber-based structures

Crystal structure determination of Efavirenz

International Nuclear Information System (INIS)

Popeneciu, Horea; Dumitru, Ristoiu; Tripon, Carmen; Borodi, Gheorghe; Pop, Mihaela Maria

2015-01-01

Needle-shaped single crystals of the title compound, C 14 H 9 ClF 3 NO 2 , were obtained from a co-crystallization experiment of Efavirenz with maleic acid in a (1:1) ratio, using methanol as solvent. Crystal structure determination at room temperature revealed a significant anisotropy of the lattice expansion compared to the previously reported low-temperature structure. In both low- and room temperature structures the cyclopropylethynyl fragment in one of the asymmetric unit molecules is disordered. While at low-temperature only one C atom exhibits positional disorder, at room temperature the disorder is present for two C atoms of the cyclopropane ring

Determination coefficient distribution rhenium and tungsten using method extraction with solvent methyl ethyl ketone

International Nuclear Information System (INIS)

Riftanio Natapratama Hidayat; Maria Christina Prihatiningsih; Duyeh Setiawan

2015-01-01

Determination of the distribution coefficient (K d ) of the rhenium and tungsten conducted for the purpose of knowing the value of K d of the two elements. K d value determination is applied to the process of separation rhenium-188 from target of tungsten-188 for the purposes purification of radioisotopes that are made to meet the radionuclide and radiochemical purity. The K d value determination using solvent extraction with methyl ethyl ketone (MEK). Prior to the determination of K d values, determined beforehand the optimum conditions of extraction process based on the effect of agitation time, the volume of MEK, and the pH of the solution. Confirmation the results of the extraction was conducted using UV-Vis spectrophotometer with a complexing KSCN under acidic conditions and reductant SnCl 2 . The results showed that the optimum condition extraction process to feed each of 10 ppm is when the agitation for 10 minutes, the volume of MEK in 20 ml, and the pH below 5. Obtained the maximum recovery of rhenium are drawn to the organic phase as much as 9.545 ppm. However, the condition of the extraction process does not affect the migration of tungsten to the organic phase. Then the maximum K d values obtained at 2.7566 rhenium and tungsten maximum K d is 0.0873. Optimum conditions of extraction process can be further tested on radioactive rhenium and tungsten as an alternative to the separation of radioisotopes. (author)

Growth of Yb3+-doped Y2O3 single crystal rods by the micro-pulling-down method

International Nuclear Information System (INIS)

Mun, J.H.; Novoselov, A.; Yoshikawa, A.; Boulon, G.; Fukuda, T.

2005-01-01

The rare-earth sesquioxides (RE 2 O 3 , RE = Lu, Y and Sc) are very promising host crystals for advanced laser diode (LD)-pumped Yb 3+ -doped solid-state lasers due to unusual combination, almost unique of favourable structural, thermal and spectroscopic properties which are described. In spite of these favourable properties, the bulk single crystal growth technology for the rare-earth sesquioxides has not been established yet. The extremely high melting temperature at around 2400 deg. C has prevented it. However, we shall show that yttrium oxide crystals (Yb x Y 1-x ) 2 O 3 , x = 0.0, 0.005, 0.05, 0.08 and 0.15 of cylindrical shape as laser rods with 4.2 mm in diameter and 15-20 mm in length have been grown from rhenium crucibles by the micro-pulling-down method. The crystal quality characterisation of undoped Y 2 O 3 crystal was determined using X-ray rocking curve (XRC) analysis. Yb were homogeneously distributed in Y 2 O 3 host crystal

Method of fabricating patterned crystal structures

KAUST Repository

Yu, Liyang

2016-12-15

A method of manufacturing a patterned crystal structure for includes depositing an amorphous material. The amorphous material is modified such that a first portion of the amorphous thin-film layer has a first height/volume and a second portion of the amorphous thin-film layer has a second height/volume greater than the first portion. The amorphous material is annealed to induce crystallization, wherein crystallization is induced in the second portion first due to the greater height/volume of the second portion relative to the first portion to form patterned crystal structures.

Chromatographic separation of rhenium in alumina-methanol/sulfuric acid system

International Nuclear Information System (INIS)

Oguma, Koichi

1983-01-01

The adsorption behavior of a number of metals on alumina was surveyed in a methanol-(0.005 -- 0.5) M H 2 SO 4 (3 : 1 v/v) developing solvent by thin-layer chromatography. Over the acid concentration range tested, Re(VII) does not favor the alumina phase to any great extent while the most other metals are strongly adsorbed on alumina. These findings allowed to establish a column chromatographic technique for selective separation of rhenium in a methanol-0.05 M H 2 SO 4 (3 : 1 v/v) eluent. The separation technique thus established was applied to molybdenite analysis for rhenium. About 100-mg powdered sample containing ca. 100 ppm rhenium was decomposed with HNO 3 and then evaporated nearly to dryness. The residue was dissolved in NH 4 OH and the excess NH 4 OH was expelled by evaporation to dryness. The residue was dissolved in 2.5-ml 0.5 M H 2 SO 4 and 10-ml water, the insoluble materials filtered off, and the filtrate diluted to exactly 25 ml with water. A 10-ml aliquot of this solution was mixed with 30-ml methanol and the mixture was passed through a column (diameter 15 mm, bed height 30 mm) containing 5 g of alumina. The column was then washed with 20 ml of a methanol-0.05 M H 2 SO 4 (3 : 1 v/v) mixture. Rhenium was recovered from the loaded solution and the subsequent washings, and was determined spectrophotometrically with Methylene Blue as a chromogenic reagent. The values obtained from four samples of molybdenite are in good agreement with those obtained by neutron activation analysis. The relative standard deviation (n = 4; calculated from the range) was between 2.0 and 5.2 %. (author)

Superhard Rhenium/Tungsten Diboride Solid Solutions.

Science.gov (United States)

Lech, Andrew T; Turner, Christopher L; Lei, Jialin; Mohammadi, Reza; Tolbert, Sarah H; Kaner, Richard B

2016-11-02

Rhenium diboride (ReB 2 ), containing corrugated layers of covalently bonded boron, is a superhard metallic compound with a microhardness reaching as high as 40.5 GPa (under an applied load of 0.49 N). Tungsten diboride (WB 2 ), which takes a structural hybrid between that of ReB 2 and AlB 2 , where half of the boron layers are planar (as in AlB 2 ) and half are corrugated (as in ReB 2 ), has been shown not to be superhard. Here, we demonstrate that the ReB 2 -type structure can be maintained for solid solutions of tungsten in ReB 2 with tungsten content up to a surprisingly large limit of nearly 50 atom %. The lattice parameters for the solid solutions linearly increase along both the a- and c-axes with increasing tungsten content, as evaluated by powder X-ray and neutron diffraction. From micro- and nanoindentation hardness testing, all of the compositions within the range of 0-48 atom % W are superhard, and the bulk modulus of the 48 atom % solid solution is nearly identical to that of pure ReB 2 . These results further indicate that ReB 2 -structured compounds are superhard, as has been predicted from first-principles calculations, and may warrant further studies into additional solid solutions or ternary compounds taking this structure type.

Syntheses and structures of technetium(V) and rhenium(V) oxo complexes of peptide having KYC-sequence

Energy Technology Data Exchange (ETDEWEB)

Takayama, T.; Suzuki, K.; Sekine, T.; Kudo, H. [Dept. of Chemistry, Tohoku Univ., Sendai (Japan)

2000-07-01

Technetium(V) and rhenium(V) oxo complexes of a peptide having a KYC-sequence such as KYCAR (H{sub 3}L{sup 5}) and KYCAREPPTRTNAYQGQG-NH{sub 2} (H{sub 3}L{sup 18}) were synthesized, and structures of the complexes were characterized by spectroscopic techniques. All of the complexes were synthesized by the ligand exchange reaction of [(n-C{sub 4}H{sub 9}){sub 4}N][MOCl{sub 4}] (M = {sup 99}Tc, Re) with peptide in methanol or dimethylformamide solution. These complexes have a square pyramidal structure with an oxo ligand at the apical position. The peptide is coordinated to a metal atom through N{sub amine} of lysine. S{sub thiol} of cysteine, and N{sub amide} of tyrosine and cysteine in the equatorial plane. A lysine (CH{sub 2}){sub 4}NH{sub 2} group of the L{sup 5} ligand has the syn conformation with respect to metal-oxo bonding in the complex. The syn isomer was selectively formed in the ligand exchange reaction. The conversion of the syn isomer to the anti isomer was observed only for syn-[ReO(L{sup 5})], in which the coordination of water to the trans position of the oxo ligand was involved. (orig.)

Crystal Structure of the 30S Ribosomal Subunit from Thermus Thermophilus: Purification, Crystallization and Structure Determination

International Nuclear Information System (INIS)

Clemons, William M. Jr.; Brodersen, Ditlev E.; McCutcheonn, John P.; May, Joanna L.C.; Carter, Andrew P.; Morgan-Warren, Robert J.; Wimberly, Brian T.; Ramakrishnan, Venki

2001-01-01

We describe the crystallization and structure determination of the 30 S ribosomal subunit from Thermus thermophilus. Previous reports of crystals that diffracted to 10 (angstrom) resolution were used as a starting point to improve the quality of the diffraction. Eventually, ideas such as the addition of substrates or factors to eliminate conformational heterogeneity proved less important than attention to detail in yielding crystals that diffracted beyond 3 (angstrom) resolution. Despite improvements in technology and methodology in the last decade, the structure determination of the 30 S subunit presented some very challenging technical problems because of the size of the asymmetric unit, crystal variability and sensitivity to radiation damage. Some steps that were useful for determination of the atomic structure were: the use of anomalous scattering from the LIII edges of osmium and lutetium to obtain the necessary phasing signal; the use of tunable, third-generation synchrotron sources to obtain data of reasonable quality at high resolution; collection of derivative data precisely about a mirror plane to preserve small anomalous differences between Bijvoet mates despite extensive radiation damage and multi-crystal scaling; the pre-screening of crystals to ensure quality, isomorphism and the efficient use of scarce third-generation synchrotron time; pre-incubation of crystals in cobalt hexaammine to ensure isomorphism with other derivatives; and finally, the placement of proteins whose structures had been previously solved in isolation, in conjunction with biochemical data on protein-RNA interactions, to map out the architecture of the 30 S subunit prior to the construction of a detailed atomic-resolution model.

The crystal structure and twinning of neodymium gallium perovskite single crystals

International Nuclear Information System (INIS)

Ubizskii, S.B.; Vasylechko, L.O.; Savytskii, D.I.; Matkovskii, A.O.; Syvorotka, I.M.

1994-01-01

By means of X-ray structure analysis, the crystal structure of neodymium gallium perovskite (NGP) single crystals (NdGaO 3 ) being used as a substrate for HTSC film epitaxy has been refined and the position of atoms has been determined. The possibility of YBa 2 Cu 3 O 7-x film epitaxy on the plane (110) of NGP crystal as well as its advantages and pitfalls are analysed from structural data. The twinning types in the NGP crystal were established. The twinning structure of NGP substrates is found to be stable up to a temperature of 1173 K, as differentiated from the LaGaO 3 and LaAlO 3 substrates. It is intimated that the twinning in the NGP substrates oriented as (001) can result in creation of 90 degrees twin bonds in a film, and in the case of (110)-oriented plates it is possible to ignore the twinning presence in substrate completely. (author)

Mass spectrometry of rhenium complexes: a comparative study by using LDI-MS, MALDI-MS, PESI-MS and ESI-MS.

Science.gov (United States)

Petroselli, Gabriela; Mandal, Mridul Kanti; Chen, Lee Chuin; Ruiz, Gustavo T; Wolcan, Ezequiel; Hiraoka, Kenzo; Nonami, Hiroshi; Erra-Balsells, Rosa

2012-03-01

A group of rhenium (I) complexes including in their structure ligands such as CF(3)SO(3)-, CH(3)CO(2)-, CO, 2,2'-bipyridine, dipyridil[3,2-a:2'3'-c]phenazine, naphthalene-2-carboxylate, anthracene-9-carboxylate, pyrene-1-carboxylate and 1,10-phenanthroline have been studied for the first time by mass spectrometry. The probe electrospray ionization (PESI) is a technique based on electrospray ionization (ESI) that generates electrospray from the tip of a solid metal needle. In this work, mass spectra for organometallic complexes obtained by PESI were compared with those obtained by classical ESI and high flow rate electrospray ionization assisted by corona discharge (HF-ESI-CD), an ideal method to avoid decomposition of the complexes and to induce their oxidation to yield intact molecular cation radicals in gas state [M](+·) and to produce their reduction yielding the gas species [M](-·). It was found that both techniques showed in general the intact molecular ions of the organometallics studied and provided additional structure characteristic diagnostic fragments. As the rhenium complexes studied in the present work showed strong absorption in the UV-visible region, particularly at 355 nm, laser desorption ionization (LDI) mass spectrometry experiments could be conducted. Although intact molecular ions could be detected in a few cases, LDI mass spectra showed diagnostic fragments for characterization of the complexes structure. Furthermore, matrix-assisted laser desorption ionization (MALDI) mass spectra were obtained. Nor-harmane, a compound with basic character, was used as matrix, and the intact molecular ions were detected in two examples, in negative ion mode as the [M](-·) species. Results obtained with 2-[(2E)-3-(4-tert-buthylphenyl)-2-methylprop-2-enylidene] malononitrile (DCTB) as matrix are also described. LDI experiments provided more information about the rhenium complex structures than did the MALDI ones. Copyright © 2012 John Wiley & Sons, Ltd.

Influence of the acid and basic properties of rhenium oxide supported on alumina catalyst on the catalytic performance in olefin metathesis; Influence des proprietes acido-basiques de l`oxyde de rhenium supporte sur les performances catalytiques en metathese des olefines

Energy Technology Data Exchange (ETDEWEB)

Nahama, F.

1996-11-30

The aim of this work is to study the influence of the acid-basic properties of rhenium oxide supported on alumina catalyst on the catalytic performance in olefin metathesis. The literature data indicate that the environment of the active site does possess acid properties. However, the nature of the acid sites is still matter of debate. Concerning the Re O{sub x} - Al{sub 2}O{sub 3} interactions, we have shown that perrhenate ions are electrostatically absorbed on alumina. The uptake of rhenium is favoured at acidic pH (below 4), and the absorbed rhenium is in equilibrium with rhenium in solution. The results of rhenium extraction by water strongly suggest that the surface compounds of the calcined Re{sub 2}O{sub 7}/Al{sub 2}O{sub 3} materials is aluminium perrhenate. Characterization of surface acidity of the catalyst by infrared spectroscopy reveals that the initiation of the metathesis reaction is governed essentially by Lewis acidity. This strongly supports the role of Lewis acidity, which is exalted by the increase of the rhenium content and the calcination temperature. Finally, we point out by ammonia adsorption-thermodesorption a band at 1320 cm{sup -1} characteristic of the Lewis acidity of aluminium perrhenate. This result is a second indication of the presence of aluminium perrhenate on the Re{sub 2}O{sub 7}/Al{sub 2}O{sub 3} catalyst surface. (author)

Alignment structures in ferroelectric liquid crystals

Energy Technology Data Exchange (ETDEWEB)

Islam, N.U

1998-07-01

Although for many years liquid crystals were of purely scientific interest, they have now become ubiquitous in everyday life. The use of the nematic liquid crystal phase in flat panel display applications has been the main factor in this popularity. However, with the advent of the SuperTwist Nematic (STN) device, the limits to which this phase could be exploited for display applications was perhaps reached. With the discovery by Clark et al. of the Surface Stabilised Ferroelectric Liquid Crystal (SSFLC) configuration, the possibility arose of using chiral smectic liquid crystals to create large area, passively addressed, fast switching, flat panel displays. Unfortunately, the structures that form within smectic liquid crystals, and the dynamics of the switching within these, are still not fully understood. In this thesis we address the former of these, making a detailed the study of the structures that form within tilted smectic liquid crystal devices. We present here the first complete theoretical and experimental study of various different ferroelectric liquid crystal materials, where we employed theoretical models based on a simple set of assumptions to understand the behaviour of a set of increasingly complex experimental systems. We started with the simplest of these, Freely Suspended Smectic Films (FSSFs) and then worked with progressively more realistic systems in the form of homeotropically, and later, homogeneously aligned liquid crystal cells. The equilibrium structures that form get particularly complex in the last case, taking the form of tilted and chevron layering structures. In each of these cases, the predictions of the modelling are compared with our experimental results. Further, we present here the first model of the chevron cusp that seeks to include the effects of biaxiality in the S{sub C} phase. We also present a model that seeks to analyse the stability of the chevron layering structure and its relationship with tilted layers. This includes

Alignment structures in ferroelectric liquid crystals

International Nuclear Information System (INIS)

Islam, N.U.

1998-01-01

Although for many years liquid crystals were of purely scientific interest, they have now become ubiquitous in everyday life. The use of the nematic liquid crystal phase in flat panel display applications has been the main factor in this popularity. However, with the advent of the SuperTwist Nematic (STN) device, the limits to which this phase could be exploited for display applications was perhaps reached. With the discovery by Clark et al. of the Surface Stabilised Ferroelectric Liquid Crystal (SSFLC) configuration, the possibility arose of using chiral smectic liquid crystals to create large area, passively addressed, fast switching, flat panel displays. Unfortunately, the structures that form within smectic liquid crystals, and the dynamics of the switching within these, are still not fully understood. In this thesis we address the former of these, making a detailed the study of the structures that form within tilted smectic liquid crystal devices. We present here the first complete theoretical and experimental study of various different ferroelectric liquid crystal materials, where we employed theoretical models based on a simple set of assumptions to understand the behaviour of a set of increasingly complex experimental systems. We started with the simplest of these, Freely Suspended Smectic Films (FSSFs) and then worked with progressively more realistic systems in the form of homeotropically, and later, homogeneously aligned liquid crystal cells. The equilibrium structures that form get particularly complex in the last case, taking the form of tilted and chevron layering structures. In each of these cases, the predictions of the modelling are compared with our experimental results. Further, we present here the first model of the chevron cusp that seeks to include the effects of biaxiality in the S C phase. We also present a model that seeks to analyse the stability of the chevron layering structure and its relationship with tilted layers. This includes an

Development of unified X-ray fluorescent analysis to determine rhenium content in multicomponent oxide compositions

International Nuclear Information System (INIS)

Drobot, D.V.; Belyaev, A.V.; Kutvitskij, V.A.; Rysev, A.P.

1999-01-01

A procedure to prepare rhenium-containing glass-like specimens on the basis of bismuth and boron oxides is proposed. The glasses produced are studied by X-ray fluorescent analysis and routine spectrometric thiocyanate analysis. The results make it possible to determine rhenium in oxide mixtures in the range of its content 0.01 - 10% with S r = 0.03 [ru

A Study on the Trapping Characteristics of Rhenium Oxide Using Ca(OH)_2

International Nuclear Information System (INIS)

Lee, Tae-Kyo; Eun, Hee-Chul; Choi, Jung-Hoon; Lee, Ki-Rak; Han, Seung-Youb; Park, Hwan-Seo

2017-01-01

The objective of this study was to obtain basic data for trapping gaseous technetium (Tc) oxide generated from the voloxidation process in spent nuclear fuel pyroprocessing. Rhenium (Re) and Ca(OH)_2 were used as surrogates for the technetium and a trapping material, respectively. The trapping characteristics of rhenium oxide were investigated with changing temperatures and molar ratios of calcium (Ca) over rhenium, and the thermal behaviors of the trapping products were observed. The products following after the trapping test were identified as Ca(ReO_4)_2 and Ca_5Re_2O_1_2. The conversion to Ca_5Re_2O_1_2 was preferred with increasing temperatures, and the trapping products were completely converted into Ca5Re2O12 under conditions exceeding 800 ℃, or when maintained at 750 ℃ for 4 hr. The trapping efficiency at a molar ratio of 2.5 (Ca:Re=5:2) was significantly superior to that at the molar ratio of 2.

Tungsten-rhenium composite tube fabricated by CVD for application in 18000C high thermal efficiency fuel processing furnace

International Nuclear Information System (INIS)

Svedberg, R.C.; Bowen, W.W.; Buckman, R.W. Jr.

1980-04-01

Chemical Vapor Deposit (CVD) rhenium was selected as the muffle material for an 1800 0 C high thermal efficiency fuel processing furnace. The muffle is exposed to high vacuum on the heater/insulation/instrumentation side and to a flowing argon-8 V/0 hydrogen gas mixture at one atmosphere pressure on the load volume side. During operation, the muffle cycles from room temperature to 1800 0 C and back to room temperature once every 24 hours. Operational life is dependent on resistance to thermal fatigue during the high temperature exposure. For a prototypical furnace, the muffle is approximately 13 cm I.D. and 40 cm in length. A small (about one-half size) rhenium closed end tube overcoated with tungsten was used to evaluate the concept. The fabrication and testing of the composite tungsten-rhenium tube and prototypic rhenium muffle is described

Determination of rhenium (7) trace amounts by spectrophotometric titration in medium of mixed solvents

International Nuclear Information System (INIS)

Kuznetsov, V.V.; Samorukova, O.L.

1978-01-01

The method has been proposed of determining rhenium (7) microamounts by spectrophotometric titration in the medium water-dimethyl-sulphoxide with the reagent nitrochromazo. The method is based on the formation of ionic pairs K + ReO 4 - in water-organic solvents. The results of rhenium determination are satisfactory in a wide concentration range up to 0.3 mkg in 15 ml which makes the method proposed close in sensitivity to photometric methods and much better in reproducibility

Noncontact surface tension and viscosity measurements of rhenium in the liquid and undercooled states

International Nuclear Information System (INIS)

Ishikawa, Takehiko; Paradis, Paul-Francois; Yoda, Shinichi

2004-01-01

Surface tension and viscosity of liquid rhenium, which have hardly been measured due to the extremely high melting temperature of rhenium, were measured using an electrostatic levitation method combined with the oscillation drop technique. Sample position instability problems caused by the photon pressure of the heating lasers and by sample evaporation were solved by modifying the electrodes design. Good sample stability allowed the measurements of the surface tension and the viscosity over wide temperature ranges including the undercooled states. Over the 2800-3600 K interval, the surface tension of rhenium was measured as σ(T)=2.71x10 3 -0.23(T-T m ), where T m is the melting temperature, 3453 K. At T m , the datum agrees well with the literature values. Similarly, on the same temperature range, the viscosity was determined as η(T)=0.08 exp[1.33x10 5 /(RT)] (mPa s)

Monte Carlo criticality analysis of simple geometries containing tungsten-rhenium alloys engrained with uranium dioxide and uranium mononitride

International Nuclear Information System (INIS)

Webb, Jonathan A.; Charit, Indrajit

2011-01-01

Highlights: → The addition of rhenium to the tungsten matrix within W-UO 2 and W-UN CERMET materials can help reduce the risk of submersion criticality accidents while increasing the strength and ductility of tungsten based nuclear fuel elements. → The addition of rhenium up to 30 at.% to simple geometries containing W-UO 2 mixtures can increase the critical mass by 65 kg. → The addition of rhenium up to 30 at.% to simple geometries containing W-UN mixtures can increase the critical mass by 22 kg. → The addition of rhenium by up to 30 at.% to simple geometries containing W-UO 2 mixtures can reduce the change in reactivity change due to water submersion by $5.07. → The addition of rhenium by up to 30 at.% to simple geometries containing W-UN mixtures can reduce the change in reactivity due to water submersion by $3.24. - Abstract: The critical mass and dimensions of simple geometries containing highly enriched uranium dioxide (UO 2 ) and uranium mononitride (UN) encapsulated in tungsten-rhenium alloys are determined using MCNP5 criticality calculations. Spheres as well as cylinders with length to radius ratios of 1.82 are computationally built to consist of 60 vol.% fuel and 40 vol.% metal matrix. Within the geometries, the uranium is enriched to 93 wt.% uranium-235 and the rhenium content within the metal alloy was modeled over the range of 0-30 at.%. The spheres containing UO 2 were determined to have a critical radius of 18.29-19.11 cm and a critical mass ranging from 366 kg to 424 kg. The cylinders containing UO 2 were found to have a critical radius ranging from 17.07 cm to 17.84 cm with a corresponding critical mass of 406-471 kg. Spheres engrained with UN were determined to have a critical radius ranging from 14.82 cm to 15.19 cm and a critical mass between 222 kg and 242 kg. Cylinders which were engrained with UN were determined to have a critical radius ranging from 13.81 cm to 14.15 cm and a corresponding critical mass of 245-267 kg. The critical

Optically induced structural phase transitions in ion Coulomb crystals

DEFF Research Database (Denmark)

Horak, Peter; Dantan, Aurelien Romain; Drewsen, Michael

2012-01-01

We investigate numerically the structural dynamics of ion Coulomb crystals confined in a three-dimensional harmonic trap when influenced by an additional one-dimensional optically induced periodical potential. We demonstrate that transitions between thermally excited crystal structures, such as b......We investigate numerically the structural dynamics of ion Coulomb crystals confined in a three-dimensional harmonic trap when influenced by an additional one-dimensional optically induced periodical potential. We demonstrate that transitions between thermally excited crystal structures...

Effect of rhenium irradiations on the mechanical properties of tungsten for nuclear fusion applications

Energy Technology Data Exchange (ETDEWEB)

Khan, Aneeqa, E-mail: aneeqa.khan-3@postgrad.manchester.ac.uk [School of Mechanical, Aerospace and Civil Engineering, The University of Manchester, M13 9PL (United Kingdom); Elliman, Robert; Corr, Cormac [Research School of Physics and Engineering, The Australian National University, Canberra, ACT 2601 (Australia); Lim, Joven J.H.; Forrest, Andrew [School of Materials, The University of Manchester, M13 9PL (United Kingdom); Mummery, Paul [School of Mechanical, Aerospace and Civil Engineering, The University of Manchester, M13 9PL (United Kingdom); Evans, Llion M. [Culham Centre for Fusion Energy, Culham Science Centre, Abingdon, Oxon, OX14 3DB (United Kingdom)

2016-08-15

As-received and annealed tungsten samples were irradiated at a temperature of 400 °C with Re and W ions to peak concentrations of 1600 appm (atomic parts per million) and damage levels of 40 dpa (displacements per atom). Mechanical properties were investigated using nanoindentation, and the orientation and depth dependence of irradiation damage was investigated using Electron Back Scatter Diffraction (EBSD). Following irradiation there was a 13% increase in hardness in the as received sheet and a 23% increase in the annealed material for both tungsten and rhenium irradiation. The difference between the tungsten and rhenium irradiated samples was negligible, suggesting that for the concentrations and damage levels employed, the presence of rhenium does not have a significant effect on the hardening mechanism. Energy dependent EBSD of annealed samples provided information about the depth distribution of the radiation damage in individual tungsten grains and confirmed that the radiation damage is orientation dependant.

Low-leakage superconducting tunnel junctions with a single-crystal Al{sub 2}O{sub 3} barrier

Energy Technology Data Exchange (ETDEWEB)

Oh, S [National Institute of Standards and Technology, Boulder, CO 80305 (United States); Department of Physics, University of Illinois, Urbana, IL 61801 (United States); Cicak, K; Osborn, K D; Simmonds, R W; Pappas, D P [National Institute of Standards and Technology, Boulder, CO 80305 (United States); McDermott, R; Cooper, K B; Steffen, M; Martinis, J M [University of California, Santa Barbara, CA 93106 (United States)

2005-10-01

We have developed a two-step growth scheme for single-crystal Al{sub 2}O{sub 3} tunnel barriers. The barriers are epitaxially grown on single-crystal rhenium (Re) base electrodes that are grown epitaxially on a sapphire substrate, while polycrystalline Al is used as the top electrode. We show that by first growing an amorphous aluminium (Al) oxide layer at room temperature and crystallizing it at a high temperature in oxygen environment, a morphologically intact single-crystal Al{sub 2}O{sub 3} layer is obtained. Tunnel junctions fabricated from these trilayers show very low subgap leakage current. This single-crystal Al{sub 2}O{sub 3} junction may open a new venue for coherent quantum devices.

What makes a crystal structure report valid?

NARCIS (Netherlands)

Spek, Anthony L.|info:eu-repo/dai/nl/156517566

2018-01-01

Single crystal X-ray crystallography has developed into a unique, highly automated and accessible tool to obtain detailed information on molecular structures. Proper archival makes that referees, readers and users of the results of reported crystal structures no longer need to depend solely on the

SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURES ...

African Journals Online (AJOL)

B. S. Chandravanshi

ABSTRACT. Reaction of [VO(acac)2] (acac = acetylacetonate) with ... Single crystal X-ray structural studies indicate that the hydrazone ligands coordinate to ..... Molecular structure of complex (1) at 30% probability displacement. Figure 4.

Tetrathiafulvalene-based azine ligands for anion and metal cation coordination

Directory of Open Access Journals (Sweden)

Awatef Ayadi

2015-08-01

Full Text Available The synthesis and full characterization of two tetrathiafulvalene-appended azine ligands, namely 2-([2,2’-bi(1,3-dithiolylidene]-4-yl-6-((2,4-dinitrophenylhydrazonomethylpyridine (L1 and 5-([2,2’-bi(1,3-dithiolylidene]-4-yl-2-((2,4-dinitrophenylhydrazonomethylpyridine (L2 are described. The crystal structure of ligand L1 indicates that the ligand is completely planar with the presence of a strong intramolecular N3–H3···O1 hydrogen bonding. Titration experiments with inorganic anions showed that both ligands are suitable candidates for the sensing of fluoride anions. Ligand L2 was reacted with a Re(I cation to yield the corresponding rhenium tricarbonyl complex 3. In the crystal structure of the newly prepared electroactive rhenium complex the TTF is neutral and the rhenium cation is hexacoordinated. The electrochemical behavior of the three compounds indicates that they are promising for the construction of crystalline radical cation salts.

Crystal structure from one-electron theory

DEFF Research Database (Denmark)

Skriver, H. L.

1985-01-01

The authors have studied the crystal structure of all the 3d, 4d, and 5d transition metals at zero pressure and temperature by means of the linear muffin-tin orbital method and Andersen's force theorem. They find that, although the structural energy differences seem to be overestimated by the the......The authors have studied the crystal structure of all the 3d, 4d, and 5d transition metals at zero pressure and temperature by means of the linear muffin-tin orbital method and Andersen's force theorem. They find that, although the structural energy differences seem to be overestimated...

Submersion criticality safety of tungsten-rhenium urania cermet fuel for space propulsion and power applications

Energy Technology Data Exchange (ETDEWEB)

Craft, A.E., E-mail: aaron.craft@inl.gov [Center for Space Nuclear Research (CSNR), INL, Idaho Falls, ID (United States); O’Brien, R.C., E-mail: Robert.OBrien@inl.gov [Center for Space Nuclear Research (CSNR), INL, Idaho Falls, ID (United States); Howe, S.D., E-mail: Steven.Howe@inl.gov [Center for Space Nuclear Research (CSNR), INL, Idaho Falls, ID (United States); King, J.C., E-mail: kingjc@mines.edu [Nuclear Science and Engineering Program, Metallurgical and Materials Engineering Department, Colorado School of Mines, Golden, CO 80401 (United States)

2014-07-01

Highlights: • Criticality safety studies consider a generic space nuclear reactor in reentry scenarios. • Describes the submersion criticality behavior for a reactor fueled with a tungsten cermet fuel. • Study considers effects of varying fuel content, geometry, and other conditions. - Abstract: Nuclear thermal rockets are the preferred propulsion technology for a manned mission to Mars, and tungsten–uranium oxide cermet fuels could provide significant performance and cost advantages for nuclear thermal rockets. A nuclear reactor intended for use in space must remain subcritical before and during launch, and must remain subcritical in launch abort scenarios where the reactor falls back to Earth and becomes submerged in terrestrial materials (including seawater, wet sand, or dry sand). Submersion increases reflection of neutrons and also thermalizes the neutron spectrum, which typically increases the reactivity of the core. This effect is typically very significant for compact, fast-spectrum reactors. This paper provides a submersion criticality safety analysis for a representative tungsten/uranium oxide fueled reactor with a range of fuel compositions. Each submersion case considers both the rhenium content in the matrix alloy and the uranium oxide volume fraction in the cermet. The inclusion of rhenium significantly improves the submersion criticality safety of the reactor. While increased uranium oxide content increases the reactivity of the core, it does not significantly affect the submersion behavior of the reactor. There is no significant difference in submersion behavior between reactors with rhenium distributed within the cermet matrix and reactors with a rhenium clad in the coolant channels. The combination of the flooding of the coolant channels in submersion scenarios and the presence of a significant amount of spectral shift absorbers (i.e. high rhenium concentration) further decreases reactivity for short reactor cores compared to longer cores.

Separation of tungsten and rhenium on alumina

Directory of Open Access Journals (Sweden)

MILOVAN SM. STOILJKOVIC

2004-09-01

Full Text Available The conditions for the efficient separation of tungsten(VI and rhenium (VII on alumina were established. The distribution coefficients Kd for tungstate and perrhenate anions, as well as the separation factors a (a = KdWO42-/Kd ReO4- were determined using hydrochloric or nitric acid as the aqueous media. A solution of sodium chloride in the pH range 2–6 was also examined. Under all the tested experimental conditions, alumina is a much better adsorbent for tungsten than for rhenium. The obtained results indicated that the best separation of these two elements is achieved when 0.01– 0.1 mol dm-3 HCl or 1.0 mol dm-3 HNO3 are used as the aqueous media. If NaCl is used as the aqueous phase, the best separation is achieved with 0.20 mol dm-3 NaCl, pH 4–6. Under these experimental conditions, the breakthrough and saturation capacities of alumina for tungsten at pH 4 are 17 and 26 mg W/g Al2O3, respectively. With increasing pH, these values decrease. Thus, at pH 6 they are only 4 and 13 mg W/g Al2O3, respectively.

SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE ...

African Journals Online (AJOL)

Preferred Customer

Reaction of [MoO2(acac)2] (where acac = acetylacetonate) with N'-(2-hydroxy-4- ... Single crystal X-ray structural studies indicate that the hydrazone ligand coordinates .... Molecular structure of the complex at 30% probability displacement.

Crystal structure refinement with SHELXL

Energy Technology Data Exchange (ETDEWEB)

Sheldrick, George M., E-mail: gsheldr@shelx.uni-ac.gwdg.de [Department of Structural Chemistry, Georg-August Universität Göttingen, Tammannstraße 4, Göttingen 37077 (Germany)

2015-01-01

New features added to the refinement program SHELXL since 2008 are described and explained. The improvements in the crystal structure refinement program SHELXL have been closely coupled with the development and increasing importance of the CIF (Crystallographic Information Framework) format for validating and archiving crystal structures. An important simplification is that now only one file in CIF format (for convenience, referred to simply as ‘a CIF’) containing embedded reflection data and SHELXL instructions is needed for a complete structure archive; the program SHREDCIF can be used to extract the .hkl and .ins files required for further refinement with SHELXL. Recent developments in SHELXL facilitate refinement against neutron diffraction data, the treatment of H atoms, the determination of absolute structure, the input of partial structure factors and the refinement of twinned and disordered structures. SHELXL is available free to academics for the Windows, Linux and Mac OS X operating systems, and is particularly suitable for multiple-core processors.

Two-dimensional photonic crystal accelerator structures

Directory of Open Access Journals (Sweden)

Benjamin M. Cowan

2003-10-01

Full Text Available Photonic crystals provide a method of confining a synchronous speed-of-light mode in an all-dielectric structure, likely a necessary feature in any optical accelerator. We explore computationally a class of photonic crystal structures with translational symmetry in a direction transverse to the electron beam. We demonstrate synchronous waveguide modes and discuss relevant parameters of such modes. We then explore how accelerator parameters vary as the geometry of the structure is changed and consider trade-offs inherent in the design of an accelerator of this type.

Separation of Rhenium from Lead-Rich Molybdenite Concentrate via Hydrochloric Acid Leaching Followed by Oxidative Roasting

Directory of Open Access Journals (Sweden)

Guanghui Li

2016-11-01

Full Text Available Lead-rich molybdenite is a typical rhenium-bearing molybdenum resource in China, which has not been efficiently utilized due to its high contents of lead and gangue minerals. In this study, hydrochloric acid was used for preliminarily removing lead and calcite from a lead-rich molybdenite concentrate. Oxidative roasting-ammonia leaching was then carried out for separation of rhenium and extraction of molybdenum. The hydrochloric acid leaching experiments revealed that 93.6% Pb and 97.4% Ca were removed when the leaching was performed at 95 °C for 10 min with HCl concentration of 8 wt. % and liquid-solid ratio of 5 (mL/g. The results of direct oxidative roasting indicated that 89.3% rhenium was volatilized from the raw concentrate after roasting at 600 °C for 120 min in air. In contrast, the rhenium volatilization was enhanced distinctly to 98.0% after the acid-leached concentrate (leaching residue was roasted at 550 °C for 100 min. By the subsequent ammonia leaching, 91.5% molybdenum was leached out from the calcine produced from oxidative roasting of the acid-leached concentrate, while only 79.3% Mo was leached from the calcine produced by roasting molybdenite concentrate without pretreatment.

Photonics of liquid-crystal structures: A review

Energy Technology Data Exchange (ETDEWEB)

Palto, S. P., E-mail: palto@online.ru; Blinov, L M; Barnik, M I; Lazarev, V V; Umanskii, B A; Shtykov, N M [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

2011-07-15

The original results of studies of the electro-optical and laser effects which have been performed at the Laboratory of Liquid Crystals of the Institute of Crystallography, Russian Academy of Sciences, over the last few years are reviewed. Cholesteric liquid crystals as vivid representatives of photonic structures and their behavior in an electric field are considered in detail. The formation of higher harmonics in the periodic distribution of the director field in a helical liquid crystal structure and, correspondingly, the new (anharmonic) mode of electro-optical effects are discussed. Another group of studies is devoted to bistable light switching by an electric field in chiral nematics. Polarization diffraction gratings controlled by an electric field are also considered. The results of studies devoted to microlasers on various photonic structures with cholesteric and nematic liquid crystals are considered in detail. Particular attention is given to the new regime: leaky-mode lasing. Designs of liquid crystal light amplifiers and their polarization, field, and spectral characteristics are considered in the last section.

Effect of operational parameters and internal recycle on rhenium solvent extraction from leach liquors using a mixer-settler

Directory of Open Access Journals (Sweden)

Mostafa Hosseinzadeh

2014-06-01

Full Text Available The extraction of rhenium from molybdenite roasting dust leach solution was performed using a mixer-settler extractor by tributyl phosphate (TBP diluted in kerosene as the extractant. In the single-stage extraction experiments, effect of the aqueous to organic phase ratios, Qa/Qo, and the number of extraction stages, N, on the rhenium extraction was studied. It was found that using the phase ratio of 1:1 in a two-stage extraction, 87.5% depletion of rhenium was obtained. The comparison of experimental results with the continuous co-current extraction showed a good agreement. The effect of internal recycle of organic phase was investigated in the phase ratio of 1:1 by changing the flow rate ratio of recycle-to-fresh organic phase, Qro/Qfo. The optimum performance was achieved in the phase ratio, Qro/Qfo, equal to 3:7. It was found that improvement in the performance of the mixer-settler for the rhenium-TBP system can be obtained in the phase ratio of 1:1when Qro/Qfo = 3:7.

A Study on the Trapping Characteristics of Rhenium Oxide Using Ca(OH){sub 2}

Energy Technology Data Exchange (ETDEWEB)

Lee, Tae-Kyo; Eun, Hee-Chul; Choi, Jung-Hoon; Lee, Ki-Rak; Han, Seung-Youb; Park, Hwan-Seo [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2017-01-15

The objective of this study was to obtain basic data for trapping gaseous technetium (Tc) oxide generated from the voloxidation process in spent nuclear fuel pyroprocessing. Rhenium (Re) and Ca(OH){sub 2} were used as surrogates for the technetium and a trapping material, respectively. The trapping characteristics of rhenium oxide were investigated with changing temperatures and molar ratios of calcium (Ca) over rhenium, and the thermal behaviors of the trapping products were observed. The products following after the trapping test were identified as Ca(ReO{sub 4}){sub 2} and Ca{sub 5}Re{sub 2}O{sub 12}. The conversion to Ca{sub 5}Re{sub 2}O{sub 12} was preferred with increasing temperatures, and the trapping products were completely converted into Ca5Re2O12 under conditions exceeding 800 ℃, or when maintained at 750 ℃ for 4 hr. The trapping efficiency at a molar ratio of 2.5 (Ca:Re=5:2) was significantly superior to that at the molar ratio of 2.

Electronic structures and properties of the rhenium alkoxy derivatives Re2O3(OMe)6, Re4O6(OMe)12, and ReMoO2(OMe)7

International Nuclear Information System (INIS)

Ermakov, A.I.; Belousov, V.V.; Drobot, D.V.; Shcheglov, P.A.

2006-01-01

The geometrical structures, charge distributions, dipole moments, frequencies of normal vibrations, NMR spectra, and total energies of the chemical bonds for the rhenium alkoxy derivatives Re 2 O 3 (OMe) 6 , Re 4 O 6 (OMe) 12 , and ReMoO 2 (OMe) 7 were calculated by the DFT-B3LYP and Hartree-Fock ab initio methods based on the effective core potential theory (LANL2DZ approximation) and the semiempirical PM3(tm) method. Two optimized structures of Re 2 O 3 (OMe) 6 with close energies were found to substantially differ in geometry, 1 H, 13 C, and 17 O NMR spectra, and dipole moment. Various characteristics of the electronic structures and the trans-effect of the ligands in the compounds under consideration were discussed [ru

Comparison of multiple crystal structures with NMR data for engrailed homeodomain

Energy Technology Data Exchange (ETDEWEB)

Religa, Tomasz L. [MRC Centre for Protein Engineering (United Kingdom)], E-mail: tlr25@mrc-lmb.cam.ac.uk

2008-03-15

Two methods are currently available to solve high resolution protein structures-X-ray crystallography and nuclear magnetic resonance (NMR). Both methods usually produce highly similar structures, but small differences between both solutions are always observed. Here the raw NMR data as well as the solved NMR structure were compared to the multiple crystal structures solved for the WT 60 residue three helix bundle engrailed homeodomain (EnHD) and single point mutants. There was excellent agreement between TALOS-predicted and crystal structure-observed dihedral angles and a good agreement for the {sup 3}J(H{sup N}H{sup {alpha}}) couplings for the multiple crystal structures. Around 1% of NOEs were violated for any crystal structure, but no NOE was inconsistent with all of the crystal structures. Violations usually occurred for surface residues or for residues for which multiple discreet conformations were observed between the crystal structures. Comparison of the disorder shown in the multiple crystal structures shows little correlation with dynamics under native conditions for this protein.

Precipitation in solid solution and structural transformations in single crystals of high rhenium ruthenium-containing nickel superalloys at high-temperature creep

Energy Technology Data Exchange (ETDEWEB)

Alekseev, A.A.; Petrushin, N.V.; Zaitsev, D.V.; Treninkov, I.A.; Filonova, E.V. [All-Russian Scientific Research Institute of Aviation Materials (VIAM), Moscow (Russian Federation)

2010-07-01

The phase composition and structure of single crystals of two superalloys (alloy 1 and alloy 2) were investigated in this work. For alloy 1 (Re - 9 wt%) the kinetics of precipitation in solid solution at heat treatment (HT) was investigated. TEM and X-Ray examinations have revealed that during HT rhombic phase (R-phase) precipitation (Immm class (BCR)) occurs. The TTT diagram is plotted, it contains the time-temperature area of the existence of R-phase particles. The element content of R-phase is identified (at. %): Re- 51.5; Co- 23.5; Cr- 14.8; Mo- 4.2; W- 3.3; Ta- 2.7. For alloy 2 (Re - 6.5 wt %, Ru - 4 wt %) structural transformations at high-temperature creep are investigated. By dark-field TEM methods it is established, that in alloy 2 the additional phase with a rhombic lattice is formed during creep. Particles of this phase precipitate in {gamma}-phase and their quantity increases during high-temperature creep. It is revealed that during creep 3-D dislocation network is formed in {gamma}-phase. At the third stage of creep the process of inversion structure formation is observed in the alloy, i.e. {gamma}'-phase becomes a matrix. Thus during modeling creep the volume fraction of {gamma}'-phase in the samples increases from 30% (at creep duration of 200 hrs) up to 55% (at 500 hrs). The processes of structure formation in Re and Ru-containing nickel superalloys are strongly affected by decomposition of solid solution during high-temperature creep that includes precipitation of additional TCP-phases. (orig.)

Structure analysis on synthetic emerald crystals

Science.gov (United States)

Lee, Pei-Lun; Lee, Jiann-Shing; Huang, Eugene; Liao, Ju-Hsiou

2013-05-01

Single crystals of emerald synthesized by means of the flux method were adopted for crystallographic analyses. Emerald crystals with a wide range of Cr3+-doping content up to 3.16 wt% Cr2O3 were examined by X-ray single crystal diffraction refinement method. The crystal structures of the emerald crystals were refined to R 1 (all data) of 0.019-0.024 and w R 2 (all data) of 0.061-0.073. When Cr3+ substitutes for Al3+, the main adjustment takes place in the Al-octahedron and Be-tetrahedron. The effect of substitution of Cr3+ for Al3+ in the beryl structure results in progressively lengthening of the Al-O distance, while the length of the other bonds remains nearly unchanged. The substitution of Cr3+ for Al3+ may have caused the expansion of a axis, while keeping the c axis unchanged in the emerald lattice. As a consequence, the Al-O-Si and Al-O-Be bonding angles are found to decrease, while the angle of Si-O-Be increases as the Al-O distance increases during the Cr replacement.

A tungsten-rhenium interatomic potential for point defect studies

Science.gov (United States)

Setyawan, Wahyu; Gao, Ning; Kurtz, Richard J.

2018-05-01

A tungsten-rhenium (W-Re) classical interatomic potential is developed within the embedded atom method interaction framework. A force-matching method is employed to fit the potential to ab initio forces, energies, and stresses. Simulated annealing is combined with the conjugate gradient technique to search for an optimum potential from over 1000 initial trial sets. The potential is designed for studying point defects in W-Re systems. It gives good predictions of the formation energies of Re defects in W and the binding energies of W self-interstitial clusters with Re. The potential is further evaluated for describing the formation energy of structures in the σ and χ intermetallic phases. The predicted convex-hulls of formation energy are in excellent agreement with ab initio data. In pure Re, the potential can reproduce the formation energies of vacancies and self-interstitial defects sufficiently accurately and gives the correct ground state self-interstitial configuration. Furthermore, by including liquid structures in the fit, the potential yields a Re melting temperature (3130 K) that is close to the experimental value (3459 K).

Studies on growth, crystal structure and characterization of novel organic nicotinium trifluoroacetate single crystals

Energy Technology Data Exchange (ETDEWEB)

Dhanaraj, P.V. [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India); Rajesh, N.P., E-mail: rajeshnp@hotmail.com [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India); Sundar, J. Kalyana; Natarajan, S. [Department of Physics, Madurai Kamaraj University, Madurai 625 021 (India); Vinitha, G. [Department of Physics, Crescent Engineering College, Chennai 600 048 (India)

2011-09-15

Highlights: {yields} Good quality crystals of nicotinium trifluoroacetate in monoclinic system were grown for first time. {yields} Nicotinium trifluoroacetate crystal exhibits third order nonlinear optical properties. {yields} The optical spectrum of nicotinium trifluoroacetate crystal reveals the wide transmission in the entire range with cutoff wavelength at 286 nm. {yields} Nicotinium trifluoroacetate is a low dielectric constant material. - Abstract: An organic material, nicotinium trifluoroacetate (NTF) was synthesized and single crystals in monoclinic system were grown from aqueous solution for the first time. Its solubility and metastable zone width were estimated. The crystal structure of NTF was analyzed to reveal the molecular arrangements and the formation of hydrogen bonds in the crystal. High-resolution X-ray diffraction rocking curve measurements were performed to analyze the structural perfection of the grown crystals. Functional groups in NTF were identified by Fourier transform infrared spectral analysis. Thermal behaviour and stability of NTF were studied by thermogravimetric and differential thermal analysis and differential scanning calorimetry. Mechanical and dielectric properties of NTF crystals were analyzed. Optical studies reveal that NTF crystals are transparent in the wavelength range 286-1100 nm. The third order nonlinear optical parameters of NTF were derived by the Z-scan technique.

The Crystal Structures of Two Novel Cadmium-Picolinic Acid ...

African Journals Online (AJOL)

The crystal structures of two novel cadmium-picolinic acid complexes grown in aqueous solutions at selected pH values are reported. The structures are compared to expected solution species under the same conditions. The crystal structure of complex 1 exhibits a seven coordinate structure which contains a protonated ...

Band structures in fractal grading porous phononic crystals

Science.gov (United States)

Wang, Kai; Liu, Ying; Liang, Tianshu; Wang, Bin

2018-05-01

In this paper, a new grading porous structure is introduced based on a Sierpinski triangle routine, and wave propagation in this fractal grading porous phononic crystal is investigated. The influences of fractal hierarchy and porosity on the band structures in fractal graidng porous phononic crystals are clarified. Vibration modes of unit cell at absolute band gap edges are given to manifest formation mechanism of absolute band gaps. The results show that absolute band gaps are easy to form in fractal structures comparatively to the normal ones with the same porosity. Structures with higher fractal hierarchies benefit multiple wider absolute band gaps. This work provides useful guidance in design of fractal porous phononic crystals.

Construction of crystal structure prototype database: methods and applications.

Science.gov (United States)

Su, Chuanxun; Lv, Jian; Li, Quan; Wang, Hui; Zhang, Lijun; Wang, Yanchao; Ma, Yanming

2017-04-26

Crystal structure prototype data have become a useful source of information for materials discovery in the fields of crystallography, chemistry, physics, and materials science. This work reports the development of a robust and efficient method for assessing the similarity of structures on the basis of their interatomic distances. Using this method, we proposed a simple and unambiguous definition of crystal structure prototype based on hierarchical clustering theory, and constructed the crystal structure prototype database (CSPD) by filtering the known crystallographic structures in a database. With similar method, a program structure prototype analysis package (SPAP) was developed to remove similar structures in CALYPSO prediction results and extract predicted low energy structures for a separate theoretical structure database. A series of statistics describing the distribution of crystal structure prototypes in the CSPD was compiled to provide an important insight for structure prediction and high-throughput calculations. Illustrative examples of the application of the proposed database are given, including the generation of initial structures for structure prediction and determination of the prototype structure in databases. These examples demonstrate the CSPD to be a generally applicable and useful tool for materials discovery.

Construction of crystal structure prototype database: methods and applications

International Nuclear Information System (INIS)

Su, Chuanxun; Lv, Jian; Wang, Hui; Wang, Yanchao; Ma, Yanming; Li, Quan; Zhang, Lijun

2017-01-01

Crystal structure prototype data have become a useful source of information for materials discovery in the fields of crystallography, chemistry, physics, and materials science. This work reports the development of a robust and efficient method for assessing the similarity of structures on the basis of their interatomic distances. Using this method, we proposed a simple and unambiguous definition of crystal structure prototype based on hierarchical clustering theory, and constructed the crystal structure prototype database (CSPD) by filtering the known crystallographic structures in a database. With similar method, a program structure prototype analysis package (SPAP) was developed to remove similar structures in CALYPSO prediction results and extract predicted low energy structures for a separate theoretical structure database. A series of statistics describing the distribution of crystal structure prototypes in the CSPD was compiled to provide an important insight for structure prediction and high-throughput calculations. Illustrative examples of the application of the proposed database are given, including the generation of initial structures for structure prediction and determination of the prototype structure in databases. These examples demonstrate the CSPD to be a generally applicable and useful tool for materials discovery. (paper)

sup(99m)Tc-sulfur-rhenium-colloid and 111In-indiumcitrate in the bone marrow scintigraphy

International Nuclear Information System (INIS)

Glaubitt, D.; Haberland, K.; Knoch, K.; Fejer, F.L.; Zachariah, S.; Staedtische Krankenanstalten Krefeld

1975-01-01

Bone marrow scintigraphy using 111 In-Indium-citrate and sup(99m)Tc-sulfur rhenium colloid was compared with each other in 6 male and 3 female patients. Our results in all patients were in favour of 111 In-citrate which caused a better delineation of morphological details than sup(99m)Tc-sulfur rhenium colloid did. In the first days after intravenous administration of 111 In-citrate, radioindium accumulated markedly in the pudendal region, this finding being more distinct in male patients than in female ones. On account of these results a considerable radiation dose has to be assumed in bone marrow scintigraphy using 111 In-citrate as long as the absorbed dose from 111 In has not been estimated under consideration of the radioindium accumulation in the pudendal region. 111 In-citrate should be applied in bone marrow scanning only exceptionally and sup(99m)Tc-sulfur rhenium colloid be preferred in the routine diagnostics of bone marrow. (orig.) [de

Crystal engineering of ibuprofen compounds: From molecule to crystal structure to morphology prediction by computational simulation and experimental study

Science.gov (United States)

Zhang, Min; Liang, Zuozhong; Wu, Fei; Chen, Jian-Feng; Xue, Chunyu; Zhao, Hong

2017-06-01

We selected the crystal structures of ibuprofen with seven common space groups (Cc, P21/c, P212121, P21, Pbca, Pna21, and Pbcn), which was generated from ibuprofen molecule by molecular simulation. The predicted crystal structures of ibuprofen with space group P21/c has the lowest total energy and the largest density, which is nearly indistinguishable with experimental result. In addition, the XRD patterns for predicted crystal structure are highly consistent with recrystallization from solvent of ibuprofen. That indicates that the simulation can accurately predict the crystal structure of ibuprofen from the molecule. Furthermore, based on this crystal structure, we predicted the crystal habit in vacuum using the attachment energy (AE) method and considered solvent effects in a systematic way using the modified attachment energy (MAE) model. The simulation can accurately construct a complete process from molecule to crystal structure to morphology prediction. Experimentally, we observed crystal morphologies in four different polarity solvents compounds (ethanol, acetonitrile, ethyl acetate, and toluene). We found that the aspect ratio decreases of crystal habits in this ibuprofen system were found to vary with increasing solvent relative polarity. Besides, the modified crystal morphologies are in good agreement with the observed experimental morphologies. Finally, this work may guide computer-aided design of the desirable crystal morphology.

Rhenium(5) and molybdenum(5) complexes with 4',4[sup (]5[sup )]-divaleryldibenzo-18-crown-6. Kompleksnye soedineniya reniya(5) i molibdena(5) s 4',4[sup (]5[sup )]-divalerildibenzo-18-kraun-6

Energy Technology Data Exchange (ETDEWEB)

Ashurova, N Kh; Yakubov, K G; Tashmukhamedova, A K; Basitova, S M [Tadzhikskij Gosudarstvennyj Univ., Dushanbe (Tajikistan)

1993-02-01

Methods for synthesizing oxohalide complexes of rhenium and molybdenum with +5 oxidation degree with 4',4[sup (5)]-divaleryldibenzo-18-crown-6 were developed. Content and composition of prepared compounds were investigated by the methods of element analysis, crystal optics, conductometry, IR spectroscopy in the near and far regions, thermogravimetry. Oxidation degree of the complex-forming metal was determined. It was established that composition of the compounds coressponded to the general formula MOLX [sub [center dot

Isolation, crystallization and crystal structure determination of bovine kidney Na(+),K(+)-ATPase.

Science.gov (United States)

Gregersen, Jonas Lindholt; Mattle, Daniel; Fedosova, Natalya U; Nissen, Poul; Reinhard, Linda

2016-04-01

Na(+),K(+)-ATPase is responsible for the transport of Na(+) and K(+) across the plasma membrane in animal cells, thereby sustaining vital electrochemical gradients that energize channels and secondary transporters. The crystal structure of Na(+),K(+)-ATPase has previously been elucidated using the enzyme from native sources such as porcine kidney and shark rectal gland. Here, the isolation, crystallization and first structure determination of bovine kidney Na(+),K(+)-ATPase in a high-affinity E2-BeF3(-)-ouabain complex with bound magnesium are described. Crystals belonging to the orthorhombic space group C2221 with one molecule in the asymmetric unit exhibited anisotropic diffraction to a resolution of 3.7 Å with full completeness to a resolution of 4.2 Å. The structure was determined by molecular replacement, revealing unbiased electron-density features for bound BeF3(-), ouabain and Mg(2+) ions.

Crystal structure study of new lanthanide silicates with silico-carnotite structure

International Nuclear Information System (INIS)

Piccinelli, F.; Lausi, A.; Speghini, A.; Bettinelli, M.

2012-01-01

The crystal structures of new rare earth-based silicate compounds (Ca 3 Eu 2 Si 3 O 12 , Ca 3 Gd 2 Si 3 O 12 , Ca 3 Dy 2 Si 3 O 12 , Ca 3 Er 2 Si 3 O 12 and Ca 3 Lu 2 Si 3 O 12 ) have been determined using powder X-ray diffraction. From Rietveld refinement calculations on the collected powder patterns we observe a different distribution of the rare earth ions on the three available crystal sites characterized by different coordination numbers, depending on the ionic radius of the rare earth ion. The reasons of the instability of the silico-carnotite structure for lanthanide ions larger than Eu 3+ have been deduced. In addition, in order to detect crystal phase transitions, the powder patterns of Ca 3 Eu 2 Si 3 O 12 and Ca 3 Sm 2 Si 3 O 12 samples have been collected as a function of the temperature (RT-1000 °C range), but no phase transitions have been observed. - Graphical abstract: Synchrotron X-ray diffraction allows us the accurate determination of the RE 3+ ions distribution on the three available crystal sites of the silico-carnotite structure. Highlights: ► The structure of the Ca 3 M 2 Si 3 O 12 (M=Eu, Gd, Dy, Er and Lu) was determined. ► Different distribution of RE 3+ ions on the three available crystal sites was observed. ► The instability of the silico-carnotite structure for RE=La→Sm was discussed.

Crystal structure of aspartame anhydrate from powder diffraction data. Structural aspects of the dehydration process of aspartame

NARCIS (Netherlands)

Guguta, C.; Meekes, H.L.M.; Gelder, R. de

2006-01-01

Aspartame has three pseudo-polymorphic forms, two hydrates and a hemi-hydrate, for which crystal structures were determined from single-crystal diffraction data. This paper presents the crystal structure of the anhydrate, which was obtained by dehydrating the hemi-hydrate. The crystal structure of

Therapeutic applications of Rhenium-188 in nuclear medicine and oncology - Current status and expected future perspectives

International Nuclear Information System (INIS)

Knapp, F. F. Jr.

2005-01-01

Full text: The increasing use of unsealed radioactive targeting agents for cancer treatment requires the routine availability of cost-effective radioisotopes. Rhenium-188 (Re-188; half-life 16.9 hours) is a high-energy beta-emitter (E max 2.12 MeV), readily available no- max carrier-added from the alumina-based tungsten-188 (half-life 69 days)/rhenium-188 generator system. Rhenium-188 also emits a 155 keV (15%) gamma photon, permitting gamma camera imaging for biodistribution and dosimetry evaluation. The versatile chemistry of rhenium allows attachment to a wide variety of targeting molecules for Re-188 applications in nuclear oncology for both palliative metastatic treatment and targeted tumor therapy - radionuclide synovectomy, and coronary restenosis therapy. The long parent half-life and consistent performance provide an indefinite generator shelf-life of several months with high Re-188 elution yields (75-85 %) and consistently low W-188 parent breakthrough ( -6 ). Simple post-elution concentration methods have been developed which provide very high specific volume solution of Re-188 for radiolabeling (> 700 mCi/mL saline/1 Ci generator). Over 60 physician-sponsored clinical trials are currently in progress worldwide with applications in nuclear medicine, nuclear oncology and interventional cardiology. A variety of Re-188-labeled therapeutic radiopharmaceuticals and devices are being developed for clinical trials currently in progress for treatment of both benign and metastatic oncological disorders. Palliation of metastatic bone pain with Re-188-HEDP - prepared from a simple 'kit' - has been demonstrated as a cost-effective alternative to similar agents. Recent studies have in fact demonstrated the enhancement of progression-free interval and survival time by repeated Re-188-HEDP injections to patients with metastatic disease from prostate cancer. The use of the Re-188-labeled antiNCA95 (CD66) antibody in conjunction with external beam irradiation is an

Crystal structure of actinide metals at high compression

International Nuclear Information System (INIS)

Fast, L.; Soederlind, P.

1995-08-01

The crystal structures of some light actinide metals are studied theoretically as a function of applied pressure. The first principles electronic structure theory is formulated in the framework of density functional theory, with the gradient corrected local density approximation of the exchange-correlation functional. The light actinide metals are shown to be well described as itinerant (metallic) f-electron metals and generally, they display a crystal structure which have, in agreement with previous theoretical suggestions, increasing degree of symmetry and closed-packing upon compression. The theoretical calculations agree well with available experimental data. At very high compression, the theory predicts closed-packed structures such as the fcc or the hcp structures or the nearly closed-packed bcc structure for the light actinide metals. A simple canonical band picture is presented to explain in which particular closed-packed form these metals will crystallize at ultra-high pressure

RHENIUM SOLUBILITY IN BOROSILICATE NUCLEAR WASTE GLASS IMPLICATIONS FOR THE PROCESSING AND IMMOBILIZATION OF TECHNETIUM-99 (AND SUPPORTING INFORMATION WITH GRAPHICAL ABSTRACT)

Energy Technology Data Exchange (ETDEWEB)

AA KRUGER; A GOEL; CP RODRIGUEZ; JS MCCLOY; MJ SCHWEIGER; WW LUKENS; JR, BJ RILEY; D KIM; M LIEZERS; P HRMA

2012-08-13

The immobilization of 99Tc in a suitable host matrix has proved a challenging task for researchers in the nuclear waste community around the world. At the Hanford site in Washington State in the U.S., the total amount of 99Tc in low-activity waste (LAW) is {approx} 1,300 kg and the current strategy is to immobilize the 99Tc in borosilicate glass with vitrification. In this context, the present article reports on the solubility and retention of rhenium, a nonradioactive surrogate for 99Tc, in a LAW sodium borosilicate glass. Due to the radioactive nature of technetium, rhenium was chosen as a simulant because of previously established similarities in ionic radii and other chemical aspects. The glasses containing target Re concentrations varying from 0 to10,000 ppm by mass were synthesized in vacuum-sealed quartz ampoules to minimize the loss of Re by volatilization during melting at 1000 DC. The rhenium was found to be present predominantly as Re7 + in all the glasses as observed by X-ray absorption near-edge structure (XANES). The solubility of Re in borosilicate glasses was determined to be {approx}3,000 ppm (by mass) using inductively coupled plasma-optical emission spectroscopy (ICP-OES). At higher rhenium concentrations, some additional material was retained in the glasses in the form of alkali perrhenate crystalline inclusions detected by X-ray diffraction (XRD) and laser ablation-ICP mass spectrometry (LA-ICP-MS). Assuming justifiably substantial similarities between Re7 + and Tc 7+ behavior in this glass system, these results implied that the processing and immobilization of 99Tc from radioactive wastes should not be limited by the solubility of 99Tc in borosilicate LAW glasses.

CCDC 1416891: Experimental Crystal Structure Determination : Methyl-triphenyl-germanium

KAUST Repository

Bernatowicz, Piotr; Shkurenko, Aleksander; Osior, Agnieszka; Kamieński, Bohdan; Szymański, Sławomir

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

Structural Color Patterns by Electrohydrodynamic Jet Printed Photonic Crystals.

Science.gov (United States)

Ding, Haibo; Zhu, Cun; Tian, Lei; Liu, Cihui; Fu, Guangbin; Shang, Luoran; Gu, Zhongze

2017-04-05

In this work, we demonstrate the fabrication of photonic crystal patterns with controllable morphologies and structural colors utilizing electrohydrodynamic jet (E-jet) printing with colloidal crystal inks. The final shape of photonic crystal units is controlled by the applied voltage signal and wettability of the substrate. Optical properties of the structural color patterns are tuned by the self-assembly of the silica nanoparticle building blocks. Using this direct printing technique, it is feasible to print customized functional patterns composed of photonic crystal dots or photonic crystal lines according to relevant printing mode and predesigned tracks. This is the first report for E-jet printing with colloidal crystal inks. Our results exhibit promising applications in displays, biosensors, and other functional devices.

Effect of deformation and annealing on mechanical properties of nickel-rhenium alloys

International Nuclear Information System (INIS)

Mashkova, V.M.

1978-01-01

Studied have been the mechanical properties of nickel-rhenium alloys, depending on the extent of deformation and heat treatment leading to softening. The mechanical properties of the alloys have been estimated by the results of the tensile tests of wire samples. The softening of the alloy at different temperatures is judged about by the variation in hardness. The results of the study indicate that the most abrupt reduction in the hardness of the cold-hardened metal occurs at 900-1,000 deg C and the hold-time of 1 min. Increase in the hold-time at such temperature almost does not reduce the hardness. It is established that in order to soften nickel-rhenium alloys in the process of the cold-deformation at brief annealings in the air the hold-time should not exceed 5 min at 800-900 deg C

SYNTHESIS, CHARACTERIZATION, AND CRYSTAL STRUCTURE ...

African Journals Online (AJOL)

a

KEY WORDS: Barium, Crystal structure, 2,6-Pyridinedicarboxylic acid .... The rational design of novel metal-organic frameworks has attracted great ..... Bond, A.D.; Jones, W. Supramolecular Organization and Materials Design, Jones, W.; Rao,.

Crystal structure of enolase from Drosophila melanogaster.

Science.gov (United States)

Sun, Congcong; Xu, Baokui; Liu, Xueyan; Zhang, Zhen; Su, Zhongliang

2017-04-01

Enolase is an important enzyme in glycolysis and various biological processes. Its dysfunction is closely associated with diseases. Here, the enolase from Drosophila melanogaster (DmENO) was purified and crystallized. A crystal of DmENO diffracted to 2.0 Å resolution and belonged to space group R32. The structure was solved by molecular replacement. Like most enolases, DmENO forms a homodimer with conserved residues in the dimer interface. DmENO possesses an open conformation in this structure and contains conserved elements for catalytic activity. This work provides a structural basis for further functional and evolutionary studies of enolase.

Crystallization and Characterization of Galdieria sulphuraria RUBISCO in Two Crystal Forms: Structural Phase Transition Observed in P21 Crystal Form

Directory of Open Access Journals (Sweden)

Boguslaw Stec

2007-10-01

Full Text Available We have isolated ribulose-1,5-bisphosphate-carboxylase/oxygenase (RUBISCOfrom the red algae Galdieria Sulphuraria. The protein crystallized in two different crystalforms, the I422 crystal form being obtained from high salt and the P21 crystal form beingobtained from lower concentration of salt and PEG. We report here the crystallization,preliminary stages of structure determination and the detection of the structural phasetransition in the P21 crystal form of G. sulphuraria RUBISCO. This red algae enzymebelongs to the hexadecameric class (L8S8 with an approximate molecular weight 0.6MDa.The phase transition in G. sulphuraria RUBISCO leads from two hexadecamers to a singlehexadecamer per asymmetric unit. The preservation of diffraction power in a phasetransition for such a large macromolecule is rare.

Rhenium(V) and technetium(V) complexes of bis(o-hydroxyphenyl)phenylphosphine (PO22-) and (o-hydroxyphenyl)diphenylphosphine (PO-) ligands

International Nuclear Information System (INIS)

Luo, Hongyan; Setyawati, Ika; Rettig, S.J.; Orvig, C.

1995-01-01

The synthesis of several phosphine-based chelating compounds and chelates formed between these compounds and rhenium or technetium is discussed. Four categories of products result, (i) bis-(o-hydroxyphenyl) diphenylphosphine (PO) complexes, (ii) mono- (PO) complexes, (iii) bis-bis(o-hydroxyphenyl)-phenylphosphine (PO 2 ) complexes, and mixed-(PO) and (PO 2 ) complexes. Molecular structures of these compounds (including isomers) were probed by NMR, MS, and IR spectroscopies and by X-ray crystallography

Synthesis and crystal structure analysis of uranyl triple acetates

Energy Technology Data Exchange (ETDEWEB)

Klepov, Vladislav V., E-mail: vladislavklepov@gmail.com [Institute for Energy and Climate Research (IEK-6), Forschungszentrum Jülich GmbH, 52428 Jülich (Germany); Department of Chemistry, Samara National Research University, 443086 Samara (Russian Federation); Serezhkina, Larisa B.; Serezhkin, Victor N. [Department of Chemistry, Samara National Research University, 443086 Samara (Russian Federation); Alekseev, Evgeny V., E-mail: e.alekseev@fz-juelich.de [Institute for Energy and Climate Research (IEK-6), Forschungszentrum Jülich GmbH, 52428 Jülich (Germany); Institut für Kristallographie, RWTH Aachen University, 52066 Aachen (Germany)

2016-12-15

Single crystals of triple acetates NaR[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}·6H{sub 2}O (R=Mg, Co, Ni, Zn), well-known for their use as reagents for sodium determination, were grown from aqueous solutions and their structural and spectroscopic properties were studied. Crystal structures of the mentioned phases are based upon (Na[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}){sup 2–} clusters and [R(H{sub 2}O){sub 6}]{sup 2+} aqua-complexes. The cooling of a single crystal of NaMg[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}·6H{sub 2}O from 300 to 100 K leads to a phase transition from trigonal to monoclinic crystal system. Intermolecular interactions between the structural units and their mutual packing were studied and compared from the point of view of the stereoatomic model of crystal structures based on Voronoi-Dirichlet tessellation. Using this method we compared the crystal structures of the triple acetates with Na[UO{sub 2}(CH{sub 3}COO){sub 3}] and [R(H{sub 2}O){sub 6}][UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 2} and proposed reasons of triple acetates stability. Infrared and Raman spectra were collected and their bands were assigned. - Graphical abstract: Single crystals of uranium based triple acetates, analytical reagents for sodium determination, were synthesized and structurally, spectroscopically and topologically characterized. The structures were compared with the structures of compounds from preceding families [M(H{sub 2}O){sub 6})][UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 2} (M = Mg, Co, Ni, Zn) and Na[UO{sub 2}(CH{sub 3}COO){sub 3}]. Analysis was performed with the method of molecular Voronoi-Dirichlet polyhedra to reveal a large contribution of the hydrogen bonds into intermolecular interactions which can be a reason of low solubility of studied complexes.

Crystal structure of tris(hydroxylammonium orthophosphate

Directory of Open Access Journals (Sweden)

Malte Leinemann

2015-11-01

Full Text Available The crystal structure of the title salt, ([H3NOH]+3·[PO4]3−, consists of discrete hydroxylammonium cations and orthophosphate anions. The atoms of the cation occupy general positions, whereas the anion is located on a threefold rotation axis that runs through the phosphorus atom and one of the phosphate O atoms. In the crystal structure, cations and anions are linked by intermolecular O—H...O and N—H...O hydrogen bonds into a three-dimensional network. Altogether, one very strong O—H...O, two N—H...O hydrogen bonds of medium strength and two weaker bifurcated N—H...O interactions are observed.

Study on the application of crown ether for neutron activation analysis of rubidium and rhenium in rock samples

International Nuclear Information System (INIS)

Wang Xiaolin; Fu Yibei; Liu Yinong; Xiong Zonghua; Hao Fanhua

1996-01-01

The extraction behaviour of rubidium and rhenium with 18-crown-6 (18C6) and benzo-15-crown-5 (B15C5) in nitrobenzene from picric acid or potassium hydroxide solution are studied and methods for separation and determination are developed. The molar ratio of 18C6 to Rb and B15C5 to Re in the extracted species is probably 2:1. Rubidium and rhenium in rock samples are satisfactorily determined by neutron activation method

Rhenium Dichalcogenides: Layered Semiconductors with Two Vertical Orientations.

Science.gov (United States)

Hart, Lewis; Dale, Sara; Hoye, Sarah; Webb, James L; Wolverson, Daniel

2016-02-10

The rhenium and technetium diselenides and disulfides are van der Waals layered semiconductors in some respects similar to more well-known transition metal dichalcogenides (TMD) such as molybdenum sulfide. However, their symmetry is lower, consisting only of an inversion center, so that turning a layer upside-down (that is, applying a C2 rotation about an in-plane axis) is not a symmetry operation, but reverses the sign of the angle between the two nonequivalent in-plane crystallographic axes. A given layer thus can be placed on a substrate in two symmetrically nonequivalent (but energetically similar) ways. This has consequences for the exploitation of the anisotropic properties of these materials in TMD heterostructures and is expected to lead to a new source of domain structure in large-area layer growth. We produced few-layer ReS2 and ReSe2 samples with controlled "up" or "down" orientations by micromechanical cleavage and we show how polarized Raman microscopy can be used to distinguish these two orientations, thus establishing Raman as an essential tool for the characterization of large-area layers.

Ultrasmall-angle X-ray scattering analysis of photonic crystal structure

International Nuclear Information System (INIS)

Abramova, V. V.; Sinitskii, A. S.; Grigor'eva, N. A.; Grigor'ev, S. V.; Belov, D. V.; Petukhov, A. V.; Mistonov, A. A.; Vasil'eva, A. V.; Tret'yakov, Yu. D.

2009-01-01

The results of an ultrasmall-angle X-ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily distinguish between samples with predominantly twinned fcc structure and nearly perfect fcc stacking. The difference observed between samples fabricated under identical conditions is attributed to random layer stacking in the self-assembled colloidal crystals used as templates for fabricating the inverse opals. The present method provides a versatile tool for analyzing photonic crystal structure in studies of inverse opals made of various materials, colloidal crystals, and three-dimensional photonic crystals of other types.

Identification of rhenium donors and sulfur vacancy acceptors in layered MoS{sub 2} bulk samples

Energy Technology Data Exchange (ETDEWEB)

Brandão, F. D., E-mail: fdbrand@fisica.ufmg.br; Ribeiro, G. M.; Vaz, P. H.; González, J. C.; Krambrock, K. [Departamento de Física, Universidade Federal de Minas Gerais, CP 702, 30.123-970 Belo Horizonte, MG (Brazil)

2016-06-21

MoS{sub 2} monolayers, a two-dimensional (2D) direct semiconductor material with an energy gap of 1.9 eV, offer many opportunities to be explored in different electronic devices. Defects often play dominant roles in the electronic and optical properties of semiconductor devices. However, little experimental information about intrinsic and extrinsic defects or impurities is available for this 2D system, and even for macroscopic 3D samples for which MoS{sub 2} shows an indirect bandgap of 1.3 eV. In this work, we evaluate the nature of impurities with unpaired spins using electron paramagnetic resonance (EPR) in different geological macroscopic samples. Regarding the fact that monolayers are mostly obtained from natural crystals, we expect that the majority of impurities found in macroscopic samples are also randomly present in MoS{sub 2} monolayers. By EPR at low temperatures, rhenium donors and sulfur vacancy acceptors are identified as the main impurities in bulk MoS{sub 2} with a corresponding donor concentration of about 10{sup 8–12} defects/cm{sup 2} for MoS{sub 2} monolayer. Electrical transport experiments as a function of temperature are in good agreement with the EPR results, revealing a shallow donor state with an ionization energy of 89 meV and a concentration of 7 × 10{sup 15 }cm{sup −3}, which we attribute to rhenium, as well as a second deeper donor state with ionization energy of 241 meV with high concentration of 2 × 10{sup 19 }cm{sup −3} and net acceptor concentration of 5 × 10{sup 18 }cm{sup −3} related to sulfur vacancies.

Femtosecond Fluorescence and Intersystem Crossing in Rhenium(I) Carbonyl-Bipyridine Complexes

Czech Academy of Sciences Publication Activity Database

Cannizzo, A.; Blanco-Rodríguez, A. M.; Nahhas, A. E.; Šebera, Jakub; Záliš, Stanislav; Vlček, Antonín; Chergui, M.

2008-01-01

Roč. 130, č. 28 (2008), s. 8967-8974 ISSN 0002-7863 R&D Projects: GA MŠk 1P05OC068 Institutional research plan: CEZ:AV0Z40400503 Keywords : rhenium(I) * carbonyl-bipyridine * intersystem crossing Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 8.091, year: 2008

Molecular Engineering of Technetium and Rhenium Based Radiopharmaceuticals

International Nuclear Information System (INIS)

Zubieta, J.

2003-01-01

The research was based on the observation that despite the extraordinarily rich coordination chemistry of technetium and rhenium and several notable successes in reagent design, the extensive investigations by numerous research groups on a variety of N 2 S 2 and N 3 S donor type ligands and on HYNIC have revealed that the chemistries of these ligands with Tc and Re are rather complex, giving rise to considerable difficulties in the development of reliable procedures for the development of radiopharmaceutical reagents

Rhenium(V) complexing with benzimidazole in acidic media

International Nuclear Information System (INIS)

Zakaeva, R.Sh.; Gagieva, S.Ch.; Kaloev, N.I.; Bukov, N.N.; Panyushkin, V.T.

2003-01-01

Coordination compounds of rhenium(V) with 1H-benzimidazole (L) separated from acid media: (HL) 2 [ReOX 5 ](H 2 O) n and [ReOL x X y (H 2 O) z ](H 2 O) n (HL and L - protonated and deprotonated forms of benzimidazole; X = Cl - , Br - ) were studied by the methods of IR spectroscopy, 1 H NMR spectroscopy and thermal gravimetric analysis. Methods of ligand coordination in the complexes are discussed on the basis of data obtained [ru

Fabrication and use of zircaloy/tantalum-sheathed cladding thermocouples and molybdenum/rhenium-sheathed fuel centerline thermocouples

International Nuclear Information System (INIS)

Wilkins, S.C.; Sepold, L.K.

1985-01-01

The thermocouples described in this report are zircaloy/tantalum-sheathed and molybdenum/rhenium alloy-sheathed instruments intended for fuel rod cladding and fuel centerline temperature measurements, respectively. Both types incorporate beryllium oxide insulation and tungsten/rhenium alloy thermoelements. These thermocouples, operated at temperatures of 2000 0 C and above, were developed for use in the internationally sponsored Severe Fuel Damage test series in the Power Burst Facility. The fabrication steps for both thermocouple types are described in detail. A laser-welding attachment technique for the cladding-type thermocouple is presented, and experience with alternate materials for cladding and fuel therocouples is discussed

Crystal structure and solid-state properties of discrete hexa cationic ...

Indian Academy of Sciences (India)

Subsequently, weight loss of 33% in two stages from 242 to 691◦C can be assigned to the decomposition of triazole ligands. 3.3 Description of the crystal structure. The solid-state structure of ZnT was unambiguously determined by the single crystal X-ray diffraction tech- nique (figures 2 and 3). Compound ZnT crystallizes in.

Crystal structure and magnetism of UOsAl

Energy Technology Data Exchange (ETDEWEB)

Andreev, A.V., E-mail: andreev@fzu.cz [Institute of Physics, Academy of Sciences, Na Slovance 2, 182 21 Prague (Czech Republic); Daniš, S. [Department of Condensed Matter Physics, Charles University, Ke Karlovu 5, 121 16 Prague (Czech Republic); Šebek, J.; Henriques, M.S.; Vejpravová, J. [Institute of Physics, Academy of Sciences, Na Slovance 2, 182 21 Prague (Czech Republic); Gorbunov, D.I. [Institute of Physics, Academy of Sciences, Na Slovance 2, 182 21 Prague (Czech Republic); Dresden High Magnetic Field Laboratory (HLD-EMFL), Helmholtz-Zentrum, Dresden-Rossendorf, D-01314 Dresden (Germany); Havela, L. [Department of Condensed Matter Physics, Charles University, Ke Karlovu 5, 121 16 Prague (Czech Republic)

2017-04-15

Crystal structure, magnetization, and specific heat were studied on single crystal of uranium intermetallic compound UOsAl. It is a hexagonal Laves phase of MgZn{sub 2} type, space group P6{sub 3}/mmc, with lattice parameters a=536.4 pm, c=845.3 pm. Shortest inter-uranium distance 313 pm (along the c-axis) is considerably smaller than the Hill limit (340 pm). The compound is a weakly temperature-dependent paramagnet with magnetic susceptibility of ≈1.5*10{sup −8} m{sup 3} mol{sup −1} (at T=2 K), which is slightly higher with magnetic field along the a-axis compared to the c-axis. The Sommerfeld coefficient of electronic specific heat has moderate value of γ=36 mJ mol{sup −1} K{sup −2}. - Highlights: • Crystal structure and magnetic properties were studied on single crystal of UOsAl with hexagonal structure of MgZn{sub 2} type. • Shortest inter-uranium distance 313 pm (along the c-axis) is considerably smaller than the Hill limit (340 pm). • UOsAl has paramagnetic ground state as the compounds with T=Fe and Ru, i.e. 3d and 4d analogues of Os.

Programmatic conversion of crystal structures into 3D printable files using Jmol

OpenAIRE

Scalfani, Vincent F.; Williams, Antony J.; Tkachenko, Valery; Karapetyan, Karen; Pshenichnov, Alexey; Hanson, Robert M.; Liddie, Jahred M.; Bara, Jason E.

2016-01-01

Background Three-dimensional (3D) printed crystal structures are useful for chemistry teaching and research. Current manual methods of converting crystal structures into 3D printable files are time-consuming and tedious. To overcome this limitation, we developed a programmatic method that allows for facile conversion of thousands of crystal structures directly into 3D printable files. Results A collection of over 30,000 crystal structures in crystallographic information file (CIF) format from...

Crystal structure and crystal growth of the polar ferrimagnet CaBaFe4O7

Science.gov (United States)

Perry, R. S.; Kurebayashi, H.; Gibbs, A.; Gutmann, M. J.

2018-05-01

Magnetic materials are a cornerstone for developing spintronic devices for the transport of information via magnetic excitations. To date, relatively few materials have been investigated for the purpose of spin transport, mostly due to the paucity of suitable candidates as these materials are often chemically complex and difficult to synthesize. We present the crystal growth and a structure solution on the high-temperature crystal structure of the layered, polar ferrimagnet CaBaFe4O7 , which is a possible new contender for spintronics research. The space group is identified as P 3 by refinement of single crystal and powder neutron diffraction data. At 400 K, the trigonal lattice parameters are a =11.0114 (11 )Å and c =10.330 (3 )Å . The structure is similar to the low-temperature phase with alternating layers of triangular and Kagome-arranged Fe-O tetrahedra. We also present details of the crystal growth by traveling solvent method.

Solving crystal structures with the symmetry minimum function

International Nuclear Information System (INIS)

Estermann, M.A.

1995-01-01

Unravelling the Patterson function (the auto-correlation function of the crystal structure) (A.L. Patterson, Phys. Rev. 46 (1934) 372) can be the only way of solving crystal structures from neutron and incomplete diffraction data (e.g. powder data) when direct methods for phase determination fail. The negative scattering lengths of certain isotopes and the systematic loss of information caused by incomplete diffraction data invalidate the underlying statistical assumptions made in direct methods. In contrast, the Patterson function depends solely on the quality of the available diffraction data. Simpson et al. (P.G. Simpson et al., Acta Crystallogr. 18 (1965) 169) showed that solving a crystal structure with a particular superposition of origin-shifted Patterson functions, the symmetry minimum function, is advantageous over using the Patterson function alone, for single-crystal X-ray data.This paper describes the extension of the Patterson superposition approach to neutron data and powder data by (a) actively using the negative regions in the Patterson map caused by negative scattering lengths and (b) using maximum entropy Patterson maps (W.I.F. David, Nature 346 (1990) 731). Furthermore, prior chemical knowledge such as bond lengths and angles from known fragments have been included. Two successful structure solutions of a known and a previously unknown structure (M. Hofmann, J. Solid State Chem., in press) illustrate the potential of this new development. ((orig.))

CCDC 1416891: Experimental Crystal Structure Determination : Methyl-triphenyl-germanium

KAUST Repository

Bernatowicz, Piotr

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1408042: Experimental Crystal Structure Determination : 6,13-dimesitylpentacene

KAUST Repository

Shi, Xueliang

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1475929: Experimental Crystal Structure Determination : trimethylammonium tribromo-tin(iv)

KAUST Repository

Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

CCDC 1475930: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

KAUST Repository

Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

CCDC 1475931: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

KAUST Repository

Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

CCDC 1482638: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

KAUST Repository

Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

Nonlinear coherent structures in granular crystals

Science.gov (United States)

Chong, C.; Porter, Mason A.; Kevrekidis, P. G.; Daraio, C.

2017-10-01

The study of granular crystals, which are nonlinear metamaterials that consist of closely packed arrays of particles that interact elastically, is a vibrant area of research that combines ideas from disciplines such as materials science, nonlinear dynamics, and condensed-matter physics. Granular crystals exploit geometrical nonlinearities in their constitutive microstructure to produce properties (such as tunability and energy localization) that are not conventional to engineering materials and linear devices. In this topical review, we focus on recent experimental, computational, and theoretical results on nonlinear coherent structures in granular crystals. Such structures—which include traveling solitary waves, dispersive shock waves, and discrete breathers—have fascinating dynamics, including a diversity of both transient features and robust, long-lived patterns that emerge from broad classes of initial data. In our review, we primarily discuss phenomena in one-dimensional crystals, as most research to date has focused on such scenarios, but we also present some extensions to two-dimensional settings. Throughout the review, we highlight open problems and discuss a variety of potential engineering applications that arise from the rich dynamic response of granular crystals.

Unique Reversible Crystal-to-Crystal Phase Transition – Structural and Functional Properties of Fused Ladder Thienoarenes

KAUST Repository

Abe, Yuichiro

2017-08-15

Donor-acceptor type molecules based on fused ladder thienoarenes, indacenodithiophene (IDT) and dithienocyclopenta-thienothiophene (DTCTT), coupled with benzothiadiazole, are prepared and their solid-state structures are investigated. They display a rich variety of solid phases ranging from amorphous glass states to crystalline states, upon changes in the central aromatic core and side group structures. Most notably, the DTCTT-based derivatives showed reversible crystal-to-crystal phase transitions in heating and cooling cycles. Unlike what has been seen in π−conjugated molecules variable temperature XRD revealed that structural change occurs continuously during the transition. A columnar self-assembled structure with slip-stacked π−π interaction is proposed to be involved in the solid-state. This research provides the evidence of unique structural behavior of the DTCTT-based molecules through the detailed structural analysis. This unique structural transition paves the way for these materials to have self-healing of crystal defects, leading to improved optoelectronic properties.

Unique Reversible Crystal-to-Crystal Phase Transition – Structural and Functional Properties of Fused Ladder Thienoarenes

KAUST Repository

Abe, Yuichiro; Savikhin, Victoria; Yin, Jun; Grimsdale, Andrew C.; Soci, Cesare; Toney, Michael F.; Lam, Yeng Ming

2017-01-01

Donor-acceptor type molecules based on fused ladder thienoarenes, indacenodithiophene (IDT) and dithienocyclopenta-thienothiophene (DTCTT), coupled with benzothiadiazole, are prepared and their solid-state structures are investigated. They display a rich variety of solid phases ranging from amorphous glass states to crystalline states, upon changes in the central aromatic core and side group structures. Most notably, the DTCTT-based derivatives showed reversible crystal-to-crystal phase transitions in heating and cooling cycles. Unlike what has been seen in π−conjugated molecules variable temperature XRD revealed that structural change occurs continuously during the transition. A columnar self-assembled structure with slip-stacked π−π interaction is proposed to be involved in the solid-state. This research provides the evidence of unique structural behavior of the DTCTT-based molecules through the detailed structural analysis. This unique structural transition paves the way for these materials to have self-healing of crystal defects, leading to improved optoelectronic properties.

THERMIONIC EMISSION ENHANCEMENT FROM CESIUM COATED RHENIUM IN ELECTRIC FIELDS

Energy Technology Data Exchange (ETDEWEB)

de Steese, J. G.; Zollweg, R. J.

1963-04-15

The plasma-anode technique was used to observe anomalously high thermionic emission from a rhenium surface with small cesium coverage, where the work function of the composite surface is greater than the ionization potential of cesium. Data suggest that emission enhancement is caused by increased cesium coverage because of cesiumion trapping near the emitter surface under the influence of an ion-rich sheath. (auth)

Photonic Crystal Laser-Driven Accelerator Structures

International Nuclear Information System (INIS)

Cowan, Benjamin M.

2007-01-01

Laser-driven acceleration holds great promise for significantly improving accelerating gradient. However, scaling the conventional process of structure-based acceleration in vacuum down to optical wavelengths requires a substantially different kind of structure. We require an optical waveguide that (1) is constructed out of dielectric materials, (2) has transverse size on the order of a wavelength, and (3) supports a mode with speed-of-light phase velocity in vacuum. Photonic crystals---structures whose electromagnetic properties are spatially periodic---can meet these requirements. We discuss simulated photonic crystal accelerator structures and describe their properties. We begin with a class of two-dimensional structures which serves to illustrate the design considerations and trade-offs involved. We then present a three-dimensional structure, and describe its performance in terms of accelerating gradient and efficiency. We discuss particle beam dynamics in this structure, demonstrating a method for keeping a beam confined to the waveguide. We also discuss material and fabrication considerations. Since accelerating gradient is limited by optical damage to the structure, the damage threshold of the dielectric is a critical parameter. We experimentally measure the damage threshold of silicon for picosecond pulses in the infrared, and determine that our structure is capable of sustaining an accelerating gradient of 300 MV/m at 1550 nm. Finally, we discuss possibilities for manufacturing these structures using common microfabrication techniques

Feasibility of one-shot-per-crystal structure determination using Laue diffraction

Energy Technology Data Exchange (ETDEWEB)

Cornaby, Sterling [School of Applied and Engineering Physics, Cornell University, Ithaca, New York (United States); CHESS (Cornell High Energy Synchrotron Source), Cornell University, Ithaca, New York (United States); Szebenyi, Doletha M. E. [MacCHESS (Macromolecular Diffraction Facilities at CHESS), Cornell University, Ithaca, New York (United States); Smilgies, Detlef-M. [CHESS (Cornell High Energy Synchrotron Source), Cornell University, Ithaca, New York (United States); Schuller, David J.; Gillilan, Richard; Hao, Quan [MacCHESS (Macromolecular Diffraction Facilities at CHESS), Cornell University, Ithaca, New York (United States); Bilderback, Donald H., E-mail: dhb2@cornell.edu [School of Applied and Engineering Physics, Cornell University, Ithaca, New York (United States); CHESS (Cornell High Energy Synchrotron Source), Cornell University, Ithaca, New York (United States)

2010-01-01

Structure determination was successfully carried out using single Laue exposures from a group of lysozyme crystals. The Laue method may be a viable option for collection of one-shot-per-crystal data from microcrystals. Crystal size is an important factor in determining the number of diffraction patterns which may be obtained from a protein crystal before severe radiation damage sets in. As crystal dimensions decrease this number is reduced, eventually falling to one, at which point a complete data set must be assembled using data from multiple crystals. When only a single exposure is to be collected from each crystal, the polychromatic Laue technique may be preferable to monochromatic methods owing to its simultaneous recording of a large number of fully recorded reflections per image. To assess the feasibility of solving structures using single Laue images from multiple crystals, data were collected using a ‘pink’ beam at the CHESS D1 station from groups of lysozyme crystals with dimensions of the order of 20–30 µm mounted on MicroMesh grids. Single-shot Laue data were used for structure determination by molecular replacement and correct solutions were obtained even when as few as five crystals were used.

Feasibility of one-shot-per-crystal structure determination using Laue diffraction

International Nuclear Information System (INIS)

Cornaby, Sterling; Szebenyi, Doletha M. E.; Smilgies, Detlef-M.; Schuller, David J.; Gillilan, Richard; Hao, Quan; Bilderback, Donald H.

2010-01-01

Structure determination was successfully carried out using single Laue exposures from a group of lysozyme crystals. The Laue method may be a viable option for collection of one-shot-per-crystal data from microcrystals. Crystal size is an important factor in determining the number of diffraction patterns which may be obtained from a protein crystal before severe radiation damage sets in. As crystal dimensions decrease this number is reduced, eventually falling to one, at which point a complete data set must be assembled using data from multiple crystals. When only a single exposure is to be collected from each crystal, the polychromatic Laue technique may be preferable to monochromatic methods owing to its simultaneous recording of a large number of fully recorded reflections per image. To assess the feasibility of solving structures using single Laue images from multiple crystals, data were collected using a ‘pink’ beam at the CHESS D1 station from groups of lysozyme crystals with dimensions of the order of 20–30 µm mounted on MicroMesh grids. Single-shot Laue data were used for structure determination by molecular replacement and correct solutions were obtained even when as few as five crystals were used

Structural and morphological characterization of fullerite crystals prepared from the vapor phase

International Nuclear Information System (INIS)

Haluska, M.; Fejdi, P.; Vybornov, M.; Kuzmany, H.

1993-01-01

Crystal structure, habits and surface structures of fullerite crystals prepared from vapor phase were characterized by X-ray analysis, interfacial angle measurements and optical and scanning electron microscopy (SEM). The study of selected C 60 crystals confirmed the fcc structure at room temperature. The crystal habit is determined by two types of morphological faces, namely {100} and {111}. SEM was used for the observation of thermal etched surfaces. (orig.)

Rhenium(V) oxo complexes relevant to technetium renal imaging agents derived from mercaptoacetylglycylglycylaminobenzoic acid isomers. Structural and molecular mechanics studies

International Nuclear Information System (INIS)

Hansen, L.; Taylor, A. Jr; Marzilli, L.G.; Cini, R.

1992-01-01

The synthesis and characterization of three rhenium(V) oxo complexes derived from isomers of mercaptoacetylglycylglycylaminobenzoic acid (MAG 2 -ABAH 5 ) are reported. The isomers were synthesized from o-, m- and p-aminobenzoic acid and differed in the position of the terminal carboxyl group. The anions of 8-10, [ReO(MAG 2 -*ABAH)] - (* = para (8), meta (9), ortho (10)), contained the tetraanionic form of the ligands with the carboxyl group protonated. Compounds 8,9, and 10 were synthesized by exchange reactions of ReOCl 3 (Me 2 SO)(Ph 3 P) under moderate conditions and were isolated as [Ph 4 P] + , [Bu 4 N] + , and [Ph 4 P] + salts, respectively. The structures of 8 and 10 were determined by X-ray diffraction methods; except for the location of the carboxyl group, the structures are similar. The coordination geometry is pseudo square pyramidal, with nitrogen and sulfur donor atoms forming a square base and the oxo ligand at the apex. The orientation of the carboxyl group in 10 is anti to the Re double-bond O group. Since the carboxyl groups are protonated in 8 and 10 and in other relevant structures from this class of radiopharmaceuticals including [Ph 4 As][TcO(MAG 3 H)] (MAG 3 H = tetraanionic form of mercaptoacetyltriglycine), the authors developed molecular mechanics parameters that allowed them to calculate the structures of 8, 10, and [TcO(MAG 3 H)] - . They then extended the calculations to all three isomeric complexes in their deprotonated forms and to [TcO(MAG 3 )] 2- in order to approximate their solution phase structures. They conclude that the [TcO(MAG 3 )] 2- species is conformationally flexible, and they have made an initial assessment of structures vs renal clearance

Photocatalytic Conversion of CO2 to CO using Rhenium Bipyridine Platforms Containing Ancillary Phenyl or BODIPY Moieties

Science.gov (United States)

Andrade, Gabriel A.; Pistner, Allen J.; Yap, Glenn P.A.; Lutterman, Daniel A.; Rosenthal, Joel

2013-01-01

Harnessing of solar energy to drive the reduction of carbon dioxide to fuels requires the development of efficient catalysts that absorb sunlight. In this work, we detail the synthesis, electrochemistry and photophysical properties of a set of homologous fac-ReI(CO)3 complexes containing either an ancillary phenyl (8) or BODIPY (12) substituent. These studies demonstrate that both the electronic properties of the rhenium center and BODIPY chromophore are maintained for these complexes. Photolysis studies demonstrate that both assemblies 8 and 12 are competent catalysts for the photochemical reduction of CO2 to CO in DMF using triethanolamine (TEOA) as a sacrificial reductant. Both compounds 8 and 12 display TOFs for photocatalytic CO production upon irradiation with light (λex ≥ 400 nm) of ~5 hr−1 with TON values of approximately 20. Although structural and photophysical measurements demonstrate that electronic coupling between the BODIPY and fac-ReI(CO)3 units is limited for complex 12, this work clearly shows that the photoactive BODIPY moiety is tolerated during catalysis and does not interfere with the observed photochemistry. When taken together, these results provide a clear roadmap for the development of advanced rhenium bipyridine complexes bearing ancillary BODIPY groups for the efficient photocatalytic reduction of CO2 using visible light. PMID:24015374

NMR structure of the protein NP-247299.1: comparison with the crystal structure

International Nuclear Information System (INIS)

Jaudzems, Kristaps; Geralt, Michael; Serrano, Pedro; Mohanty, Biswaranjan; Horst, Reto; Pedrini, Bill; Elsliger, Marc-André; Wilson, Ian A.; Wüthrich, Kurt

2010-01-01

Comparison of the NMR and crystal structures of a protein determined using largely automated methods has enabled the interpretation of local differences in the highly similar structures. These differences are found in segments of higher B values in the crystal and correlate with dynamic processes on the NMR chemical shift timescale observed in solution. The NMR structure of the protein NP-247299.1 in solution at 313 K has been determined and is compared with the X-ray crystal structure, which was also solved in the Joint Center for Structural Genomics (JCSG) at 100 K and at 1.7 Å resolution. Both structures were obtained using the current largely automated crystallographic and solution NMR methods used by the JCSG. This paper assesses the accuracy and precision of the results from these recently established automated approaches, aiming for quantitative statements about the location of structure variations that may arise from either one of the methods used or from the different environments in solution and in the crystal. To evaluate the possible impact of the different software used for the crystallographic and the NMR structure determinations and analysis, the concept is introduced of reference structures, which are computed using the NMR software with input of upper-limit distance constraints derived from the molecular models representing the results of the two structure determinations. The use of this new approach is explored to quantify global differences that arise from the different methods of structure determination and analysis versus those that represent interesting local variations or dynamics. The near-identity of the protein core in the NMR and crystal structures thus provided a basis for the identification of complementary information from the two different methods. It was thus observed that locally increased crystallographic B values correlate with dynamic structural polymorphisms in solution, including that the solution state of the protein involves

PDF analysis on re-crystallized structure from amorphous BiT

Energy Technology Data Exchange (ETDEWEB)

Yoneda, Yasuhiro [Japan Atomic Energy Research Institute, Synchrotron Radiation Research Center, Kouto 1-1-1, Mikazuki-cho, Sayo-gun, Hyogo 679-5148 (Japan)]. E-mail: yoneda@spring8.or.jp; Kohara, Shinji [Synchrotron Radiation Research Laboratory, Japan Synchrotron Radiation, Research Institute, Kouto 1-1-1, Mikazuki-cho, Sayo-gun, Hyogo 679-5198 (Japan); Hamazaki, Shin' ichi [Department of Electronics, Iwaki Meisei University, Iino 5-5-1, Chuohdai, Fukushima 970-8551 (Japan); Takashige, Masaaki [Department of Electronics, Iwaki Meisei University, Iino 5-5-1, Chuohdai, Fukushima 970-8551 (Japan); Mizuki, Jun' ichiro [Japan Atomic Energy Research Institute, Synchrotron Radiation Research Center, Kouto 1-1-1, Mikazuki-cho, Sayo-gun, Hyogo 679-5148 (Japan)

2005-08-15

A glass sample of composition Bi{sub 4}Ti{sub 3}O{sub 12} was prepared by rapid quenching. The as-quenched sample was confirmed to be amorphous by synchrotron X-ray measurements. The crystallization process of the amorphous sample was also investigated by high-energy X-ray diffraction and by atomic pair distribution function analysis. The perovskite layer in the crystal Bi{sub 4}Ti{sub 3}O{sub 12} is transformed to a pyrochlore structure in the amorphous sample. The amorphous sample first crystallized to a metastable phase by acquiring long-range ordering of the pyrochlore structure at T {sub cryst1}, and then secondary crystallized into a reverted Bi{sub 4}Ti{sub 3}O{sub 12} structure at T {sub cryst2}.

Nucleation of colloidal crystals on configurable seed structures

NARCIS (Netherlands)

Hermes, M; Vermolen, E.C.M.; Leunissen, M.E.; Vossen, D.L.J.; van Oostrum, P.D.J.; Dijkstra, M.; van Blaaderen, A.

2011-01-01

Nucleation is an important stage in the growth of crystals. During this stage, the structure and orientation of a crystal are determined. However, short time- and length-scales make nucleation poorly understood. Micrometer-sized colloidal particles form an ideal model system to study nucleation due

Crystal structure of MboIIA methyltransferase.

Science.gov (United States)

Osipiuk, Jerzy; Walsh, Martin A; Joachimiak, Andrzej

2003-09-15

DNA methyltransferases (MTases) are sequence-specific enzymes which transfer a methyl group from S-adenosyl-L-methionine (AdoMet) to the amino group of either cytosine or adenine within a recognized DNA sequence. Methylation of a base in a specific DNA sequence protects DNA from nucleolytic cleavage by restriction enzymes recognizing the same DNA sequence. We have determined at 1.74 A resolution the crystal structure of a beta-class DNA MTase MboIIA (M.MboIIA) from the bacterium Moraxella bovis, the smallest DNA MTase determined to date. M.MboIIA methylates the 3' adenine of the pentanucleotide sequence 5'-GAAGA-3'. The protein crystallizes with two molecules in the asymmetric unit which we propose to resemble the dimer when M.MboIIA is not bound to DNA. The overall structure of the enzyme closely resembles that of M.RsrI. However, the cofactor-binding pocket in M.MboIIA forms a closed structure which is in contrast to the open-form structures of other known MTases.

Validation of experimental molecular crystal structures with dispersion-corrected density functional theory calculations.

Science.gov (United States)

van de Streek, Jacco; Neumann, Marcus A

2010-10-01

This paper describes the validation of a dispersion-corrected density functional theory (d-DFT) method for the purpose of assessing the correctness of experimental organic crystal structures and enhancing the information content of purely experimental data. 241 experimental organic crystal structures from the August 2008 issue of Acta Cryst. Section E were energy-minimized in full, including unit-cell parameters. The differences between the experimental and the minimized crystal structures were subjected to statistical analysis. The r.m.s. Cartesian displacement excluding H atoms upon energy minimization with flexible unit-cell parameters is selected as a pertinent indicator of the correctness of a crystal structure. All 241 experimental crystal structures are reproduced very well: the average r.m.s. Cartesian displacement for the 241 crystal structures, including 16 disordered structures, is only 0.095 Å (0.084 Å for the 225 ordered structures). R.m.s. Cartesian displacements above 0.25 A either indicate incorrect experimental crystal structures or reveal interesting structural features such as exceptionally large temperature effects, incorrectly modelled disorder or symmetry breaking H atoms. After validation, the method is applied to nine examples that are known to be ambiguous or subtly incorrect.

Validation of experimental molecular crystal structures with dispersion-corrected density functional theory calculations

International Nuclear Information System (INIS)

Streek, Jacco van de; Neumann, Marcus A.

2010-01-01

The accuracy of a dispersion-corrected density functional theory method is validated against 241 experimental organic crystal structures from Acta Cryst. Section E. This paper describes the validation of a dispersion-corrected density functional theory (d-DFT) method for the purpose of assessing the correctness of experimental organic crystal structures and enhancing the information content of purely experimental data. 241 experimental organic crystal structures from the August 2008 issue of Acta Cryst. Section E were energy-minimized in full, including unit-cell parameters. The differences between the experimental and the minimized crystal structures were subjected to statistical analysis. The r.m.s. Cartesian displacement excluding H atoms upon energy minimization with flexible unit-cell parameters is selected as a pertinent indicator of the correctness of a crystal structure. All 241 experimental crystal structures are reproduced very well: the average r.m.s. Cartesian displacement for the 241 crystal structures, including 16 disordered structures, is only 0.095 Å (0.084 Å for the 225 ordered structures). R.m.s. Cartesian displacements above 0.25 Å either indicate incorrect experimental crystal structures or reveal interesting structural features such as exceptionally large temperature effects, incorrectly modelled disorder or symmetry breaking H atoms. After validation, the method is applied to nine examples that are known to be ambiguous or subtly incorrect

Intracellular distribution and stability of a luminescent rhenium(I) tricarbonyl tetrazolato complex using epifluorescence microscopy in conjunction with X-ray fluorescence imaging

International Nuclear Information System (INIS)

Wedding, Jason L.; Harris, Hugh H.; Bader, Christie A.; Plush, Sally E.; Mak, Rachel

2016-01-01

Optical fluorescence microscopy was used in conjunction with X-ray fluorescence microscopy to monitor the stability and intracellular distribution of the luminescent rhenium(I) complex fac-[Re(CO) 3 (phen)L], where phen = 1,10-phenathroline and L = 5-(4-iodophenyl)tetrazolato, in 22Rv1 cells. The rhenium complex showed no signs of ancillary ligand dissociation, a conclusion based on data obtained via X-ray fluorescence imaging aligning iodine and rhenium distributions. A diffuse reticular localisation was detected for the complex, in the nuclear/perinuclear region of cells, by either optical or X-ray fluorescence techniques. Furthermore, X-ray fluorescence also showed that the Re-I complex disrupted the homeostasis of some biologically relevant elements, such as chlorine, potassium and zinc.

A unified picture of the crystal structures of metals

Science.gov (United States)

Söderlind, Per; Eriksson, Olle; Johansson, Börje; Wills, J. M.; Boring, A. M.

1995-04-01

THE crystal structures of the light actinides have intrigued physicists and chemists for several decades1. Simple metals and transition metals have close-packed, high-symmetry structures, such as body-centred cubic, face-centred cubic and hexagonal close packing. In contrast, the structures of the light actinides are very loosely packed and of low symmetry-tetragonal, orthorhombic and monoclinic. To understand these differences, we have performed total-energy calculations, as a function of volume, for both high-and low-symmetry structures of a simple metal (aluminium), a non-magnetic transition metal (niobium), a ferromagnetic transition metal (iron) and a light actinide (uranium). We find that the crystal structure of all of these metals is determined by the balance between electrostatic (Madelung) interactions, which favour high symmetry, and a Peierls distortion of the crystal lattice, which favours low symmetry. We show that simple metals and transition metals can adopt low-symmetry structures on expansion of the lattice; and we predict that, conversely, the light actinides will undergo transitions to structures of higher symmetry on compression.

A unified picture of the crystal structures of metals

International Nuclear Information System (INIS)

Soederlind, P.; Eriksson, O.; Johansson, B.; Wills, J.M.; Boring, A.M.

1995-01-01

The crystal structures of the light actinides have intrigued physicists and chemists for several decades. Simple metals and transition metals have close-packed, high-symmetry structures, such as body-centred cubic, face-centred cubic hexagonal close packing. In contrast, the structures of the light actinides are very loosely packed and of low symmetry -tetragonal, orthorhombic and monoclinic. To understand these differences, we have have performed total-energy calculations, as a function of volume, for both high- and low-symmetry structures of a simple metal (aluminium), a non-magnetic transition metal (niobium), a ferromagnetic transition metal (iron) and a light actinide (uranium). We find that the crystal structure of all these metals is determined by the balance between electrostatic (Madelung) interactions, which favour high symmetry, and a Peierls distortion of the crystal lattice, which favours low symmetry. We show that simple metals and transition metals can adopt low-symmetry structures on expansion of the lattice; and we predict that, conversely, the light actinides will undergo transitions to structures of higher symmetry on compression. (author)

Hydrogen-bond coordination in organic crystal structures: statistics, predictions and applications.

Science.gov (United States)

Galek, Peter T A; Chisholm, James A; Pidcock, Elna; Wood, Peter A

2014-02-01

Statistical models to predict the number of hydrogen bonds that might be formed by any donor or acceptor atom in a crystal structure have been derived using organic structures in the Cambridge Structural Database. This hydrogen-bond coordination behaviour has been uniquely defined for more than 70 unique atom types, and has led to the development of a methodology to construct hypothetical hydrogen-bond arrangements. Comparing the constructed hydrogen-bond arrangements with known crystal structures shows promise in the assessment of structural stability, and some initial examples of industrially relevant polymorphs, co-crystals and hydrates are described.

Multi-structure docking analysis of BACE1 crystal structures and non-peptidic ligands.

Science.gov (United States)

Haghighijoo, Zahra; Hemmateenejad, Bahram; Edraki, Najmeh; Miri, Ramin; Emami, Saeed

2017-09-01

In order to design novel non-peptidic inhibitors of BACE1, many research groups have attempted using computational studies including docking analyses. Since there are too many 3D structures for BACE1 in the protein database, the selection of suitable crystal structures is a key prerequisite for the successful application of molecular docking. We employed a multi-structure docking protocol. In which 615 ligands' structures were docked into 150 BACE1 structures. The large number of the resultant docking scores were post-processed by different data analysis methods including exploratory data analysis, regression analysis and discriminant analysis. It was found that using one crystal structure for docking did not result in high accuracy for predicting activity of the BACE1 inhibitors. Instead, using of the multi-structural docking scores, post-processed by chemometrics methods arrived to highly accurate predictive models. In this regards, the PDB accession codes of 4B70, 4DVF and 2WEZ could discriminate between active and inactive compounds, with higher accuracy. Clustering of the BACE1 structures based on principal component analysis of the crystallographic structures the revealed that the discriminant structures are in the center of the clusters. Thus, these structures can be selected as predominant crystal structures for docking studies of non-peptidic BACE1 inhibitors. Copyright © 2017 Elsevier Inc. All rights reserved.

Effect of the method for rhenium neptasulfide preparation on its catalytic properties in hydrogenation of nitrobenzene and m-nitrobenzoic acid

International Nuclear Information System (INIS)

Pal'chevskaya, T.A.; Bogutskaya, L.V.; Belousov, V.M.

1988-01-01

The effect of conditions of rhenium heptasulfide synthesis by thiosulfate method on its physicochemical and catalytic properties during hydrogenation of nitrobenzene and m-nitrobenzoic acid has been studied. It is shown that the maximum yield of m-aminobenzoic acid can be attained on insoluble sulfide rhenium contacts, containing excessive amount of sulfur (3.5 %). Under certain conditions of catalyst synthesis particles of Re 2 S 7 soluble in dimethylformamide are formed, which possess selectivity towards amine

Crystal structure of isomeric boron difluoride acetylnaphtholates

International Nuclear Information System (INIS)

Bukvetskij, B.V.; Fedorenko, E.V.; Mirochnik, A.G.; Karasev, V.E.

2006-01-01

Crystal structures of luminescent isomeric acetylnaphtholates of boron difluoride are investigated. Full X-ray structural analysis is done at 293 K. Coordinated of atoms, bond angles, bond lengths, interatomic distances are determined. Results of comparative evaluations of the isomers are represented [ru

Structure of a second crystal form of Bence-Jones protein Loc: Strikingly different domain associations in two crystal forms of a single protein

International Nuclear Information System (INIS)

Schiffer, M.; Ainsworth, C.; Xu, Z.B.; Carperos, W.; Olsen, K.; Solomon, A.; Stevens, F.J.; Chang, C.H.

1989-01-01

The authors have determined the structure of the immunoglobulin light-chain dimer Loc in a second crystal form that was grown from distilled water. The crystal structure was determined to 2.8-angstrom resolution; the R factor is 0.22. The two variable domains are related by local 2-fold axes and form an antigen binding pocket. The variable domain-variable domain interaction observed in this crystal form differs from the one exhibited by the protein when crystallized from ammonium sulfate in which the two variable domains formed a protrusion. The structure attained in the distilled water crystals is similar to, but not identical with, the one observed for the Mcg light-chain dimer in crystals grown from ammonium sulfate. Thus, two strikingly different structures were attained by this multisubunit protein in crystals grown under two different, commonly used, crystallization techniques. The quaternary interactions exhibited by the protein in the two crystal forms are sufficiently different to suggest fundamentally different interpretations of the structural basis for the function of this protein. This observation may have general implications regarding the use of single crystallographic determinations for detailed identification of structural and functional relationships. On the other hand, proteins whose structures can be altered by manipulation of crystallization conditions may provide useful systems for study of fundamental structural chemistry

Structure of initial crystals formed during human amelogenesis

Science.gov (United States)

Cuisinier, F. J. G.; Voegel, J. C.; Yacaman, J.; Frank, R. M.

1992-02-01

X-ray diffraction analysis revealed only the existence of carbonated hydroxyapatite (c.HA) during amelogenesis, whereas conventional transmission electron microscopy investigations showed that developing enamel crystals have a ribbon-like habit. The described compositional changes could be an indication for the presence of minerals different from c.HA. However, the absence of identification of such a mineral shows the need of studies by high resolution electron microscopy (HREM) of initial formed human enamel crystals. We demonstrate the existence of two crystal families involved in the early stages of biomineralization: (a) nanometer-size particles which appeared as a precursor phase; (b) ribbon-like crystals, with a structure closely related to c.HA, which by a progressive thickening process tend to attain the mature enamel crystal habit.

Structures of the OmpF porin crystallized in the presence of foscholine-12.

Science.gov (United States)

Kefala, Georgia; Ahn, Chihoon; Krupa, Martin; Esquivies, Luis; Maslennikov, Innokentiy; Kwiatkowski, Witek; Choe, Senyon

2010-05-01

The endogenous Escherichia coli porin OmpF was crystallized as an accidental by-product of our efforts to express, purify, and crystallize the E. coli integral membrane protein KdpD in the presence of foscholine-12 (FC12). FC12 is widely used in membrane protein studies, but no crystal structure of a protein that was both purified and crystallized with this detergent has been reported in the Protein Data Bank. Crystallization screening for KdpD yielded two different crystals of contaminating protein OmpF. Here, we report two OmpF structures, the first membrane protein crystal structures for which extraction, purification, and crystallization were done exclusively with FC12. The first structure was refined in space group P21 with cell parameters a = 136.7 A, b = 210.5 A, c = 137 A, and beta = 100.5 degrees , and the resolution of 3.8 A. The second structure was solved at the resolution of 4.4 A and was refined in the P321 space group, with unit cell parameters a = 215.5 A, b = 215.5 A, c = 137.5 A, and gamma = 120 degrees . Both crystal forms show novel crystal packing, in which the building block is a tetrahedral arrangement of four trimers. Additionally, we discuss the use of FC12 for membrane protein crystallization and structure determination, as well as the problem of the OmpF contamination for membrane proteins overexpressed in E. coli.

Rhenium and technetium complexes with phenylbis(2-pyridyl)phosphine and tris(2-pyridyl)phosphine

Energy Technology Data Exchange (ETDEWEB)

Saucedo A, S. A. [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Calle Cipres No. 10, Fracc. La Penuela, 98068 Zacatecas (Mexico); Hagenbach, A.; Abram, U., E-mail: ssaucedo@uaz.edu.m [Institut fur Chemie und Biochemie, Freie Universitat Berlin, Fabeckstr. 34-36, D-14195, Berlin (Germany)

2010-10-15

Reactions of common technetium and rhenium precursors with 2-pyridyl phosphines produce novel, air stable tricarbonyl and oxo complexes. (NEt{sub 4}){sub 2}[Re(CO){sub 3}Br{sub 3}] or (NEt{sub 4}){sub 2}[Tc(CO){sub 3}Cl{sub 3}] react with phenylbis(2-pyridyl)phosphine (PPhpy{sub 2}) or tris(2-pyridyl)phosphine (Ppy{sub 3}) under formation of neutral tricarbonyl complexes of the composition [M(CO){sub 3}X(L)] (M = Re, X = Br; M = Tc, X = Cl, L = PPhpy{sub 2} or Ppy{sub 3}), where the ligands coordinate only with two for their nitrogen atoms. Removal of the bromo ligands from (NEt{sub 4}){sub 2}[Re(CO){sub 3}(Br){sub 3}] with AgNO{sub 3}, to force a tripodal coordination, and the subsequent reaction with the Ppy{sub 3} results in the formation of the complex [Re(CO){sub 3}(NO{sub 3})(Ppy{sub 3}{sup -}N,N{sup '})] with a monodentate coordinated nitrato ligand. (NBu{sub 4})[ReOCl{sub 4}] reacts with PPhpy{sub 2} to give the asymmetric, oxo-bridged rhenium (V) dimer (NBu{sub 4})[Re{sub 2}O{sub 2}Cl{sub 5}({mu}-PPhpy{sub 2}{sup -}P,N,N,N{sup '})({mu}-O)], while a similar reaction with (ReOCl{sub 3}(PPh{sub 3}){sub 2}] in boiling Thf results in reduction of the metal and gives (ReCl{sub 3}(OPPhpy{sub 2})(PPh{sub 3})]. The products have been characterized spectroscopically and by X-ray structure analyses. (Author)

Neutron activation determination of rhenium in mineral raw materials of complex composition

International Nuclear Information System (INIS)

Shiryaeva, M.B.; Lyubimova, L.N.; Salmin, Yu.P.; Ryumina, K.N.; Tatarkin, M.A.

1984-01-01

The method of neutron-activation rhenium determination in mineral raw material of complex composition is developed, according to which easily hydrolized elements: scandium, iron, lanthanum, ytterbium, protactinium, hafnium and partially ruthenium and osmium are isolated in the form of hydroxides after smelting of a sample, which has been previously irradiated in nuclear reactor (thermal neutron flux 1.2x10 13 n/cm 2 xs for 22 hr) with sodium peroxide and leaching of the melt by water. To separate Re from other interfering elements extraction of perrhenate-ion by methylethylketone from alkali solution is used. Interfering effect of gold is eliminated by its extraction with TBP 30% solution in toluence or benzene from 1 M HNO 3 . Activity of rhenium preparations, singled out from samples of comparison, is measured, using multichannel γ-spectrometer with Ge(Li)-coaxial detector of high resolution (approximately 2.0-2.2 keV over the line 122 keV 5+ Co). Relative standard deviation in Re content range 5x10 -7 -5x10 -2 % does not exceed 0.3

Crystal structure of vanadite: Refinement of anisotropic displacement parameters

Czech Academy of Sciences Publication Activity Database

Laufek, F.; Skála, Roman; Haloda, J.; Císařová, I.

2006-01-01

Roč. 51, 3-4 (2006), s. 271-275 ISSN 1210-8197 Institutional research plan: CEZ:AV0Z30130516 Keywords : anisotropic displacement parameter * crystal structure * single-crystal X-ray refinement * vanadinite Subject RIV: DB - Geology ; Mineralogy

Crystal structure of N-(quinolin-6-ylhydroxylamine

Directory of Open Access Journals (Sweden)

Anuruddha Rajapakse

2014-11-01

Full Text Available The title compound, C9H8N2O, crystallized with four independent molecules in the asymmetric unit. The four molecules are linked via one O—H...N and two N—H...N hydrogen bonds, forming a tetramer-like unit. In the crystal, molecules are further linked by O—H...N and N—H...O hydrogen bonds forming layers parallel to (001. These layers are linked via C—H...O hydrogen bonds and a number of weak C—H...π interactions, forming a three-dimensional structure. The crystal was refined as a non-merohedral twin with a minor twin component of 0.319.

Physicochemical and crystal structure analyses of the antidiabetic agent troglitazone.

Science.gov (United States)

Kobayashi, Katsuhiro; Fukuhara, Hiroshi; Hata, Tadashi; Sekine, Akiko; Uekusa, Hidehiro; Ohashi, Yuji

2003-07-01

The antidiabetic agent troglitazone has two asymmetric carbons located at the chroman ring and the thiazolidine ring and is produced as a mixture of equal amounts of four optical isomers, 2R-5S, 2S-5R, 2R-5R, and 2S-5S. The crystalline powdered drug substance consists of two diastereomer pairs, 2R-5R/2S-5S and 2R-5S/2S-5R. There are many types of crystals obtained from various crystallization conditions. The X-ray structure analysis and the physicochemical analyses of troglitazone were performed. The solvated crystals of the 2R-5R/2S-5S pair were crystallized from several solutions: methanol, ethanol, acetonitrile, and dichloromethane. The ratio of solvent and troglitazone was 1 : 2 (L1/2-form). The monohydrate crystals were obtained from aqueous acetone solution (L1-form). On the other hand, only an anhydrate crystal of the 2R-5S/2S-5R pair was crystallized from various solutions (H0-form). The dihydrous mixed crystal (MA2-form) was obtained from a mixture of the two diastereomer pairs of 2R-5R/2S-5S and 2R-5S/2S-5R in equal amounts by the slow evaporation of aqueous acetone solution. The crystal structure of the MA2-form is similar to the H0-form. When the MA2 crystal was kept under low humidity, it was converted into the dehydrated form (MA0-form) with retention of the single crystal form. The structure of the MA0-form is isomorphous to the H0-form. The MA2-form was converted into the MA0-form and vice versa with retention of the single crystal under low and high humidity, respectively. The crystallization and storage conditions of the drug substances were successfully analyzed.

Two modifications of Y2Piv6(HPiv)6 crystals: synthesis and structures

International Nuclear Information System (INIS)

Kiseleva, E.A.; Troyanov, S.I.; Korenev, Yu.M.

2006-01-01

Crystal structure of solvate of yttrium pivalate YPiv 3 ·3HPiv is studied. Existing of two polymorphous modifications of the compound is detected. It is shown that α- and β-modifications of yttrium pivalate solvate have molecular crystal structures and are built of Y 2 Piv 6 (HPiv) 6 dimers. Difference of these two modifications is in package of dimer molecules and in center-symmetricity of dimers in α-modification structure. Molecular and crystal structure, crystal lattice parameters are determined [ru

Liquid kit for preparation of 188rhenium-etidronate

International Nuclear Information System (INIS)

Marczewski, Barbara; Dias, Carla Roberta; Moraes, Vanessa; Osso Junior, Joao Alberto

2005-01-01

The aim of this study was the preparation of a liquid kit for radiolabeling of 188 Re-HEDP (hydroxyethylidene diphosphonate). 188 Re was obtained from alumina based 188 W/ 188 Re generators. This paper reports the efficacy of a cold kit stored for more than two weeks, determined by the dependence of the radiolabeling yields of 188 Re-HEDP on the incubation time, reducing agent concentration, the effects of concentration of ligand, the p H of the reaction and the temperature. The cold kits showed a good stability when carrie-free rhenium-188 was added in the reaction mixture. (author)

Crystal structure of human protein kinase CK2

DEFF Research Database (Denmark)

Niefind, K; Guerra, B; Ermakowa, I

2001-01-01

The crystal structure of a fully active form of human protein kinase CK2 (casein kinase 2) consisting of two C-terminally truncated catalytic and two regulatory subunits has been determined at 3.1 A resolution. In the CK2 complex the regulatory subunits form a stable dimer linking the two catalyt...... as a docking partner for various protein kinases. Furthermore it shows an inter-domain mobility in the catalytic subunit known to be functionally important in protein kinases and detected here for the first time directly within one crystal structure.......The crystal structure of a fully active form of human protein kinase CK2 (casein kinase 2) consisting of two C-terminally truncated catalytic and two regulatory subunits has been determined at 3.1 A resolution. In the CK2 complex the regulatory subunits form a stable dimer linking the two catalytic...... subunits, which make no direct contact with one another. Each catalytic subunit interacts with both regulatory chains, predominantly via an extended C-terminal tail of the regulatory subunit. The CK2 structure is consistent with its constitutive activity and with a flexible role of the regulatory subunit...

Crystal structure optimisation using an auxiliary equation of state

Science.gov (United States)

Jackson, Adam J.; Skelton, Jonathan M.; Hendon, Christopher H.; Butler, Keith T.; Walsh, Aron

2015-11-01

Standard procedures for local crystal-structure optimisation involve numerous energy and force calculations. It is common to calculate an energy-volume curve, fitting an equation of state around the equilibrium cell volume. This is a computationally intensive process, in particular, for low-symmetry crystal structures where each isochoric optimisation involves energy minimisation over many degrees of freedom. Such procedures can be prohibitive for non-local exchange-correlation functionals or other "beyond" density functional theory electronic structure techniques, particularly where analytical gradients are not available. We present a simple approach for efficient optimisation of crystal structures based on a known equation of state. The equilibrium volume can be predicted from one single-point calculation and refined with successive calculations if required. The approach is validated for PbS, PbTe, ZnS, and ZnTe using nine density functionals and applied to the quaternary semiconductor Cu2ZnSnS4 and the magnetic metal-organic framework HKUST-1.

Crystal structure optimisation using an auxiliary equation of state

International Nuclear Information System (INIS)

Jackson, Adam J.; Skelton, Jonathan M.; Hendon, Christopher H.; Butler, Keith T.; 3 Institute and Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of))" data-affiliation=" (Centre for Sustainable Chemical Technologies and Department of Chemistry, University of Bath, Claverton Down, Bath BA2 7AY (United Kingdom); Global E3 Institute and Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of))" >Walsh, Aron

2015-01-01

Standard procedures for local crystal-structure optimisation involve numerous energy and force calculations. It is common to calculate an energy–volume curve, fitting an equation of state around the equilibrium cell volume. This is a computationally intensive process, in particular, for low-symmetry crystal structures where each isochoric optimisation involves energy minimisation over many degrees of freedom. Such procedures can be prohibitive for non-local exchange-correlation functionals or other “beyond” density functional theory electronic structure techniques, particularly where analytical gradients are not available. We present a simple approach for efficient optimisation of crystal structures based on a known equation of state. The equilibrium volume can be predicted from one single-point calculation and refined with successive calculations if required. The approach is validated for PbS, PbTe, ZnS, and ZnTe using nine density functionals and applied to the quaternary semiconductor Cu 2 ZnSnS 4 and the magnetic metal-organic framework HKUST-1

Crystal structure optimisation using an auxiliary equation of state

Energy Technology Data Exchange (ETDEWEB)

Jackson, Adam J.; Skelton, Jonathan M.; Hendon, Christopher H.; Butler, Keith T. [Centre for Sustainable Chemical Technologies and Department of Chemistry, University of Bath, Claverton Down, Bath BA2 7AY (United Kingdom); Walsh, Aron, E-mail: a.walsh@bath.ac.uk [Centre for Sustainable Chemical Technologies and Department of Chemistry, University of Bath, Claverton Down, Bath BA2 7AY (United Kingdom); Global E" 3 Institute and Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of)

2015-11-14

Standard procedures for local crystal-structure optimisation involve numerous energy and force calculations. It is common to calculate an energy–volume curve, fitting an equation of state around the equilibrium cell volume. This is a computationally intensive process, in particular, for low-symmetry crystal structures where each isochoric optimisation involves energy minimisation over many degrees of freedom. Such procedures can be prohibitive for non-local exchange-correlation functionals or other “beyond” density functional theory electronic structure techniques, particularly where analytical gradients are not available. We present a simple approach for efficient optimisation of crystal structures based on a known equation of state. The equilibrium volume can be predicted from one single-point calculation and refined with successive calculations if required. The approach is validated for PbS, PbTe, ZnS, and ZnTe using nine density functionals and applied to the quaternary semiconductor Cu{sub 2}ZnSnS{sub 4} and the magnetic metal-organic framework HKUST-1.

CCDC 870534: Experimental Crystal Structure Determination : Dichloro-trimethyl-tantalum(v)

KAUST Repository

Chen, Yin; Callens, E.; Abou-Hamad, E.; Merle, N.; White, A.J.P.; Taoufik, M.; Coperet, C.; Le Roux, E.; Basset, J.-M.

2013-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1475931: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

KAUST Repository

Dang, Yangyang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1475929: Experimental Crystal Structure Determination : trimethylammonium tribromo-tin(iv)

KAUST Repository

Dang, Yangyang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1482638: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

KAUST Repository

Dang, Yangyang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1475930: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

KAUST Repository

Dang, Yangyang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

Crystal structure of clathrates of Hofmann dma-type

International Nuclear Information System (INIS)

NIshikiori, Sh.; Ivamoto, T.

1999-01-01

Seven new clathrates Cd(DMA) 2 Ni(CN) 4 ·xG (x=1, G=aniline, 2,3-xylidine, 2,4-xylidine, 2,5-xylidine, 2,6-xylidine, 3,5-xylidine, and x=2, G=2,4,6-trimethylaniline) of Hofmann type are synthesized by amine substitution for dimethylamine (DMA). On the base of x-ray diffraction data it is shown that geometry of guest molecule in cage-like hollow determines the structure of the host and crystal structure of clathrates. Two-dimension metallocomplex of the host of studied clathrates is characterized by elastic folded structure appearing as a result of angular deformation of bond between Cd atoms and host cyanide bridge. Guest molecule orientation is fixed by hydrogen bond. Structural elasticity of the host complex directs to differences in crystal structure of clathrates formed and to considerable variety of incorporated guests [ru

Crystal structure mediates mode of cell death in TiO2 nanotoxicity

International Nuclear Information System (INIS)

Braydich-Stolle, Laura K.; Schaeublin, Nicole M.; Murdock, Richard C.; Jiang, Jingkun; Biswas, Pratim; Schlager, John J.; Hussain, Saber M.

2009-01-01

Certain properties that nanoparticles possess differentiate them from their bulk counterparts, and these characteristics must be evaluated prior to nanoparticle studies and include: size, shape, dispersion, physical and chemical properties, surface area, and surface chemistry. Early nanotoxicity studies evaluating TiO 2 have yielded conflicting data which identify either size or crystal structure as the mediating property for nano-TiO 2 toxicity. However, it is important to note that none of these studies examined size with the crystal structure composition controlled for or examined crystal structure while controlling the nanoparticle size. The goal of this study was to evaluate the role of size and crystal structure in TiO 2 nanotoxicity while controlling for as many other nanoproperties as possible using the HEL-30 mouse keratinocyte cell line as a model for dermal exposure. In the size-dependent studies, all the nanoparticles are 100% anatase, and aggregate sizes were determined in order to take into account the effect of agglomeration on size-dependent toxicity. In addition, varying crystal structures were assessed while the size of the nanoparticles was controlled. We were able to identify that both size and crystal structure contribute to cytotoxicity and that the mechanism of cell death varies based on crystal structure. The 100% anatase TiO 2 nanoparticles, regardless of size, induced cell necrosis, while the rutile TiO 2 nanoparticles initiated apoptosis through formation of reactive oxygen species (ROS).

Shear induced structures in crystallizing cocoa butter

Science.gov (United States)

Mazzanti, Gianfranco; Guthrie, Sarah E.; Sirota, Eric B.; Marangoni, Alejandro G.; Idziak, Stefan H. J.

2004-03-01

Cocoa butter is the main structural component of chocolate and many cosmetics. It crystallizes in several polymorphs, called phases I to VI. We used Synchrotron X-ray diffraction to study the effect of shear on its crystallization. A previously unreported phase (phase X) was found and a crystallization path through phase IV under shear was observed. Samples were crystallized under shear from the melt in temperature controlled Couette cells, at final crystallization temperatures of 17.5^oC, 20^oC and 22.5^oC in Beamline X10A of NSLS. The formation of phase X was observed at low shear rates (90 s-1) and low crystallization temperature (17.5^oC), but was absent at high shear (720 s-1) and high temperature (20^oC). The d-spacing and melting point suggest that this new phase is a mixture rich on two of the three major components of cocoa butter. We also found that, contrary to previous reports, the transition from phase II to phase V can happen through the intermediate phase IV, at high shear rates and temperature.

Crystal structure and vibrational spectra of piperazinium bis(4-hydroxybenzenesulphonate) molecular-ionic crystal

Science.gov (United States)

Marchewka, M. K.; Pietraszko, A.

2008-02-01

The piperazinium bis(4-hydroxybenzenesulphonate) crystallizes from water solution at room temperature in P2 1/ c space group of monoclinic system. The crystals are built up of doubly protonated piperazinium cations and ionized 4-hydroxybenzenesulphonate anions that interact through weak hydrogen bonds of O-H⋯O and N-H⋯O type. Mutual orientation of anions is determined by non-conventional hydrogen bonds of C-H⋯π type. Room temperature powder FT IR and FT Raman measurements were carried out. The vibrational spectra are in full agreement with the structure obtained from X-ray crystallography. The big single crystals of the title salt can be grown.

Local layer structure of smectic liquid crystals by X-ray micro-diffraction

CERN Document Server

Takanishi, Y

2003-01-01

The local layer structure of smectic liquid crystal has been measured using time-resolved synchrotron X-ray micro-diffraction. Typical layer disorders observed in surface stabilized (anti-) ferroelectric liquid crystals, i.e. a stripe texture, a needed-like defect and a zigzag defect, are directly analyzed. The detailed analysis slows that the surface anchoring force due to the interaction between the liquid crystal molecule and the alignment thin film plays an important role to realize both the static and dynamic local layer structures. The layer structure of the circular domain observed in the liquid crystal of bent-shaped molecules found to depend on the applied electric field though the optical micrograph shows little difference. The frustrated, double and single layer structures of the bent-shaped molecule liquid crystal are determined depending on the terminal alkyl chain length. (author)

Prediction of inorganic superconductors with quasi-one-dimensional crystal structure

International Nuclear Information System (INIS)

Volkova, L M; Marinin, D V

2013-01-01

Models of superconductors having a quasi-one-dimensional crystal structure based on the convoluted into a tube Ginzburg sandwich, which comprises a layered dielectric–metal–dielectric structure, have been suggested. The critical crystal chemistry parameters of the Ginzburg sandwich determining the possibility of the emergence of superconductivity and the T c value in layered high-T c cuprates, which could have the same functions in quasi-one-dimensional fragments (sandwich-type tubes), have been examined. The crystal structures of known low-temperature superconductors, in which one can mark out similar quasi-one-dimensional fragments, have been analyzed. Five compounds with quasi-one-dimensional structures, which can be considered as potential parents of new superconductor families, possibly with high transition temperatures, have been suggested. The methods of doping and modification of these compounds are provided. (paper)

Synthesis and crystal structures of three new benzotriazolylpropanamides

Directory of Open Access Journals (Sweden)

Donna S. Amenta

2017-06-01

Full Text Available The base-catalyzed Michael addition of 2-methylacrylamide to benzotriazole afforded 3-(1H-benzotriazol-1-yl-2-methylpropanamide, C10H12N4O (1, in 32% yield in addition to small amounts of isomeric 3-(2H-benzotriazol-2-yl-2-methylpropanamide, C10H12N4O (2. In a similar manner, 3-(1H-benzotriazol-1-yl-N,N-dimethylpropanamide, C11H14N4O (3, was prepared from benzotriazole and N,N-dimethylacrylamide. All three products have been structurally characterized by single-crystal X-ray diffraction. The crystal structures of 1 and 2 comprise infinite arrays formed by N—H...O and N—H...N bridges, as well as π–π interactions, while the molecules of 3 are aggregated to simple π-dimers in the crystal.

Effects of thermo-order-mechanical coupling on band structures in liquid crystal nematic elastomer porous phononic crystals.

Science.gov (United States)

Yang, Shuai; Liu, Ying

2018-08-01

Liquid crystal nematic elastomers are one kind of smart anisotropic and viscoelastic solids simultaneously combing the properties of rubber and liquid crystals, which is thermal sensitivity. In this paper, the wave dispersion in a liquid crystal nematic elastomer porous phononic crystal subjected to an external thermal stimulus is theoretically investigated. Firstly, an energy function is proposed to determine thermo-induced deformation in NE periodic structures. Based on this function, thermo-induced band variation in liquid crystal nematic elastomer porous phononic crystals is investigated in detail. The results show that when liquid crystal elastomer changes from nematic state to isotropic state due to the variation of the temperature, the absolute band gaps at different bands are opened or closed. There exists a threshold temperature above which the absolute band gaps are opened or closed. Larger porosity benefits the opening of the absolute band gaps. The deviation of director from the structural symmetry axis is advantageous for the absolute band gap opening in nematic state whist constrains the absolute band gap opening in isotropic state. The combination effect of temperature and director orientation provides an added degree of freedom in the intelligent tuning of the absolute band gaps in phononic crystals. Copyright © 2018 Elsevier B.V. All rights reserved.

Hexagonal perovskites with cationic vacancies. 29. Structure of Ba/sub 4/ScReWvacantO/sub 12/ - on the function of octahedral cationic vacancies in perovskite stacking polytypes

Energy Technology Data Exchange (ETDEWEB)

Kemmler-Sack, S; Herrmann, M [Tuebingen Univ. (Germany, F.R.). Lehrstuhl fuer Anorganische Chemie 2

1981-09-01

The hexagonal perovskite stacking polytype Ba/sub 4/ScReWvacantO/sub 12/ crystallizes in a rhombohedral 12 L structure (space group R-3m; sequence (hhcc)/sub 3/). The refined, intensity related R' value is 6.6%. The octahedral net consists of blocks of three face connected octahedra with a central vacancy, in the two outer positions the rhenium and tungsten atoms are located; these units are linked via common corners by single octahedra, occupied with scandium. The construction principles of hexagonal oxygen perovskites with octahedral, cationic vacancies are reported.

Crystal structure and optical properties of silver nanorings

Science.gov (United States)

Zhou, Li; Fu, Xiao-Feng; Yu, Liao; Zhang, Xian; Yu, Xue-Feng; Hao, Zhong-Hua

2009-04-01

We report the polyol synthesis and crystal structure characterization of silver nanorings, which have perfect circular shape, smooth surface, and elliptical wire cross-section. The characterization results show that the silver nanorings have well-defined crystal of singly twinned along the whole ring. The spatial distribution of the scattering of a silver nanoring with slanted incidence reveals the unique focus effect of the nanoring, and the focus scattering varies with the incident wavelength. The silver nanorings with perfect geometry and well-defined crystal have potential applications in nanoscaled photonics, plasmonic devices, and optical manipulation.

Crystal structure of PrRh4.8B2

International Nuclear Information System (INIS)

Higashi, Iwami; Shishido, Toetsu; Takei, Humihiko; Kobayashi, Takaaki

1988-01-01

The crystal structure of a new rare earth ternary boride PrRh 4.8 B 2 was investigated, by single-crystal X-ray diffractometry. PrRh 4.8 B 2 crystallizes in the orthorhombic space group Immm with a = 9.697(4), b = 5.577(2), c = 25.64(3) A, Z=12. The intensity data were collected on a four-circle diffractometer with graphite-monochromatized Mo Kα radiation. The structure was solved by the Patterson method and refined with a full-matrix least-squares program to an R value (equal to Σvertical strokeΔFvertical stroke/Σvertical strokeF 0 vertical stroke) of 0.055 for 1176 reflections. (orig.)

PAK4 crystal structures suggest unusual kinase conformational movements.

Science.gov (United States)

Zhang, Eric Y; Ha, Byung Hak; Boggon, Titus J

2018-02-01

In order for protein kinases to exchange nucleotide they must open and close their catalytic cleft. These motions are associated with rotations of the N-lobe, predominantly around the 'hinge region'. We conducted an analysis of 28 crystal structures of the serine-threonine kinase, p21-activated kinase 4 (PAK4), including three newly determined structures in complex with staurosporine, FRAX486, and fasudil (HA-1077). We find an unusual motion between the N-lobe and C-lobe of PAK4 that manifests as a partial unwinding of helix αC. Principal component analysis of the crystal structures rationalizes these movements into three major states, and analysis of the kinase hydrophobic spines indicates concerted movements that create an accessible back pocket cavity. The conformational changes that we observe for PAK4 differ from previous descriptions of kinase motions, and although we observe these differences in crystal structures there is the possibility that the movements observed may suggest a diversity of kinase conformational changes associated with regulation. Protein kinases are key signaling proteins, and are important drug targets, therefore understanding their regulation is important for both basic research and clinical points of view. In this study, we observe unusual conformational 'hinging' for protein kinases. Hinging, the opening and closing of the kinase sub-domains to allow nucleotide binding and release, is critical for proper kinase regulation and for targeted drug discovery. We determine new crystal structures of PAK4, an important Rho-effector kinase, and conduct analyses of these and previously determined structures. We find that PAK4 crystal structures can be classified into specific conformational groups, and that these groups are associated with previously unobserved hinging motions and an unusual conformation for the kinase hydrophobic core. Our findings therefore indicate that there may be a diversity of kinase hinging motions, and that these may

Crystal-Size-Dependent Structural Transitions in Nanoporous Crystals: Adsorption-Induced Transitions in ZIF-8

KAUST Repository

Zhang, Chen

2014-09-04

© 2014 American Chemical Society. Understanding the crystal-size dependence of both guest adsorption and structural transitions of nanoporous solids is crucial to the development of these materials. We find that nano-sized metal-organic framework (MOF) crystals have significantly different guest adsorption properties compared to the bulk material. A new methodology is developed to simulate the adsorption and transition behavior of entire MOF nanoparticles. Our simulations predict that the transition pressure significantly increases with decreasing particle size, in agreement with crystal-size-dependent experimental measurements of the N2-ZIF-8 system. We also propose a simple core-shell model to examine this effect on length scales that are inaccessible to simulations and again find good agreement with experiments. This study is the first to examine particle size effects on structural transitions in ZIFs and provides a thermodynamic framework for understanding the underlying mechanism.

Structural and optical properties of WTe2 single crystals synthesized by DVT technique

Science.gov (United States)

Dixit, Vijay; Vyas, Chirag; Pathak, V. M.; Soalanki, G. K.; Patel, K. D.

2018-05-01

Layered transition metal di-chalcogenide (LTMDCs) crystals have attracted much attention due to their potential in optoelectronic device applications recently due to realization of their monolayer based structures. In the present investigation we report growth of WTe2 single crystals by direct vapor transport (DVT) technique. These crystals are then characterized by energy dispersive analysis of x-rays (EDAX) to study stoichiometric composition after growth. The structural properties are studied by x-ray diffraction (XRD) and selected area electron diffraction (SAED) is used to confirm orthorhombic structure of grown WTe2 crystal. Surface morphological properties of the crystals are also studied by scanning electron microscope (SEM). The optical properties of the grown crystals are studied by UV-Visible spectroscopy which gives direct band gap of 1.44 eV for grown WTe2 single crystals.

Complexes of technetium, rhenium, and rhodium with sexidentate Schiff-base ligands

International Nuclear Information System (INIS)

Hunter, G.; Kilcullen, N.

1989-01-01

The monocationic technetium (IV) and rhenium (IV) complexes with the sexidentate Schiff-base ligands tris[2-(2'-hydroxybenzylideneethyl)]amine and its substituted derivatives have been prepared and their electrochemical properties studied. The variable-temperature 90.6 MHz 13 C-{ 1 H} n.m.r. spectrum of the rhodium (III) complex of tris[2-(2-hydroxy-5'-isopropylbenzylideneethyl)-amine] has been observed, indicating fluxionality at temperatures above 218 K. (author)

A hybrid computational-experimental approach for automated crystal structure solution

Science.gov (United States)

Meredig, Bryce; Wolverton, C.

2013-02-01

Crystal structure solution from diffraction experiments is one of the most fundamental tasks in materials science, chemistry, physics and geology. Unfortunately, numerous factors render this process labour intensive and error prone. Experimental conditions, such as high pressure or structural metastability, often complicate characterization. Furthermore, many materials of great modern interest, such as batteries and hydrogen storage media, contain light elements such as Li and H that only weakly scatter X-rays. Finally, structural refinements generally require significant human input and intuition, as they rely on good initial guesses for the target structure. To address these many challenges, we demonstrate a new hybrid approach, first-principles-assisted structure solution (FPASS), which combines experimental diffraction data, statistical symmetry information and first-principles-based algorithmic optimization to automatically solve crystal structures. We demonstrate the broad utility of FPASS to clarify four important crystal structure debates: the hydrogen storage candidates MgNH and NH3BH3; Li2O2, relevant to Li-air batteries; and high-pressure silane, SiH4.

Synergistic effect of rhenium and ruthenium in nickel-based single-crystal superalloys

Energy Technology Data Exchange (ETDEWEB)

Yu, X.X. [Department of Physics, Tsinghua University, Beijing 100084 (China); Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Wang, C.Y., E-mail: cywang@mail.tsinghua.edu.cn [Department of Physics, Tsinghua University, Beijing 100084 (China); Central Iron and Steel Research Institute, Beijing 100081 (China); Zhang, X.N. [Institute of Microstructure and Property of Advanced Materials, Beijing University of Technology, Beijing 100124 (China); Yan, P. [Central Iron and Steel Research Institute, Beijing 100081 (China); Zhang, Z., E-mail: zezhang@zju.edu.cn [State Key Laboratory of Silicon Materials, Department of Materials Science and Engineering, Zhejiang University, Hangzhou 310027 (China)

2014-01-05

Highlights: • Re and Ru synergistic effects in nickel-based superalloys are investigated. • The Al site occupation of Re atom in the γ′ phase is observed directly. • The addition of Ru results in the repartitioning of Re to γ phase. -- Abstract: The microstructures of ternary Ni–Al–Re and quaternary Ni–Al–Re–Ru single-crystal alloys were investigated at atomic and electronic levels to clarify the synergistic effect of Re and Ru in nickel-based single-crystal superalloys. In the Ni–Al–Re alloy, it was directly observed that Re atom occupied the Al site of γ′ phase. In the Ni–Al–Re–Ru alloy, the mechanisms of Re repartition between γ and γ′ phases were proposed. In the dendritic cores, high concentrations of Re exceeded the solubility limit of γ′ phase and partitioned to γ phase, which led to the homogenization. In the interdendritic regions, Ru resulted in the repartitioning of Re to γ phase which was proved by transmission electron microscopy and first-principles calculations.

Gallium arsenide single crystal solar cell structure and method of making

Science.gov (United States)

Stirn, Richard J. (Inventor)

1983-01-01

A production method and structure for a thin-film GaAs crystal for a solar cell on a single-crystal silicon substrate (10) comprising the steps of growing a single-crystal interlayer (12) of material having a closer match in lattice and thermal expansion with single-crystal GaAs than the single-crystal silicon of the substrate, and epitaxially growing a single-crystal film (14) on the interlayer. The material of the interlayer may be germanium or graded germanium-silicon alloy, with low germanium content at the silicon substrate interface, and high germanium content at the upper surface. The surface of the interface layer (12) is annealed for recrystallization by a pulsed beam of energy (laser or electron) prior to growing the interlayer. The solar cell structure may be grown as a single-crystal n.sup.+ /p shallow homojunction film or as a p/n or n/p junction film. A Ga(Al)AS heteroface film may be grown over the GaAs film.

First principles study of structural, electronic and optical properties of KCl crystal

International Nuclear Information System (INIS)

Chen, Z.J.; Xiao, H.Y.; Zu, X.T.

2006-01-01

The structural, electronic and optical properties of KCl crystal in B1, B2, B3 and T1 structures have been systematically studied using first-principle pseudopotential calculations. In addition, pressure-induced phase transition has also been investigated. It was found that when the pressure is below 2.8 GPa, the B1 structure is the most stable. Above 2.8 GPa KCl crystal will undergo a structural phase transition from the relatively open NaCl structure into the more dense CsCl atomic arrangement. Our results also suggested that at about 1.2 GPa structural phase transition from B3 to T1 will occur. When the pressure arrives at 39.9 GPa, the phase transition will occur from B2 to T1. In addition, we found KCl Crystal has indirect band gap in B2 structure and direct band gap in B1, B3 and T1 structures. The band gap value is the smallest in the T1 structure and is the largest in the B1 and B3 structures. Our calculations are found to be in good agreement with available experimental and theoretical results. The dielectric function and energy loss function of KCl crystal in four structures (B1, B2, B3 and T1) have been calculated as well as the anisotropy of the optical properties of KCl crystal in T1 structure

Solvent effects on the crystal growth structure and morphology of the pharmaceutical dirithromycin

Science.gov (United States)

Wang, Yuan; Liang, Zuozhong

2017-12-01

Solvent effects on the crystal structure and morphology of pharmaceutical dirithromycin molecules were systematically investigated using both experimental crystallization and theoretical simulation. Dirithromycin is one of the new generation of macrolide antibiotics with two polymorphic forms (Form I and Form II) and many solvate forms. Herein, six solvates of the dirithromycin, including acetonitrile, acetonitrile/water, acetone, 1-propanol, N,N-dimethylformamide (DMF) and cyclohexane, were studied. Experimentally, we crystallized the dirithromycin molecules in different solvents by the solvent evaporating method and measured the crystal structures with the X-ray diffraction (XRD). We compared these crystal structures of dirithromycin solvates and analyzed the solvent property-determined structure evolution. The solvents have a strong interaction with the dirithromycin molecule due to the formation of inter-molecular interactions (such as the hydrogen bonding and close contacts (sum of vdW radii)). Theoretically, we calculated the ideal crystal habit based on the solvated structures with the attachment growth (AE) model. The predicted morphologies and aspect ratios of dirithromycin solvates agree well with the experimental results. This work could be helpful to better understand the structure and morphology evolution of solvates controlled by solvents and guide the crystallization of active pharmaceutical ingredients in the pharmaceutical industry.

Cyclic saturation dislocation structures of multiple-slip-oriented copper single crystals

International Nuclear Information System (INIS)

Li, X.W.; Chinese Academy of Sciences, Shenyang; Umakoshi, Y.; Li, S.X.; Wang, Z.G.

2001-01-01

The dislocation structures of [011] and [ anti 111] multiple-slip-oriented Cu single crystals cyclically saturated at constant plastic strain amplitudes were investigated through transmission electron microscopy. The results obtained on [001] multiple-slip-oriented Cu single crystals were also included for summarization. Unlike the case for single-slip-oriented Cu single crystals, the crystallographic orientation has a strong effect on the saturation dislocation structure in these three multiple-slip-oriented crystals. For the [011] crystal, different dislocation patterns such as veins, PSB walls, labyrinths and PSB ladders were observed. The formation of PSB ladders is believed to be a major reason for the existence of a plateau region in the cyclic stress-strain (CSS) curve for the [011] crystal. The cyclic saturation dislocation structure of a [ anti 111] crystal cycled at a low applied strain amplitude γ pl of 2.0 x 10 -4 was found to consist of irregular cells, which would develop into a more regular arrangement (e. g. PSB ladder-like) and the scale of which tends to decrease with increasing γ pl . Finally, three kinds of representative micro-deformation mode were summarized and termed as labyrinth-mode (or [001]-mode), cell-mode (or [ anti 111]-mode) and PSB ladder-mode (or [011]-mode). (orig.)

CRYSTAL STRUCTURE ANALYSIS OF A PUTATIVE OXIDOREDUCTASE FROM KLEBSIELLA PNEUMONIAE

Energy Technology Data Exchange (ETDEWEB)

Baig, M.; Brown, A.; Eswaramoorthy, S.; Swaminathan, S.

2009-01-01

Klebsiella pneumoniae, a gram-negative enteric bacterium, is found in nosocomial infections which are acquired during hospital stays for about 10% of hospital patients in the United States. The crystal structure of a putative oxidoreductase from K. pneumoniae has been determined. The structural information of this K. pneumoniae protein was used to understand its function. Crystals of the putative oxidoreductase enzyme were obtained by the sitting drop vapor diffusion method using Polyethylene glycol (PEG) 3350, Bis-Tris buffer, pH 5.5 as precipitant. These crystals were used to collect X-ray data at beam line X12C of the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory (BNL). The crystal structure was determined using the SHELX program and refi ned with CNS 1.1. This protein, which is involved in the catalysis of an oxidation-reduction (redox) reaction, has an alpha/beta structure. It utilizes nicotinamide adenine dinucleotide phosphate (NADP) or nicotine adenine dinucleotide (NAD) to perform its function. This structure could be used to determine the active and co-factor binding sites of the protein, information that could help pharmaceutical companies in drug design and in determining the protein’s relationship to disease treatment such as that for pneumonia and other related pathologies.

Crystal structure and thermal property of polyethylene glycol octadecyl ether

International Nuclear Information System (INIS)

Meng, Jie-yun; Tang, Xiao-fen; Li, Wei; Shi, Hai-feng; Zhang, Xing-xiang

2013-01-01

Highlights: ► The crystal structure of C18En for n ≥ 20 is a monoclinic system. ► Polyethylene glycol octadecyl ether crystallizes perfectly. ► The number of repeat units has significant effect on the melting, crystallizing temperature and enthalpy. ► The thermal stable temperature increases rapidly with increasing the number of repeat unit. - Abstract: The crystal structure, phase change property and thermal stable temperature (T d ) of polyethylene glycol octadecyl ether [HO(CH 2 CH 2 O) n C 18 H 37 , C18En] with various numbers of repeat units (n = 2, 10, 20 and 100) as phase change materials (PCMs) were investigated using temperature variable Fourier transformed infrared spectroscopy (FTIR), wide-angle X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TG). C18En crystallizes perfectly at 0 °C; and the crystal structure for n ≥ 20 is a monoclinic system. The number of repeat units has great effect on the phase change properties of C18En. The thermal stable temperature increases rapidly with increasing the number of repeat units. They approach to that of PEG-2000 as the number of repeat units is more than 10. T d increases rapidly with increasing the number of repeat units. C18En are a series of promising polymeric PCMs

imide, crystal structure, thermal and dielectric studies

Indian Academy of Sciences (India)

methyl imidazolium methylidene bis(trifluoromethanesulfonyl)imide, crystal structure, thermal and dielectric studies. BOUMEDIENE HADDAD1,2,3,∗, TAQIYEDDINE MOUMENE2, DIDIER VILLEMIN1,. JEAN-FRANÇOIS LOHIER1 and EL-HABIB ...

Magnetic assembly of nonmagnetic particles into photonic crystal structures.

Science.gov (United States)

He, Le; Hu, Yongxing; Kim, Hyoki; Ge, Jianping; Kwon, Sunghoon; Yin, Yadong

2010-11-10

We report the rapid formation of photonic crystal structures by assembly of uniform nonmagnetic colloidal particles in ferrofluids using external magnetic fields. Magnetic manipulation of nonmagnetic particles with size down to a few hundred nanometers, suitable building blocks for producing photonic crystals with band gaps located in the visible regime, has been difficult due to their weak magnetic dipole moment. Increasing the dipole moment of magnetic holes has been limited by the instability of ferrofluids toward aggregation at high concentration or under strong magnetic field. By taking advantage of the superior stability of highly surface-charged magnetite nanocrystal-based ferrofluids, in this paper we have been able to successfully assemble 185 nm nonmagnetic polymer beads into photonic crystal structures, from 1D chains to 3D assemblies as determined by the interplay of magnetic dipole force and packing force. In a strong magnetic field with large field gradient, 3D photonic crystals with high reflectance (83%) in the visible range can be rapidly produced within several minutes, making this general strategy promising for fast creation of large-area photonic crystals using nonmagnetic particles as building blocks.

Crystal structure prediction of flexible molecules using parallel genetic algorithms with a standard force field.

Science.gov (United States)

Kim, Seonah; Orendt, Anita M; Ferraro, Marta B; Facelli, Julio C

2009-10-01

This article describes the application of our distributed computing framework for crystal structure prediction (CSP) the modified genetic algorithms for crystal and cluster prediction (MGAC), to predict the crystal structure of flexible molecules using the general Amber force field (GAFF) and the CHARMM program. The MGAC distributed computing framework includes a series of tightly integrated computer programs for generating the molecule's force field, sampling crystal structures using a distributed parallel genetic algorithm and local energy minimization of the structures followed by the classifying, sorting, and archiving of the most relevant structures. Our results indicate that the method can consistently find the experimentally known crystal structures of flexible molecules, but the number of missing structures and poor ranking observed in some crystals show the need for further improvement of the potential. Copyright 2009 Wiley Periodicals, Inc.

Synthesis, Crystal Structure and Anti-ischaemic Activity of (E)-1-{4 ...

African Journals Online (AJOL)

chloro- phenyl)prop-2-en-1-one (C28H29ClN2O3, Mr = 476.98) (5) was synthesized and studied by the single crystal X-ray diffraction method. Its structure was confirmed by 1HNMR, 13CNMR,HRMSand X-ray single crystal structure ...

Nitrido-technetium(V) complexes with amino acids: Preparation and X-ray crystal structure of the L-cysteinate ethyl ester technetium(V) complex

International Nuclear Information System (INIS)

Marchi, A.; Rossi, R.; Marvelli, L.; Bertolasi, V.

1993-01-01

Technetium-99m is the radionuclide of choice in diagnostic nuclear medicine due to its ideal photon energy of 140 keV and half-life of 6 h. Neutral, stable, and lipophilic technetium complexes with diamino dithiol ligands (DADT) have been widely studied as potential brain perfusion agents and a 99m Tc complex of N,N'-1,2-ethylenediylbis(L-cysteine diethyl ester) (L,L-ECD) has been proposed as a marker of regional cerebral blood flow. It crosses the blood brain barrier (BBB) and is retained in the brain owing to enzymatic hydrolysis of one ester group yielding to a more polar species. More recently, 99m Tc-cysteine complex has been evaluated in animal distribution studies for tumor diagnosis, but its chemical structure has not been determined. A large number of transition metal complexes with amino acids and peptides have been synthesized and structurally characterized to understand their interactions with proteins and antibodies, as well as biocatalytic processes, but only a limited number of rhenium and technetium compounds have been reported. Up to now, the only technetium complex to be characterized by X-ray analysis that contains amino acids as ligand is [TcO(L,L-ECD)]. The author's interest in the nitrido-technetium chemistry is due to the discovery of a new method for preparing radiopharmaceuticals containing the [ 99m Tc triple-bond N] 2+ core. In this communication the authors report the synthesis and characterization of nitrido-technetium complexes with L-cysteine ethyl ester (CYS-OEt), L-cysteine (CYS) and cysteamine (CSA) and the first X-ray crystal structure of a [TcN] 2+ -amino acid complex

Synthesis and structural characterization of bulk Sb2Te3 single crystal

Science.gov (United States)

Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

2018-05-01

We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

Crystal Structure of Human Enterovirus 71

Energy Technology Data Exchange (ETDEWEB)

Plevka, Pavel; Perera, Rushika; Cardosa, Jane; Kuhn, Richard J.; Rossmann, Michael G. (Purdue); (Sentinext)

2013-04-08

Enterovirus 71 is a picornavirus associated with fatal neurological illness in infants and young children. Here, we report the crystal structure of enterovirus 71 and show that, unlike in other enteroviruses, the 'pocket factor,' a small molecule that stabilizes the virus, is partly exposed on the floor of the 'canyon.' Thus, the structure of antiviral compounds may require a hydrophilic head group designed to interact with residues at the entrance of the pocket.

Crystal-Structure-Guided Design of Self-Assembling RNA Nanotriangles.

Science.gov (United States)

Boerneke, Mark A; Dibrov, Sergey M; Hermann, Thomas

2016-03-14

RNA nanotechnology uses RNA structural motifs to build nanosized architectures that assemble through selective base-pair interactions. Herein, we report the crystal-structure-guided design of highly stable RNA nanotriangles that self-assemble cooperatively from short oligonucleotides. The crystal structure of an 81 nucleotide nanotriangle determined at 2.6 Å resolution reveals the so-far smallest circularly closed nanoobject made entirely of double-stranded RNA. The assembly of the nanotriangle architecture involved RNA corner motifs that were derived from ligand-responsive RNA switches, which offer the opportunity to control self-assembly and dissociation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

CCDC 1515632: Experimental Crystal Structure Determination : hexakis(dimethyl sulfoxide)-manganese(ii) tetraiodide

KAUST Repository

Haque, M.A.; Davaasuren, Bambar; Rothenberger, Alexander; Wu, Tao

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

Hydrogen-bonded co-crystal structure of benzoic acid and zwitterionic l-proline

Directory of Open Access Journals (Sweden)

Aaron M. Chesna

2017-03-01

Full Text Available The title compound [systematic name: benzoic acid–pyrrolidin-1-ium-2-carboxylate (1/1], C7H6O2·C5H9NO2, is an example of the application of non-centrosymmetric co-crystallization for the growth of a crystal containing a typically centrosymmetric component in a chiral space group. It co-crystallizes in the space group P212121 and contains benzoic acid and l-proline in equal proportions. The crystal structure exhibits chains of l-proline zwitterions capped by benzoic acid molecules which form a C(5[R33(11] hydrogen-bonded network along [100]. The crystal structure is examined and compared to that of a similar co-crystal containing l-proline zwitterions and 4-aminobenzoic acid.

Crystal structure of Sus scrofa quinolinate phosphoribosyltransferase in complex with nicotinate mononucleotide.

Directory of Open Access Journals (Sweden)

Hyung-Seop Youn

Full Text Available We have determined the crystal structure of porcine quinolinate phosphoribosyltransferase (QAPRTase in complex with nicotinate mononucleotide (NAMN, which is the first crystal structure of a mammalian QAPRTase with its reaction product. The structure was determined from protein obtained from the porcine kidney. Because the full protein sequence of porcine QAPRTase was not available in either protein or nucleotide databases, cDNA was synthesized using reverse transcriptase-polymerase chain reaction to determine the porcine QAPRTase amino acid sequence. The crystal structure revealed that porcine QAPRTases have a hexameric structure that is similar to other eukaryotic QAPRTases, such as the human and yeast enzymes. However, the interaction between NAMN and porcine QAPRTase was different from the interaction found in prokaryotic enzymes, such as those of Helicobacter pylori and Mycobacterium tuberculosis. The crystal structure of porcine QAPRTase in complex with NAMN provides a structural framework for understanding the unique properties of the mammalian QAPRTase active site and designing new antibiotics that are selective for the QAPRTases of pathogenic bacteria, such as H. pylori and M. tuberculosis.

Crystal structure mediates mode of cell death in TiO{sub 2} nanotoxicity

Energy Technology Data Exchange (ETDEWEB)

Braydich-Stolle, Laura K.; Schaeublin, Nicole M.; Murdock, Richard C. [Wright-Patterson AFB, Applied Biotechnology Branch, Human Effectiveness Directorate, Air Force Research Laboratory (United States); Jiang, Jingkun; Biswas, Pratim [Washington University in St. Louis, Department of Energy, Environmental, and Chemical Engineering (United States); Schlager, John J.; Hussain, Saber M., E-mail: Saber.Hussain@wpafb.af.mi [Wright-Patterson AFB, Applied Biotechnology Branch, Human Effectiveness Directorate, Air Force Research Laboratory (United States)

2009-08-15

Certain properties that nanoparticles possess differentiate them from their bulk counterparts, and these characteristics must be evaluated prior to nanoparticle studies and include: size, shape, dispersion, physical and chemical properties, surface area, and surface chemistry. Early nanotoxicity studies evaluating TiO{sub 2} have yielded conflicting data which identify either size or crystal structure as the mediating property for nano-TiO{sub 2} toxicity. However, it is important to note that none of these studies examined size with the crystal structure composition controlled for or examined crystal structure while controlling the nanoparticle size. The goal of this study was to evaluate the role of size and crystal structure in TiO{sub 2} nanotoxicity while controlling for as many other nanoproperties as possible using the HEL-30 mouse keratinocyte cell line as a model for dermal exposure. In the size-dependent studies, all the nanoparticles are 100% anatase, and aggregate sizes were determined in order to take into account the effect of agglomeration on size-dependent toxicity. In addition, varying crystal structures were assessed while the size of the nanoparticles was controlled. We were able to identify that both size and crystal structure contribute to cytotoxicity and that the mechanism of cell death varies based on crystal structure. The 100% anatase TiO{sub 2} nanoparticles, regardless of size, induced cell necrosis, while the rutile TiO{sub 2} nanoparticles initiated apoptosis through formation of reactive oxygen species (ROS).

Comparison of NMR and crystal structures highlights conformational isomerism in protein active sites

International Nuclear Information System (INIS)

Serrano, Pedro; Pedrini, Bill; Geralt, Michael; Jaudzems, Kristaps; Mohanty, Biswaranjan; Horst, Reto; Herrmann, Torsten; Elsliger, Marc-André; Wilson, Ian A.; Wüthrich, Kurt

2010-01-01

Tools for systematic comparisons of NMR and crystal structures developed by the JCSG were applied to two proteins with known functions: the T. maritima anti-σ factor antagonist TM1081 and the mouse γ-glutamylamine cyclotransferase A2LD1 (gi:13879369). In an attempt to exploit the complementarity of crystal and NMR data, the combined use of the two structure-determination techniques was explored for the initial steps in the challenge of searching proteins of unknown functions for putative active sites. The JCSG has recently developed a protocol for systematic comparisons of high-quality crystal and NMR structures of proteins. In this paper, the extent to which this approach can provide function-related information on the two functionally annotated proteins TM1081, a Thermotoga maritima anti-σ factor antagonist, and A2LD1 (gi:13879369), a mouse γ-glutamylamine cyclotransferase, is explored. The NMR structures of the two proteins have been determined in solution at 313 and 298 K, respectively, using the current JCSG protocol based on the software package UNIO for extensive automation. The corresponding crystal structures were solved by the JCSG at 100 K and 1.6 Å resolution and at 100 K and 1.9 Å resolution, respectively. The NMR and crystal structures of the two proteins share the same overall molecular architectures. However, the precision of the structure determination along the amino-acid sequence varies over a significantly wider range in the NMR structures than in the crystal structures. Thereby, in each of the two NMR structures about 65% of the residues have displacements below the average and in both proteins the less well ordered residues include large parts of the active sites, in addition to some highly solvent-exposed surface areas. Whereas the latter show increased disorder in the crystal and in solution, the active-site regions display increased displacements only in the NMR structures, where they undergo local conformational exchange on the

CCDC 1024814: Experimental Crystal Structure Determination : 1,3-Dimesitylimidazolidine-2-selenone

KAUST Repository

Vummaleti, Sai V. C.; Nelson, David J.; Poater, Albert; Gó mez-Suá rez, Adriá n; Cordes, David B.; Slawin, Alexandra M. Z.; Nolan, Steven P.; Cavallo, Luigi

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1446070: Experimental Crystal Structure Determination : tris(Pentafluorophenyl)-(triethylsilyl formate)-boron

KAUST Repository

Chen, Jiawei

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1446069: Experimental Crystal Structure Determination : tris(Pentafluorophenyl)-(triethylsilyl formate)-aluminium

KAUST Repository

Chen, Jiawei

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

Crystal and electronic structure study of Mn doped wurtzite ZnO nanoparticles

Directory of Open Access Journals (Sweden)

O.M. Ozkendir

2016-08-01

Full Text Available The change in the crystal and electronic structure properties of wurtzite ZnO nanoparticles was studied according to Mn doping in the powder samples. The investigations were conducted by X-ray Absorption Fine Structure Spectroscopy (XAFS technique for the samples prepared with different heating and doping processes. Electronic analysis was carried out by the collected data from the X-ray Absorption Near-Edge Structure Spectroscopy (XANES measurements. Additional crystal structure properties were studied by Extended-XAFS (EXAFS analysis. Longer heating periods for the undoped wurtzite ZnO samples were determined to own stable crystal geometries. However, for some doped samples, the distortions in the crystal were observed as a result of the low doping amounts of Mn which was treated as an impurity. Besides, the changes in oxygen locations were determined to create defects and distortions in the samples.

Crystal structure analysis, overexpression and refolding behaviour of a DING protein with single mutation

International Nuclear Information System (INIS)

Gai, Zuoqi; Nakamura, Akiyoshi; Tanaka, Yoshikazu; Hirano, Nagisa; Tanaka, Isao; Yao, Min

2013-01-01

Crystals of a member of the DING protein family (HPBP) were obtained accidentally, and the structure was determined at 1.35 Å resolution. For further analysis, a system for preparation of HPBP was constructed and the structure of a prepared sample was confirmed by X-ray crystal structure analysis at 1.03 Å resolution. After crystallization of a certain protein–RNA complex, well diffracting crystals were obtained. However, the asymmetric unit of the crystal was too small to locate any components. Mass spectrometry and X-ray crystal structure analysis showed that it was a member of the DING protein family (HPBP). Surprisingly, the structure of HPBP reported previously was also determined accidentally as a contaminant, suggesting that HPBP has a strong tendency to crystallize. Furthermore, DING proteins were reported to relate in disease. These observations suggest that DING has potential for application in a wide range of research fields. To enable further analyses, a system for preparation of HPBP was constructed. As HPBP was expressed in insoluble form in Escherichia coli, it was unfolded chemically and refolded. Finally, a very high yield preparation method was constructed, in which 43 mg of HPBP was obtained from 1 L of culture. Furthermore, to evaluate the validity of refolding, its crystal structure was determined at 1.03 Å resolution. The determined structure was identical to the native structure, in which two disulfide bonds were recovered correctly and a phosphate ion was captured. Based on these results, it was concluded that the refolded HPBP recovers its structure correctly

Crystal structure analysis, overexpression and refolding behaviour of a DING protein with single mutation

Energy Technology Data Exchange (ETDEWEB)

Gai, Zuoqi; Nakamura, Akiyoshi [Hokkaido University, Sapporo 060-0810 (Japan); Tanaka, Yoshikazu, E-mail: tanaka@sci.hokudai.ac.jp [Hokkaido University, Sapporo 060-0810 (Japan); Hokkaido University, Sapporo 060-0810 (Japan); Hirano, Nagisa [Hokkaido University, Sapporo 060-0810 (Japan); Tanaka, Isao; Yao, Min [Hokkaido University, Sapporo 060-0810 (Japan); Hokkaido University, Sapporo 060-0810 (Japan)

2013-11-01

Crystals of a member of the DING protein family (HPBP) were obtained accidentally, and the structure was determined at 1.35 Å resolution. For further analysis, a system for preparation of HPBP was constructed and the structure of a prepared sample was confirmed by X-ray crystal structure analysis at 1.03 Å resolution. After crystallization of a certain protein–RNA complex, well diffracting crystals were obtained. However, the asymmetric unit of the crystal was too small to locate any components. Mass spectrometry and X-ray crystal structure analysis showed that it was a member of the DING protein family (HPBP). Surprisingly, the structure of HPBP reported previously was also determined accidentally as a contaminant, suggesting that HPBP has a strong tendency to crystallize. Furthermore, DING proteins were reported to relate in disease. These observations suggest that DING has potential for application in a wide range of research fields. To enable further analyses, a system for preparation of HPBP was constructed. As HPBP was expressed in insoluble form in Escherichia coli, it was unfolded chemically and refolded. Finally, a very high yield preparation method was constructed, in which 43 mg of HPBP was obtained from 1 L of culture. Furthermore, to evaluate the validity of refolding, its crystal structure was determined at 1.03 Å resolution. The determined structure was identical to the native structure, in which two disulfide bonds were recovered correctly and a phosphate ion was captured. Based on these results, it was concluded that the refolded HPBP recovers its structure correctly.

Reversible Single-Crystal-to-Single-Crystal Structural Transformation in a Mixed-Ligand 2D Layered Metal-Organic Framework: Structural Characterization and Sorption Study

Directory of Open Access Journals (Sweden)

Chih-Chieh Wang

2017-12-01

Full Text Available A 3D supramolecular network, [Cd(bipy(C4O4(H2O2]·3H2O (1 (bipy = 4,4′-bipyridine and C4O42− = dianion of H2C4O4, constructed by mixed-ligand two-dimensional (2D metal-organic frameworks (MOFs has been reported and structurally determined by the single-crystal X-ray diffraction method and characterized by other physicochemical methods. In 1, the C4O42− and bipy both act as bridging ligands connecting the Cd(II ions to form a 2D layered MOF, which are then extended to a 3D supramolecular network via the mutually parallel and interpenetrating arrangements among the 2D-layered MOFs. Compound 1 shows a two-step dehydration process with weight losses of 11.0% and 7.3%, corresponding to the weight-loss of three guest and two coordinated water molecules, respectively, and exhibits an interesting reversible single-crystal-to-single-crystal (SCSC structural transformation upon de-hydration and re-hydration for guest water molecules. The SCSC structural transformation have been demonstrated and monitored by single-crystal and X-ray powder diffraction, and thermogravimetic analysis studies.

Rhenium-catalyzed dehydrogenative olefination of C(sp(3))-H bonds with hypervalent iodine(III) reagents.

Science.gov (United States)

Gu, Haidong; Wang, Congyang

2015-06-07

A dehydrogenative olefination of C(sp(3))-H bonds is disclosed here, by merging rhenium catalysis with an alanine-derived hypervalent iodine(III) reagent. Thus, cyclic and acyclic ethers, toluene derivatives, cycloalkanes, and nitriles are all successfully alkenylated in a regio- and stereoselective manner.

On structure of some laminated crystals with organic molecules

International Nuclear Information System (INIS)

Volodina, G.F.; Ivanova, V.Ya.; Malinovskij, T.I.

1982-01-01

A survey is made of papers dealing with intercalation of organic molecules into crystals of dihalcogenides of some transition metals (TaS 2 , TiS 2 , NbS 2 , ZrS 2 , TaSe 2 ), variation of their structure and physical properties. Among the used intercalates ammonia, pyridine, aniline and other aromatic amines proved to be most satisfactory from the viewpoint of reaction rate and product stability. A possibility is discussed of intercalation into PbI 2 and CdI 2 crystals that are of the same structural type as dihalcogenides

Solid-state thermolysis of a fac-rhenium(I) carbonyl complex with a redox non-innocent pincer ligand.

Science.gov (United States)

Jurca, Titel; Chen, Wen-Ching; Michel, Sheila; Korobkov, Ilia; Ong, Tiow-Gan; Richeson, Darrin S

2013-03-25

The development of rhenium(I) chemistry has been restricted by the limited structural and electronic variability of the common pseudo-octahedral products fac-[ReX(CO)3L2] (L2 = α-diimine). We address this constraint by first preparing the bidentate bis(imino)pyridine complexes [(2,6-{2,6-Me2C6H3N=CPh}2C5H3N)Re(CO)3X] (X = Cl 2, Br 3), which were characterized by spectroscopic and X-ray crystallographic means, and then converting these species into tridentate pincer ligand compounds, [(2,6-{2,6-Me2C6H3N=CPh}2C5H3N)Re(CO)2X] (X = Cl 4, Br 5). This transformation was performed in the solid-state by controlled heating of 2 or 3 above 200 °C in a tube furnace under a flow of nitrogen gas, giving excellent yields (≥95 %). Compounds 4 and 5 define a new coordination environment for rhenium(I) carbonyl chemistry where the metal center is supported by a planar, tridentate pincer-coordinated bis(imino)pyridine ligand. The basic photophysical features of these compounds show significant elaboration in both number and intensity of the d-π* transitions observed in the UV/Vis spec tra relative to the bidentate starting materials, and these spectra were analyzed using time-dependent DFT computations. The redox nature of the bis(imino)pyridine ligand in compounds 2 and 4 was examined by electrochemical analysis, which showed two ligand reduction events and demonstrated that the ligand reduction shifts to a more positive potential when going from bidentate 2 to tridentate 4 (+160 mV for the first reduction step and +90 mV for the second). These observations indicate an increase in electrostatic stabilization of the reduced ligand in the tridentate conformation. Elaboration on this synthetic methodology documented its generality through the preparation of the pseudo-octahedral rhenium(I) triflate complex [(2,6-{2,6-Me2C6H3N=CPh}2C5H3N)Re(CO)2OTf] (7, 93 % yield). Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Theoretical Exploration of Various Lithium Peroxide Crystal Structures in a Li-Air Battery

Directory of Open Access Journals (Sweden)

Kah Chun Lau

2015-01-01

Full Text Available We describe a series of metastable Li2O2 crystal structures involving different orientations and displacements of the O22− peroxy ions based on the known Li2O2 crystal structure. Within the vicinity of the chemical potential ΔG ~ 0.20 eV/Li from the thermodynamic ground state of the Li2O2 crystal structure (i.e., Föppl structure, all of these newly found metastable Li2O2 crystal structures are found to be insulating and high-k materials, and they have a common unique signature of an O22− O-O vibration mode (ω ~ 799–865 cm−1, which is in the range of that commonly observed in Li-air battery experiments, regardless of the random O22− orientations and the symmetry in the crystal lattice. From XRD patterns analysis, the commercially available Li2O2 powder is confirmed to be the thermodynamic ground state Föppl-like structure. However, for Li2O2 compounds that are grown electrochemically under the environment of Li-O2 cells, we found that the XRD patterns alone are not sufficient for structural identification of these metastable Li2O2 crystalline phases due to the poor crystallinity of the sample. In addition, the commonly known Raman signal of O22− vibration mode is also found to be insufficient to validate the possible existence of these newly predicted Li2O2 crystal structures, as all of them similarly share the similar O22− vibration mode. However considering that the discharge voltage in most Li-O2 cells are typically several tenths of an eV below the thermodynamic equilibrium for the formation of ground state Föppl structure, the formation of these metastable Li2O2 crystal structures appears to be thermodynamically feasible.

Polarization singularities of optical fields caused by structural dislocations in crystals

International Nuclear Information System (INIS)

Savaryn, V; Vasylkiv, Yu; Krupych, O; Skab, I; Vlokh, R

2013-01-01

We analyze polarization singularities of optical beams that propagate through crystals possessing structural dislocations. We show that screw dislocations of crystalline structure can lead to the appearance of purely screw-type dislocations of light wavefronts. This can happen only in crystals that belong to trigonal and cubic systems. These polarization singularities will give rise to optical vortices with the topological charge equal to ±1, whenever a crystal sample is placed between crossed circular polarizers. We have also found that edge dislocations present in the cubic and trigonal crystals, with the Burgers vector perpendicular to the three-fold symmetry axes, can impose mixed screw-edge dislocations in the wavefronts of optical beams and generate singly charged optical vortices. The results of our analysis can be applied for detecting and identifying dislocations of different types available in crystals. (paper)

Hydrothermal synthesis, crystal structure and luminescence property ...

Indian Academy of Sciences (India)

The design and construction of ... dination polymers. It is difficult to design coordination .... The first endotherm at about 180 ... graphic data for coordination polymer 1. ... Sheldrick G M 1997 SHELXS-97: Program for solution of crystal structures ...

Crystal structure of N′-hydroxypyrimidine-2-carboximidamide

Directory of Open Access Journals (Sweden)

Nithianantham Jeeva Jasmine

2014-10-01

Full Text Available The title compound, C5H6N4O, is approximately planar, with an angle of 11.04 (15° between the planes of the pyrimidine ring and the non-H atoms of the carboximidamide unit. The molecule adopts an E configuration about the C=N double bond. In the crystal, adjacent molecules are linked by pairs of N—H...O hydrogen bonds, forming inversion dimers with an R22(10 ring motif. The dimers are further linked via N—H...N and O—H...N hydrogen bonds into a sheet structure parallel to the ac plane. The crystal structure also features N—H...O and weak C—H...O hydrogen bonds and offset π–π stacking interactions between adjacent pyrimidine rings [centroid–centroid distance = 3.622 (1 Å].

Structural templating in a nonplanar phthalocyanine using single crystal copper iodide

OpenAIRE

Rochford, L. A. (Luke A.); Ramadan, Alexandra J.; Keeble, Dean S.; Ryan, Mary P.; Heutz, Sandrine; Jones, T. S. (Tim S.)

2015-01-01

Solution-grown copper iodide crystals are used as substrates for the templated growth of the nonplanar vanadyl phthalocyanine using organic molecular beam deposition. Structural characterization reveals a single molecular orientation produced by the (111) Miller plane of the copper iodide crystals. These fundamental measurements show the importance of morphology and structure in templating interactions for organic electronics applications.

New extraction chromatographic material for rhenium separation

International Nuclear Information System (INIS)

Lucanikova, M.; Czech Technical University, Prague; Kucera, J.; Czech Technical University, Prague; Sebesta, F.

2008-01-01

Three types of the extraction chromatographic materials, composed from Aliquat R 336 deposited in the polyacrylonitrile (PAN) beads and prepared by different procedures, were compared for extraction of rhenium. The best properties were exhibited when the solid extractant was prepared by impregnation of the ready-made PAN beads. Solid extractant prepared by direct coagulation of the beads from the suspension of Aliquat R 336 in solution of PAN in nitric acid differs only by lower capacity in dynamic conditions. Material prepared from the PAN solution in dimethylsulfoxide was the worst because Aliquat R 336 was washed out from the beads during coagulation of the polymer and the extraction capacity was low. As it is shown, the first two solid extractants are fully comparable with the commercial TEVA Resin. (author)

High-Q microwave resonators with a photonic crystal structure

International Nuclear Information System (INIS)

Schuster, M.

2001-08-01

The localisation of electromagnetic energy at a defect in a photonic crystal is similar to a well known effect employed to construct high-Q microwave resonators: In a whispering gallery (WHG-) mode resonator the high Q-factor is achieved by localisation of the electromagnetic field energy by total reflection inside a disk made of dielectric material. The topic of this work is to demonstrate, that WHG-like modes can exist in an air defect in a photonic crystal that extends over several lattice periods; and that a high-Q microwave resonator can be made, utilizing these resonant modes. In numerical simulations, the transmission properties of a photonic crystal structure with hexagonal lattice symmetry have been investigated with a transfer-matrix-method. The eigenmodes of a defect structure in a photonic crystal have been calculated with a quasi-3d finite element integration technique. Experimental results confirm the simulated transmission properties and show the existence of modes inside the band gap, when a defect is introduced in the crystal. Resonator measurements show that a microwave resonator can be operated with those defect modes. It was found out that the main losses of the resonator were caused by bad microwave properties of the used dielectric material and by metal losses on the top and bottom resonator walls. Furthermore, it turned out that the detection of the photonic crystal defect mode was difficult because of a lack of simulation possibilities and high housing mode density in the resonator. (orig.)

Ab initio molecular crystal structures, spectra, and phase diagrams.

Science.gov (United States)

Hirata, So; Gilliard, Kandis; He, Xiao; Li, Jinjin; Sode, Olaseni

2014-09-16

Conspectus Molecular crystals are chemists' solids in the sense that their structures and properties can be understood in terms of those of the constituent molecules merely perturbed by a crystalline environment. They form a large and important class of solids including ices of atmospheric species, drugs, explosives, and even some organic optoelectronic materials and supramolecular assemblies. Recently, surprisingly simple yet extremely efficient, versatile, easily implemented, and systematically accurate electronic structure methods for molecular crystals have been developed. The methods, collectively referred to as the embedded-fragment scheme, divide a crystal into monomers and overlapping dimers and apply modern molecular electronic structure methods and software to these fragments of the crystal that are embedded in a self-consistently determined crystalline electrostatic field. They enable facile applications of accurate but otherwise prohibitively expensive ab initio molecular orbital theories such as Møller-Plesset perturbation and coupled-cluster theories to a broad range of properties of solids such as internal energies, enthalpies, structures, equation of state, phonon dispersion curves and density of states, infrared and Raman spectra (including band intensities and sometimes anharmonic effects), inelastic neutron scattering spectra, heat capacities, Gibbs energies, and phase diagrams, while accounting for many-body electrostatic (namely, induction or polarization) effects as well as two-body exchange and dispersion interactions from first principles. They can fundamentally alter the role of computing in the studies of molecular crystals in the same way ab initio molecular orbital theories have transformed research practices in gas-phase physical chemistry and synthetic chemistry in the last half century. In this Account, after a brief summary of formalisms and algorithms, we discuss applications of these methods performed in our group as compelling

Crystallization Process of Protein Rv0731c from Mycobacterium Tuberculosis for a Successful Atomic Resolution Crystal Structure at 1.2 Angstrom

Energy Technology Data Exchange (ETDEWEB)

Zhu, Liang Cong

2009-06-08

Proteins are bio-macromolecules consisting of basic 20 amino acids and have distinct three-dimensional folds. They are essential parts of organisms and participate in every process within cells. Proteins are crucial for human life, and each protein within the body has a specific function, such as antibodies, contractile proteins, enzymes, hormonal proteins, structural proteins, storage proteins and transport proteins. Determining three-dimensional structure of a protein can help researchers discover the remarkable protein folding, binding site, conformation and etc, in order to understand well of protein interaction and aid for possible drug design. The research on protein structure by X-ray protein crystallography carried by Li-Wei Hung's research group in the Physical Bioscience Division at Lawrence Berkeley National Laboratory (LBNL) is focusing on protein crystallography. The research in this lab is in the process of from crystallizing the proteins to determining the three dimensional crystal structures of proteins. Most protein targets are selected from Mycobacterium Tuberculosis. TB (Tuberculosis) is a possible fatal infectious disease. By studying TB target protein can help discover antituberculer drugs, and find treatment for TB. The high-throughput mode of crystallization, crystal harvesting, crystal screening and data collection are applied to the research pipeline (Figure 1). The X-ray diffraction data by protein crystals can be processed and analyzed to result in a three dimensional representation of electron density, producing a detailed model of protein structure. Rv0731c is a conserved hypothetical protein with unknown function from Mycobacterium Tuberculosis. This paper is going to report the crystallization process and brief structure information of Rv0731c.

The process development of laser surface modification of commercially pure titanium (Grade 2) with rhenium

Science.gov (United States)

Kobiela, K.; Smolina, I.; Dziedzic, R.; Szymczyk, P.; Kurzynowski, T.; Chlebus, E.

2016-12-01

The paper presents the results of the process development of laser surface modification of commercially pure titanium with rhenium. The criterion of the successful/optimal process is the repetitive geometry of the surface, characterized by predictable and repetitive chemical composition over its entire surface as well as special mechanical properties (hardness and wear resistance). The analysis of surface geometry concluded measurements of laser penetration depth and heat affected zone (HAZ), the width of a single track as well as width of a clad. The diode laser installed on the industrial robot carried out the laser treatment. This solution made possible the continuous supply of powder to the substrate during the process. The aim of an investigation is find out the possibility of improving the tribological characteristics of the surface due to the rhenium alloying. The verification of the surface properties (tribological) concluded geometry measurements, microstructure observation, hardness tests and evaluation of wear resistance.

Molecular Complex of Lumiflavin and 2-Aminobenzoic Acid : Crystal Structure, Crystal Spectra, and Solution Properties

OpenAIRE

Shieh, Huey-Sheng; Ghisla, Sandro; Hanson, Louise Karle; Ludwig, Martha L.; Nordman, Christer E.

1981-01-01

The molecular complex lumiflavin-2-aminobenzoic acid monohydrate (C13H12N402●C7H7N02●H2O)crystallizes from aqueous solution as red triclinic prisms. The space group is P1 with cell dimensions a = 9.660 A, b = 14.866 Å, c = 7.045 Å, α = 95.44°, β = 95.86°, and γ = 105.66°. The crystal structure was solved by direct methods and refined by block-diagonal least-squares procedures to an R value of 0.050 on the basis of 1338 observed reflections. The structure is composed of stacks of alternating l...

Synthesis, crystal structure, physicochemical properties of hydrogen bonded supramolecular assembly of N,N-diethylanilinium-3, 5-dinitrosalicylate crystal

Science.gov (United States)

Rajkumar, M.; Chandramohan, A.

2017-12-01

An organic salt, N,N-diethylanilinium 3,5-dinitrosalicylate was synthesized and single crystals grown by employing the slow solvent evaporation solution growth technique in methanol-acetone (1:1) mixture. The electronic transitions of the salt crystal were studied by UV-Visible spectrum. The optical transmittance window and lower wavelength cut-off of grown crystal have been identified by UV-Vis-NIR studies. The FT-IR spectrum was recorded to confirm the presence of various functional groups in the grown crystal. 1H and 13C NMR spectrum were recorded to establish the molecular structure of the title crystal. Single crystal X-ray diffraction data indicated that the crystal belongs to monoclinic crystal system with P21/n space group. The thermal stability of the crystal was established by TG/DTA studies. The mechanical properties of the grown crystal were studied by Vickers' microhardness technique. The dielectric studies indicated that the dielectric constant and dielectric loss decrease exponentially with frequency at different temperatures.

Investigation of melt structure and crystallization processes by high-temperature Raman spectroscopy method

International Nuclear Information System (INIS)

Voron'ko, Yu.K.; Kudryavtsev, A.B.; Osiko, V.V.; Sobol', A.A.

1988-01-01

A review of studies dealing with the melts of alkali, rare earth and other element phosphates, gallates, germanates, niobates and tungstates, which are carried out by the method of high-temperature Raman spectroscopy, is given. The effect of the melt structure on the mechanism of the substance cystallization is considered. It is shown that vitrification and supercooling of the melt, as well as its crystallization in the from of metastable structures, are related to the effect of nonconformity between the melt and crystal strucure. The effect of nonconformity between anion motives in the melt and crystal creates obstacles for equilibrium structure nucleation, which results in the formation mainly of metastable forms with lattice structure for from the structure of the melt, though cases of equilibrium phase crystallization are also possible. 37 refs.; 13 figs.; 2 tabs

Confirming the Revised C-Terminal Domain of the MscL Crystal Structure

OpenAIRE

Maurer, Joshua A.; Elmore, Donald E.; Clayton, Daniel; Xiong, Li; Lester, Henry A.; Dougherty, Dennis A.

2008-01-01

The structure of the C-terminal domain of the mechanosensitive channel of large conductance (MscL) has generated significant controversy. As a result, several structures have been proposed for this region: the original crystal structure (1MSL) of the Mycobacterium tuberculosis homolog (Tb), a model of the Escherichia coli homolog, and, most recently, a revised crystal structure of Tb-MscL (2OAR). To understand which of these structures represents a physiological conformation, we measured the ...

Crystal structure representations for machine learning models of formation energies

Energy Technology Data Exchange (ETDEWEB)

Faber, Felix [Department of Chemistry, Institute of Physical Chemistry and National Center for Computational Design and Discovery of Novel Materials, University of Basel Switzerland; Lindmaa, Alexander [Department of Physics, Chemistry and Biology, Linköping University, SE-581 83 Linköping Sweden; von Lilienfeld, O. Anatole [Department of Chemistry, Institute of Physical Chemistry and National Center for Computational Design and Discovery of Novel Materials, University of Basel Switzerland; Argonne Leadership Computing Facility, Argonne National Laboratory, 9700 S. Cass Avenue Lemont Illinois 60439; Armiento, Rickard [Department of Physics, Chemistry and Biology, Linköping University, SE-581 83 Linköping Sweden

2015-04-20

We introduce and evaluate a set of feature vector representations of crystal structures for machine learning (ML) models of formation energies of solids. ML models of atomization energies of organic molecules have been successful using a Coulomb matrix representation of the molecule. We consider three ways to generalize such representations to periodic systems: (i) a matrix where each element is related to the Ewald sum of the electrostatic interaction between two different atoms in the unit cell repeated over the lattice; (ii) an extended Coulomb-like matrix that takes into account a number of neighboring unit cells; and (iii) an ansatz that mimics the periodicity and the basic features of the elements in the Ewald sum matrix using a sine function of the crystal coordinates of the atoms. The representations are compared for a Laplacian kernel with Manhattan norm, trained to reproduce formation energies using a dataset of 3938 crystal structures obtained from the Materials Project. For training sets consisting of 3000 crystals, the generalization error in predicting formation energies of new structures corresponds to (i) 0.49, (ii) 0.64, and (iii) 0.37eV/atom for the respective representations.

Origin of the complex crystal structures of elements at intermediate pressure

International Nuclear Information System (INIS)

Ackland, G J; Macleod, I R

2004-01-01

We present a unifying theory for the observed complex structures of sp-bonded elements under pressure on the basis of nearly free electron picture. In the intermediate pressure regime, the dominant contribution to crystal structure arises from Fermi-surface Brillouin zone interactions-structures which allow this are favoured. This simple theory explains the observed crystal structures, transport properties and the evolution of internal and unit cell parameters with pressure and appears to hold for elements in groups I-VI. We illustrate it with experimental data for these elements and ab initio calculations for Li

Band structures and localization properties of aperiodic layered phononic crystals

Energy Technology Data Exchange (ETDEWEB)

Yan Zhizhong, E-mail: zzyan@bit.edu.cn [Department of Applied Mathematics, Beijing Institute of Technology, Beijing 100081 (China); Zhang Chuanzeng [Department of Civil Engineering, University of Siegen, D-57078 Siegen (Germany)

2012-03-15

The band structures and localization properties of in-plane elastic waves with coupling of longitudinal and transverse modes oblique propagating in aperiodic phononic crystals based on Thue-Morse and Rudin-Shapiro sequences are studied. Using transfer matrix method, the concept of the localization factor is introduced and the correctness is testified through the Rytov dispersion relation. For comparison, the perfect periodic structure and the quasi-periodic Fibonacci system are also considered. In addition, the influences of the random disorder, local resonance, translational and/or mirror symmetries on the band structures of the aperiodic phononic crystals are analyzed in this paper.

Potassium and magnesium succinatouranilates – Synthesis and crystal structure

Energy Technology Data Exchange (ETDEWEB)

Novikov, S.A., E-mail: serg.alex.novikov@gmail.com [Samara National Research University, 443086 Samara (Russian Federation); Grigoriev, M.S. [Frumkin Institute of Physical Chemistry and Electrochemistry RAS, 119071 Moscow (Russian Federation); Serezhkina, L.B.; Serezhkin, V.N. [Samara National Research University, 443086 Samara (Russian Federation)

2017-04-15

Single crystal X-ray diffraction has been applied to determine the structures of two new uranyl coordination polymers: K{sub 2}[(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}] (1) and [Mg(H{sub 2}O){sub 6}] [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]·2H{sub 2}O (2), where C{sub 4}H{sub 4}O{sub 4}{sup 2-} is succinate anion. Crystals of 1 and 2 contain polymeric complex anions [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]{sup 2-} with the same A{sub 2}Q{sup 02}{sub 3} crystallochemical formula (A=UO{sub 2}{sup 2+}, Q{sup 02}=C{sub 4}O{sub 4}H{sub 4}{sup 2-}), and have layered (1) or chain (2) structure. It has been found, that conformation of succinate ions is one of the factors, which affects the structure of [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]{sup 2-} anions. IR spectra of these new compounds are in good agreement with crystallographic data. Topological analysis of the uranium dicarboxylates with A{sub 2}Q{sup 02}{sub 3} crystallochemical formula has shown the presence of five isomers which differ from each other in coordination sequences and / or dimensionality. - Graphical abstract: Crystal structures of two new uranium(VI) coordination polymers with succinate linkers, namely K{sub 2}[(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}] (1) and [Mg(H{sub 2}O){sub 6}][(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]·2H{sub 2}O (2), were determined by single-crystal XRD. Crystals of studied compounds are based on 2D or 1D structural units with the same composition and crystallochemical formula. Topological isomerism in A{sub 2}Q{sup 02}{sub 3} crystallochemical group and conformations of succinate anions in uranyl complexes are under discussion. - Highlights: • Two new uranium coordination polymers were synthesized. • Their structural units have the same composition and crystallochemical formula. • In spite the same composition and CCF dimensionality of units is different. • Structural features of uranyl CPs

Molecular Dynamic Simulation of Space and Earth-Grown Crystal Structures of Thermostable T1 Lipase Geobacillus zalihae Revealed a Better Structure.

Science.gov (United States)

Ishak, Siti Nor Hasmah; Aris, Sayangku Nor Ariati Mohamad; Halim, Khairul Bariyyah Abd; Ali, Mohd Shukuri Mohamad; Leow, Thean Chor; Kamarudin, Nor Hafizah Ahmad; Masomian, Malihe; Rahman, Raja Noor Zaliha Raja Abd

2017-09-25

Less sedimentation and convection in a microgravity environment has become a well-suited condition for growing high quality protein crystals. Thermostable T1 lipase derived from bacterium Geobacillus zalihae has been crystallized using the counter diffusion method under space and earth conditions. Preliminary study using YASARA molecular modeling structure program for both structures showed differences in number of hydrogen bond, ionic interaction, and conformation. The space-grown crystal structure contains more hydrogen bonds as compared with the earth-grown crystal structure. A molecular dynamics simulation study was used to provide insight on the fluctuations and conformational changes of both T1 lipase structures. The analysis of root mean square deviation (RMSD), radius of gyration, and root mean square fluctuation (RMSF) showed that space-grown structure is more stable than the earth-grown structure. Space-structure also showed more hydrogen bonds and ion interactions compared to the earth-grown structure. Further analysis also revealed that the space-grown structure has long-lived interactions, hence it is considered as the more stable structure. This study provides the conformational dynamics of T1 lipase crystal structure grown in space and earth condition.

Protein NMR Structures Refined with Rosetta Have Higher Accuracy Relative to Corresponding X-ray Crystal Structures

Science.gov (United States)

2014-01-01

We have found that refinement of protein NMR structures using Rosetta with experimental NMR restraints yields more accurate protein NMR structures than those that have been deposited in the PDB using standard refinement protocols. Using 40 pairs of NMR and X-ray crystal structures determined by the Northeast Structural Genomics Consortium, for proteins ranging in size from 5–22 kDa, restrained Rosetta refined structures fit better to the raw experimental data, are in better agreement with their X-ray counterparts, and have better phasing power compared to conventionally determined NMR structures. For 37 proteins for which NMR ensembles were available and which had similar structures in solution and in the crystal, all of the restrained Rosetta refined NMR structures were sufficiently accurate to be used for solving the corresponding X-ray crystal structures by molecular replacement. The protocol for restrained refinement of protein NMR structures was also compared with restrained CS-Rosetta calculations. For proteins smaller than 10 kDa, restrained CS-Rosetta, starting from extended conformations, provides slightly more accurate structures, while for proteins in the size range of 10–25 kDa the less CPU intensive restrained Rosetta refinement protocols provided equally or more accurate structures. The restrained Rosetta protocols described here can improve the accuracy of protein NMR structures and should find broad and general for studies of protein structure and function. PMID:24392845

Synthesis and Single Crystal X-Ray Structure Determination of 3,3',5 ...

African Journals Online (AJOL)

Single crystal structure determination at 100 K revealed needle-like crystals in an orthorhombic crystal system. The asymmetric unit of the cell consists of an isolated chloride ion, one half of a tetrahedral [MnCl4]2- anion, a [H2Me4bpz]2+ dication and one half of a molecule of water. Keywords: Crystal Engineering, Hydrogen ...

Preparation and crystal structure of Ca4Sb2O

International Nuclear Information System (INIS)

Eisenmann, B.; Limartha, H.; Schaefer, H.

1980-01-01

The formerly described compound Ca 2 Sb is to be corrected to Ca 4 Sb 2 O as shown by X-ray diffractometer data of single crystals and neutron diffraction diagrams of powders. The compound crystallizes in the K 2 NiF 4 structure type. (orig.)

The crystal structure and the phase transitions of pyridinium trifluoromethanesulfonate

International Nuclear Information System (INIS)

Jesariew, Dominik; Ilczyszyn, Maria M; Pietraszko, Adam

2014-01-01

The calorimetric and optical studies and the structural properties of pyridinium trifluoromethanesulfonate (abbreviated as PyHOTf) are reported. A sequence of four fully reversible solid–solid phase transitions, at 223.0, 309.0, 359.9 and 394.3 K, has been discovered. The phase transition sequence was confirmed by x-ray diffraction data. The crystal structures of three phases (V, IV and III) have been determined from the single crystal x-ray diffraction data. Structural properties of the high temperature phases are characterized using powder x-ray diffraction data measured in the 290–425 K temperature range. The structural changes triggered by the temperature change are discussed in relation to the phase transitions. Two low temperature phases (V and IV) belong to the P4 3 2 1 2 space group of the tetragonal system. The intermediate phases (III and II) are monoclinic and the prototype high temperature phase (I) is a pseudo-cubic (tetragonal) one. The low temperature phases (V and IV) are well ordered. The crystal structure of intermediate (III and II) and prototype (I) phases are characterized by high disorder of the pyridinium cations and triflate anions. (papers)

An arc detector for neutron crystal structure investigations

Energy Technology Data Exchange (ETDEWEB)

Habib, N [Reactor and Neutron Physics Dept., Nuclear Research Center. AEA, Cairo (Egypt)

1997-12-31

An arc detector for neutron structure investigations of powder crystals using time-of-flight technique is described. In order to enable the measurement of integral intensity from about 1/4 of the Debye-Scherrer ring and for simplicity reasons, the scattering angle 20-90 degree was chosen and a special arc collimator was built. The arc collimator-detector had a divergency of about 20 minutes of arc, and the distance between detector-sample was 64 cm. Four {sup 3} He detectors were fixed on the arc of the collimator. Both efficiency and space sensitivity of the detector were determined using a point neutron source. Results of measurements show that parameters of the arc detector are acceptable for high resolution crystal structure investigations. 6 figs.

Rhenium-186 direct labelling HIgG

International Nuclear Information System (INIS)

Lungu, V.; Mihailescu, G.; Dumitrescu, G.

2001-01-01

The aim of this study is to develop and improve existing radiolabelling techniques of peptides and monoclonal antibodies with 186 Re for achievement of potential agents for cancer targeted radiotherapy. There were selected methods and techniques for the direct labelling of intact HIgG by studding chemical and radiochemical processes of -S-S- bridges prereduction, reduction of 186 ReO 4 - and coupling reaction of rhenium with HIgG. The -S-S- bridges prereduction of HIgG to sulfhydryls was effected using different reducing agents: ascorbic acid, 2,3 dimercaptopropanol, cysteine, active hydrogen. The prereduction reactions are controlled by masic ratios of HIgG/reduction agent, pH, temperature and time of incubation. A pH=4.5 and a 24 hours incubation time are in the advantage of the prereduction yield. The labelling with 186 Re of prereduced HIgG with ascorbic acid or active hydrogen and 37 deg. C incubation in 22 hours releases 92% radiochemical purity. (author)

Atomic structures and mechanical properties of single-crystal GaN nanotubes

International Nuclear Information System (INIS)

Xu, B.; Lu, A.J.; Pan, B.C.; Yu, Q.X.

2005-01-01

An approach is proposed to theoretically construct a realistic single-crystal GaN nanotube at atomic scale. The generated atomic structures of the single-crystal GaN nanotubes match the structural aspects from experiment very well. Our energetic calculations show that a single-crystal GaN nanotube with [100]-oriented lateral facets is more stable than that with [110]-oriented lateral facets, when they have around the same wall thickness. For a specified orientation of the lateral facets on the single-crystal GaN nanotubes, the energetic stabilities of the tubes obey a P rule, in which P is the ratio of the number of four-coordinated atoms to the number of three-coordinated atoms. Furthermore, the Young's modulus of the considered GaN nanotubes decrease with increasing the ratio of the number of bulk atoms to the number of surface atoms in each type of tube. Our calculations and analysis demonstrate that the surface effect of a single-crystal nanotube enhances its Young's modulus significantly

Liquid kit for preparation of {sup 188}rhenium-etidronate

Energy Technology Data Exchange (ETDEWEB)

Marczewski, Barbara; Dias, Carla Roberta; Moraes, Vanessa; Osso Junior, Joao Alberto [Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP), SP (Brazil). Centro de Radiofarmacia]. E-mail: baszot@gmail.com

2005-10-15

The aim of this study was the preparation of a liquid kit for radiolabeling of {sup 188} Re-HEDP (hydroxyethylidene diphosphonate). {sup 188} Re was obtained from alumina based {sup 188} W/{sup 188} Re generators. This paper reports the efficacy of a cold kit stored for more than two weeks, determined by the dependence of the radiolabeling yields of {sup 188} Re-HEDP on the incubation time, reducing agent concentration, the effects of concentration of ligand, the p H of the reaction and the temperature. The cold kits showed a good stability when carrie-free rhenium-188 was added in the reaction mixture. (author)

Kinetics and mechanism of nitrobenzene hydrogenation to phenylhydroxylamine in rhenium thiocomplexes solutions

International Nuclear Information System (INIS)

Korenyako, G.I.; Belousov, V.M.

1985-01-01

A study was made on kinetics of nitrobenzene hydrogenation to phenylhydroxylamine in dimethylformamide solutions of rhenium thiocomplexes. The mechanism of hydrogenation was suggested. Formation of hydride catalyst complex represents the first stage of the process. Kinetic equation derived on the basis of suggested mechanism corresponds satisfactorily with experimental results. Thermodynamic parameters of separate process stages calculated on the basis of equilibrium constant values testify as well to the benefit of suggested mechanism

Formamidine sulfinic acid as reducing agent in technetium-99m rhenium sulfide labelling

Energy Technology Data Exchange (ETDEWEB)

Neves, M; Patricio, L [Laboratorio Nacional de Engenharia e Technologia Industrial, Sacavem (Portugal). Dept. de Radioisotopes; Ferronha, H [Laboratorio Nacional de Investigacao Veterinaria, Lisboa (Portugal)

1989-08-01

Labelling kinetic studies, radiochemical characterization and particle size evaluation of {sup 99m}Tc rhenium sulfide colloid using formamidine sulfinic acid as reducing agent are described. Comparison with the same colloid which makes use of Sn-sodium pyrophosphate complex as reducing agent showed higher labelling yields, simplification of labelling procedure and a longer shelf life when formamidine sulfinic acid was used. (author) 15 refs.; 7 figs.

Growth and structural, optical, and electrical properties of zincite crystals

Science.gov (United States)

Kaurova, I. A.; Kuz'micheva, G. M.; Rybakov, V. B.

2013-03-01

An X-ray diffraction study of ZnO crystals grown by the hydrothermal method has revealed reflections that give grounds to assign them to the sp. gr. P3 rather than to P63 mc. The distribution of Zn1, Zn2, O1, and O2 over structural positions, along with vacancies and incorporated zinc atoms, explains the dissymmetrization observed in terms of the kinetic (growth) phase transition of the order-disorder type, which is caused by ordering Zn and O atoms over structural positions. The color of crystals of refined compositions (Zn0.975□0.025)Zn i(0.015)(O0.990□0.010) (green) and (Zn0.965□0.035)Zn i(0.035)O (bright green) is related to different oxygen contents, which is confirmed by the results of electron probe X-ray microanalysis and absorption spectroscopy. The degree of the structural quality of crystals, their resistivity, and activation energy are also related to oxygen vacancies.

Synthesis and structure of a rhenium(V) complex containing a ...

African Journals Online (AJOL)

methylphenyl) salicylideneimine) was prepared by the reaction of [NH4][ReO4] with H3mps in the presence of triphenylphosphine and hydrochloric acid in glacial acetic acid. Crystallization from acetonitrile gave the product 1.CH3CN.

Comparative sequence and structural analyses of G-protein-coupled receptor crystal structures and implications for molecular models.

Directory of Open Access Journals (Sweden)

Catherine L Worth

Full Text Available BACKGROUND: Up until recently the only available experimental (high resolution structure of a G-protein-coupled receptor (GPCR was that of bovine rhodopsin. In the past few years the determination of GPCR structures has accelerated with three new receptors, as well as squid rhodopsin, being successfully crystallized. All share a common molecular architecture of seven transmembrane helices and can therefore serve as templates for building molecular models of homologous GPCRs. However, despite the common general architecture of these structures key differences do exist between them. The choice of which experimental GPCR structure(s to use for building a comparative model of a particular GPCR is unclear and without detailed structural and sequence analyses, could be arbitrary. The aim of this study is therefore to perform a systematic and detailed analysis of sequence-structure relationships of known GPCR structures. METHODOLOGY: We analyzed in detail conserved and unique sequence motifs and structural features in experimentally-determined GPCR structures. Deeper insight into specific and important structural features of GPCRs as well as valuable information for template selection has been gained. Using key features a workflow has been formulated for identifying the most appropriate template(s for building homology models of GPCRs of unknown structure. This workflow was applied to a set of 14 human family A GPCRs suggesting for each the most appropriate template(s for building a comparative molecular model. CONCLUSIONS: The available crystal structures represent only a subset of all possible structural variation in family A GPCRs. Some GPCRs have structural features that are distributed over different crystal structures or which are not present in the templates suggesting that homology models should be built using multiple templates. This study provides a systematic analysis of GPCR crystal structures and a consistent method for identifying

Comparative sequence and structural analyses of G-protein-coupled receptor crystal structures and implications for molecular models.

Science.gov (United States)

Worth, Catherine L; Kleinau, Gunnar; Krause, Gerd

2009-09-16

Up until recently the only available experimental (high resolution) structure of a G-protein-coupled receptor (GPCR) was that of bovine rhodopsin. In the past few years the determination of GPCR structures has accelerated with three new receptors, as well as squid rhodopsin, being successfully crystallized. All share a common molecular architecture of seven transmembrane helices and can therefore serve as templates for building molecular models of homologous GPCRs. However, despite the common general architecture of these structures key differences do exist between them. The choice of which experimental GPCR structure(s) to use for building a comparative model of a particular GPCR is unclear and without detailed structural and sequence analyses, could be arbitrary. The aim of this study is therefore to perform a systematic and detailed analysis of sequence-structure relationships of known GPCR structures. We analyzed in detail conserved and unique sequence motifs and structural features in experimentally-determined GPCR structures. Deeper insight into specific and important structural features of GPCRs as well as valuable information for template selection has been gained. Using key features a workflow has been formulated for identifying the most appropriate template(s) for building homology models of GPCRs of unknown structure. This workflow was applied to a set of 14 human family A GPCRs suggesting for each the most appropriate template(s) for building a comparative molecular model. The available crystal structures represent only a subset of all possible structural variation in family A GPCRs. Some GPCRs have structural features that are distributed over different crystal structures or which are not present in the templates suggesting that homology models should be built using multiple templates. This study provides a systematic analysis of GPCR crystal structures and a consistent method for identifying suitable templates for GPCR homology modelling that will

Visualization of Hyperconjugation and Subsequent Structural Distortions through 3D Printing of Crystal Structures.

Science.gov (United States)

Mithila, Farha J; Oyola-Reynoso, Stephanie; Thuo, Martin M; Atkinson, Manza Bj

2016-01-01

Structural distortions due to hyperconjugation in organic molecules, like norbornenes, are well captured through X-ray crystallographic data, but are sometimes difficult to visualize especially for those applying chemical knowledge and are not chemists. Crystal structure from the Cambridge database were downloaded and converted to .stl format. The structures were then printed at the desired scale using a 3D printer. Replicas of the crystal structures were accurately reproduced in scale and any resulting distortions were clearly visible from the macroscale models. Through space interactions or effect of through space hyperconjugation was illustrated through loss of symmetry or distortions thereof. The norbornene structures exhibits distortion that cannot be observed through conventional ball and stick modelling kits. We show that 3D printed models derived from crystallographic data capture even subtle distortions in molecules. We translate such crystallographic data into scaled-up models through 3D printing.

Simulation and design of the photonic crystal microwave accelerating structure

International Nuclear Information System (INIS)

Song Ruiying; Wu Congfeng; He Xiaodong; Dong Sai

2007-01-01

The authors have derived the global band gaps for general two-dimensional (2D) photonic crystal microwave accelerating structures formed by square or triangular arrays of metal posts. A coordinate-space, finite-difference code was used to calculate the complete dispersion curves for the lattices. The fundamental and higher frequency global photonic band gaps were determined numerically. The structure formed by triangular arrays of metal posts with a missing rod at the center has advantages of higher-order-modes (HOM) suppression and main mode restriction under the condition of a/b<0.2. The relationship between the RF properties and the geometrical parameters have been studied for the 9.37 GHz photonic crystal accelerating structure. The Rs, Q, Rs/Q of the new structure may be comparable to the disk-loaded accelerating structure. (authors)

Crystal structure of calcioburbankite and the characteristic features of the burbankite structure type

International Nuclear Information System (INIS)

Belovitskaya, Yu.V.; Pekov, I.V.; Gobechiya, E.R.; Kabalov, Yu.K.; Subbotin, V.V.

2001-01-01

The crystal structure of calcioburbankite (Na,Ca) 3 (Ca,RE,Sr,Ba) 3 (CO 3 ) 5 found in carbonatites from Vuoriyarvi (North Kareliya) was solved by the Rietveld method. The experimental data were collected on an ADP-2 diffractometer (λCuK α radiation; Ni filter; 16.00 deg. 1 + α 2 ) reflections was 455). All the calculations were performed within the sp. gr. P6 3 mc; a = 10.4974(1) A, c = 6.4309(1) A, V = 613.72(1) A 3 ; R wp = 2.49%. The structure was refined with the use of the anisotropic thermal parameters for the (Na,Ca) and (Sr,Ba,Ce) cations. The comparison of the crystal structures of all of the known hexagonal representatives of the burbankite family demonstrates that the burbankite structure type (sp. gr. P6 3 mc) is stable, irrespectively of the occupancy of the ten-vertex polyhedra predominantly with Ca, Sr, or Ba cations and the occupancies of the positions in the eight-vertex polyhedra

Synthesis, crystal structure and Thermogravimetry of ortho-phthalic ...

Indian Academy of Sciences (India)

satisfied by two chelated carboxylates while fifth and sixth co-ordination positions are satisfied by monodentate ... Keywords. o-Phthalic acid; coordination polymer; X-ray crystal structure; Copper(II); EPR; TGA. 1. .... Absorption coefficient.

GPCR crystal structures: Medicinal chemistry in the pocket.

Science.gov (United States)

Shonberg, Jeremy; Kling, Ralf C; Gmeiner, Peter; Löber, Stefan

2015-07-15

Recent breakthroughs in GPCR structural biology have significantly increased our understanding of drug action at these therapeutically relevant receptors, and this will undoubtedly lead to the design of better therapeutics. In recent years, crystal structures of GPCRs from classes A, B, C and F have been solved, unveiling a precise snapshot of ligand-receptor interactions. Furthermore, some receptors have been crystallized in different functional states in complex with antagonists, partial agonists, full agonists, biased agonists and allosteric modulators, providing further insight into the mechanisms of ligand-induced GPCR activation. It is now obvious that there is enormous diversity in the size, shape and position of the ligand binding pockets in GPCRs. In this review, we summarise the current state of solved GPCR structures, with a particular focus on ligand-receptor interactions in the binding pocket, and how this can contribute to the design of GPCR ligands with better affinity, subtype selectivity or efficacy. Copyright © 2015 Elsevier Ltd. All rights reserved.

The use of radionuclides for the study of crystal structure of solids

International Nuclear Information System (INIS)

Jech, C.

1976-01-01

It is well known that by the coordinated action of atoms arranged in rows and planes in the crystal lattice, the motion of charged particles such as protons, alpha particles and heavier ions can be influenced so that their range in the single crystals is considerably enhanced in low-index directions. A technique has been developed based on such enhanced penetration (channeling) of radioactive atoms ( 220 Rn) emitted by recoil with a 100 keV energy from a 224 Ra point source to record channeling patterns which show the crystal structure. The radioactive recoil atoms impinging from this source on the surface of a single crystal penetrate deeper in places where their direction of impact is identical with low index crystal directions and planes. These places can be visualized by autoradiography when having first stripped a thin layer from the surface corresponding to the random range of the atoms. This technique is generally applicable in close packed crystals and gives information about the crystal structure of very thin surface layers. (author)

CCDC 1048727: Experimental Crystal Structure Determination : bis(2-(hydroxyimino)propanoato)-tin(ii)

KAUST Repository

Khanderi, Jayaprakash; Davaasuren, Bambar; Alshankiti, Buthainah; Rothenberger, Alexander

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1515632: Experimental Crystal Structure Determination : hexakis(dimethyl sulfoxide)-manganese(ii) tetraiodide

KAUST Repository

Haque, M.A.

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1429311: Experimental Crystal Structure Determination : N-(5-Bromoquinolin-8-yl)benzamide

KAUST Repository

Xu, Jun; Shen, Chao; Zhu, Xiaolei; Zhang, Pengfei; Ajitha, Manjaly John; Huang, Kuo-Wei; An, Zhongfu; Liu, Xiaogang

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1427126: Experimental Crystal Structure Determination : bis(1,10-Phenanthroline)-copper pentafluoropropanoate

KAUST Repository

Huang, Yangjie

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

Synthesis, crystal structure and biological activity of novel diester cyclophanes

International Nuclear Information System (INIS)

Zhang, Pengfei; Yang, Bingqin; Fang, Xianwen; Cheng, Zhao; Yang, Meipan

2012-01-01

A series of novel diester cyclophanes was synthesized by esterification of 1,2-benzenedicarbonyl chloride with eight different diols under high dilution conditions. The structures of the compounds were verified by elemental analysis, 1 H nuclear magnetic resonance (NMR), IR spectroscopy and high resolution mass spectrometry (HRMS). The crystal structures of two compounds were characterized by single crystal X-ray diffractometry (XRD). All the new cyclophanes were evaluated for biological activities and the results showed that some of these compounds have low antibacterial or antifungal activities (author)

Moessbauer determination of magnetic structure of Fe3BO6 crystal

International Nuclear Information System (INIS)

Kovalenko, P.P.; Labushkin, V.G.; Ovsepyan, A.K.; Sarkisov, Eh.R.; Smirnov, E.V.; Prokopov, A.R.; Seleznev, V.N.

1984-01-01

The magnetic structure of a Fe 3 BO 6 crystal belonging to space group Dsub(2h)sup(16)(Psub(nma)) is determined by the Moessbauer γ-radiation diffraction. The bragg reflection (700) of Moessbauer 14.4 keV γ-quanta from the Fe 3 BO 6 monocrystal has been studied experimentally. A high sensitivity of the interference of γ-quantum diffraction scattering on Fe nuclei being in crystallographically non-equivalent 8d- and 4s-positions to the type of magnetic ordering in the crystal is used for determination of the magnetic structure. Agreement of the experimental results with the theoretical calculations, conducted for types of magnetic ordering resolved by the symmetry of the crystal, permitted to reliably determine the magnetic structure of this compound. The results obtained confirm the data of neutrondiffraction studies on magnetic ordering in Fe 3 BO 6 . Advantages of the Moessbauer-diffraction study, as compared to the magnetic neutrondiffraction method, in particular, for investigation of crystals, in which the hyperfine magnetic fields on Fe nuclei have different values, are revealed and discussed in detail

Rapid X-ray crystal structure analysis in few second measurements using microstrip gas chamber

CERN Document Server

Ochi, A; Tanimori, T; Ohashi, Y; Toyokawa, H; Nishi, Y; Nishi, Y; Nagayoshi, T; Koishi, S

2001-01-01

X-ray crystal structure analysis using microstrip gas chamber was successfully carried out in a measurement time within a few seconds. The continuous rotation photograph method, in which most of the diffraction peaks can be obtained within one continuous rotation of the sample crystal (without stopping or oscillation), was applied for this measurement. As an example, the structure of a single crystal of ammonium bitartrate (r=1 mm, spherical) was measured. Diffraction spots from the sample, which were sufficient to obtain crystal structure, were successfully obtained by taking only 2 s measurements with a commercially available laboratory X-ray source.

Welcome to Crystals: A New Open-Access, Multidisciplinary Forum for Growth, Structures and Properties of Crystals

Directory of Open Access Journals (Sweden)

Gerd Meyer

2010-12-01

Full Text Available The majority of the earth’s crust is made up of crystalline material. The research areas of mineralogy, petrology, chimie minerále (inorganic chemistry and, of course, crystallography outgrew from the fascination of mankind with the color and symmetry of crystals. Crystals have translational symmetry in two or three dimensions, quasicrystals have translational symmetry in higher spaces. Further symmetries may be observed by the eye, by microscopic techniques or by the diffraction of X-ray, electron, or neutron beams. Diffraction techniques are also used, due to Max von Laue’s eminent discovery a century ago, to determine crystal structures. [...

Use of new tandem cation/anion exchange system with clinical-scale generators provides high specific volume solutions of technetium-99m and rhenium-188

International Nuclear Information System (INIS)

Knapp, F.F. Jr.; Beets, A.L.; Mirzadeh, S.; Guhlke, S.

1998-01-01

In this paper we describe the first application of our simple and inexpensive post-elution tandem cation/anion exchange column system which is based on generator elution with salts of weak acids such as ammonium acetate instead of saline solution to provide very high specific volume solutions of technetium-99m and rhenium-188 from clinical-scale molybdenum-99/technetium-99m generator prepared from low specific activity (n,y) molybdenum-99, and tungsten-188/rhenium-188 generators, respectively. Initial passage of the bolus through a strong cation exchange cartridge converts the ammonium acetate to acetic acid which is essentially not ionized at the acidic pH, allowing specific subsequent amine-type (QMA SepPak TM ) anion exchange cartridge column trapping of the microscopic levels of the pertechnetate or perrhenate. Subsequent elution of the anion cartridge with a small volume ( 500 mCi/mL) from the alumina-based tungsten-188/rhenium-188 generator. (author)

Crystal structure of bile salt hydrolase from Lactobacillus salivarius.

Science.gov (United States)

Xu, Fuzhou; Guo, Fangfang; Hu, Xiao Jian; Lin, Jun

2016-05-01

Bile salt hydrolase (BSH) is a gut-bacterial enzyme that negatively influences host fat digestion and energy harvesting. The BSH enzyme activity functions as a gateway reaction in the small intestine by the deconjugation of glycine-conjugated or taurine-conjugated bile acids. Extensive gut-microbiota studies have suggested that BSH is a key mechanistic microbiome target for the development of novel non-antibiotic food additives to improve animal feed production and for the design of new measures to control obesity in humans. However, research on BSH is still in its infancy, particularly in terms of the structural basis of BSH function, which has hampered the development of BSH-based strategies for improving human and animal health. As an initial step towards the structure-function analysis of BSH, C-terminally His-tagged BSH from Lactobacillus salivarius NRRL B-30514 was crystallized in this study. The 1.90 Å resolution crystal structure of L. salivarius BSH was determined by molecular replacement using the structure of Clostridium perfringens BSH as a starting model. It revealed this BSH to be a member of the N-terminal nucleophile hydrolase superfamily. Crystals of apo BSH belonged to space group P21212, with unit-cell parameters a = 90.79, b = 87.35, c = 86.76 Å (PDB entry 5hke). Two BSH molecules packed perfectly as a dimer in one asymmetric unit. Comparative structural analysis of L. salivarius BSH also identified potential residues that contribute to catalysis and substrate specificity.

Hierarchically structured photonic crystals for integrated chemical separation and colorimetric detection.

Science.gov (United States)

Fu, Qianqian; Zhu, Biting; Ge, Jianping

2017-02-16

A SiO 2 colloidal photonic crystal film with a hierarchical porous structure is fabricated to demonstrate an integrated separation and colorimetric detection of chemical species for the first time. This new photonic crystal based thin layer chromatography process requires no dyeing, developing and UV irradiation compared to the traditional TLC. The assembling of mesoporous SiO 2 particles via a supersaturation-induced-precipitation process forms uniform and hierarchical photonic crystals with micron-scale cracks and mesopores, which accelerate the diffusion of developers and intensify the adsorption/desorption between the analytes and silica for efficient separation. Meanwhile, the chemical substances infiltrated to the voids of photonic crystals cause an increase of the refractive index and a large contrast of structural colors towards the unloaded part, so that the sample spots can be directly recognized with the naked eye before and after separation.

Crystallization and structure of chromium cast iron with addition of Mo and Ni

International Nuclear Information System (INIS)

Pietrowski, S.

1998-01-01

The aim of the presented paper is to show the results of examination of the crystallization process using the method of thermal-derivative analysis (ATD) and the structure examination of chromium cast iron, chromium molybdenum c. i. and chromium molybdenum nickel c.i. It was found that molybdenum in amount over 2 wt % causes the crystallization of eutectic carbides M 23 C 6 and M 6 C. The M 23 C 6 carbide crystallizes upon the crystallization of eutectic carbides M 3 C and M 7 C 3 . It is shown that ATD method facilitates both interpretation and control of the crystallization as well as formation of the cast iron structure at the solid state. (author)

Crystal structure, growth and nonlinear optical studies of isonicotinamide p-nitrophenol: A new organic crystal for optical limiting applications

Science.gov (United States)

Vijayalakshmi, A.; Vidyavathy, B.; Vinitha, G.

2016-08-01

Isonicotinamide p-nitrophenol (ICPNP), a new organic material, was synthesized using methanol solvent. Single crystals of ICPNP were grown using a slow evaporation solution growth technique. Crystal structure of ICPNP is elucidated by single crystal X-ray diffraction analysis. It belongs to monoclinic crystal system with space group of P21/c. It forms two dimensional networks by O-H…O, N-H…O and C-H…O hydrogen bonds. The molecular structure of ICPNP was further confirmed by Fourier transform infrared (FTIR) spectral analysis. The optical transmittance range and the lower cut-off wavelength (421 nm) with the optical band gap (2.90 eV) of the ICPNP crystal were determined by UV-vis-NIR spectral study. Thermal behavior of ICPNP was studied by thermo gravimetric and differential thermal analyses (TG/DTA). The relative dielectric permittivity was calculated for various temperature ranges. Laser damage threshold of ICPNP crystal was found to be 1.9 GW/cm2 using an Nd:YAG laser. A Z-scan technique was employed to measure the nonlinear absorption coefficient, nonlinear refractive index and nonlinear optical susceptibility. Optical limiting behavior of ICPNP was observed at 35 mW input power.

Crystal structure of Cryptosporidium parvum pyruvate kinase.

Directory of Open Access Journals (Sweden)

William J Cook

Full Text Available Pyruvate kinase plays a critical role in cellular metabolism of glucose by serving as a major regulator of glycolysis. This tetrameric enzyme is allosterically regulated by different effector molecules, mainly phosphosugars. In response to binding of effector molecules and substrates, significant structural changes have been identified in various pyruvate kinase structures. Pyruvate kinase of Cryptosporidium parvum is exceptional among known enzymes of protozoan origin in that it exhibits no allosteric property in the presence of commonly known effector molecules. The crystal structure of pyruvate kinase from C. parvum has been solved by molecular replacement techniques and refined to 2.5 Å resolution. In the active site a glycerol molecule is located near the γ-phosphate site of ATP, and the protein structure displays a partially closed active site. However, unlike other structures where the active site is closed, the α6' helix in C. parvum pyruvate kinase unwinds and assumes an extended conformation. In the crystal structure a sulfate ion is found at a site that is occupied by a phosphate of the effector molecule in many pyruvate kinase structures. A new feature of the C. parvum pyruvate kinase structure is the presence of a disulfide bond cross-linking the two monomers in the asymmetric unit. The disulfide bond is formed between cysteine residue 26 in the short N-helix of one monomer with cysteine residue 312 in a long helix (residues 303-320 of the second monomer at the interface of these monomers. Both cysteine residues are unique to C. parvum, and the disulfide bond remained intact in a reduced environment. However, the significance of this bond, if any, remains unknown at this time.

Crystal Structure of a Eukaryotic GEN1 Resolving Enzyme Bound to DNA

Directory of Open Access Journals (Sweden)

Yijin Liu

2015-12-01

Full Text Available We present the crystal structure of the junction-resolving enzyme GEN1 bound to DNA at 2.5 Å resolution. The structure of the GEN1 protein reveals it to have an elaborated FEN-XPG family fold that is modified for its role in four-way junction resolution. The functional unit in the crystal is a monomer of active GEN1 bound to the product of resolution cleavage, with an extensive DNA binding interface for both helical arms. Within the crystal lattice, a GEN1 dimer interface juxtaposes two products, whereby they can be reconnected into a four-way junction, the structure of which agrees with that determined in solution. The reconnection requires some opening of the DNA structure at the center, in agreement with permanganate probing and 2-aminopurine fluorescence. The structure shows that a relaxation of the DNA structure accompanies cleavage, suggesting how second-strand cleavage is accelerated to ensure productive resolution of the junction.

The crystal structure of the phosphatidylinositol 4-kinase IIalpha

Czech Academy of Sciences Publication Activity Database

Bäumlová, Adriana; Chalupská, Dominika; Rozycki, B.; Jovic, M.; Wisniewski, E.; Klíma, Martin; Dubánková, Anna; Kloer, D. P.; Nencka, Radim; Balla, T.; Bouřa, Evžen

2015-01-01

Roč. 22, č. 1 (2015), s. 5 ISSN 1211-5894. [Discussions in Structural Molecular Biology. Annual Meeting of the Czech Society for Structural Biology /13./. 19.03.2015-21.03.2015, Nové Hrady] EU Projects: European Commission(XE) 333916 - STARPI4K Institutional support: RVO:61388963 Keywords : PI4K IIalpha * crystal structure Subject RIV: CE - Biochemistry

Synthesis, crystal structure and biological activity of novel diester cyclophanes

Energy Technology Data Exchange (ETDEWEB)

Zhang, Pengfei; Yang, Bingqin; Fang, Xianwen; Cheng, Zhao; Yang, Meipan, E-mail: yangbq@nwu.edu.cn [Department of Chemistry, Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Northwest University, Shaanxi (China)

2012-10-15

A series of novel diester cyclophanes was synthesized by esterification of 1,2-benzenedicarbonyl chloride with eight different diols under high dilution conditions. The structures of the compounds were verified by elemental analysis, {sup 1}H nuclear magnetic resonance (NMR), IR spectroscopy and high resolution mass spectrometry (HRMS). The crystal structures of two compounds were characterized by single crystal X-ray diffractometry (XRD). All the new cyclophanes were evaluated for biological activities and the results showed that some of these compounds have low antibacterial or antifungal activities (author)

Bismuth zinc vanadate, BiZn2VO6: New crystal structure type and electronic structure

International Nuclear Information System (INIS)

Eliziario Nunes, Sayonara; Wang, Chun-Hai; So, Karwei; Evans, John S.O.; Evans, Ivana Radosavljević

2015-01-01

We report a combined experimental and computational study of the crystal structure and electronic properties of bismuth zinc vanadate, BiZn 2 VO 6 , known for its visible light photocatalytic activity. The crystal structure has been solved from laboratory powder X-ray diffraction data using the repeated minimisations from random starting values method. BiZn 2 VO 6 adopts a new structure type, based on the following building blocks: corner- and edge-sharing ZnO 4 tetrahedra, ZnO 6 octahedra and VO 4 tetrahedra, and Bi 2 O 12 dimers. It is the only known member of the BiM 2 AO 6 (M=Pb, Ca, Cd, Mn, Zn, Mg, Cu; A=V, P, As) family which does not appear to be structurally closely related to others. The electronic structure of BiZn 2 VO 6 , calculated by DFT methods, shows that it is an indirect gap semiconductor with a calculated band gap of 1.6 eV, which compares favourably to the experimentally measured value of 2.4 eV. - Graphical abstract: The crystal structure of BiZn 2 VO 6 , a new structure type in the BiM 2 AO 6 (M=Mg, Ca, Cd, Cu, Pb, Mn, Zn; A=V, P, As) family. - Highlights: • Structure solution from PXRD data by repeated minimisations from random starting values. • New structure type in the BiM 2 AO 6 (M=Pb, Ca, Cd, Mn, Zn, Mg, Cu; A=V, P, As) family. • Electronic structure calculation

Free-standing nanomechanical and nanophotonic structures in single-crystal diamond

Science.gov (United States)

Burek, Michael John

Realizing complex three-dimensional structures in a range of material systems is critical to a variety of emerging nanotechnologies. This is particularly true of nanomechanical and nanophotonic systems, both relying on free-standing small-scale components. In the case of nanomechanics, necessary mechanical degrees of freedom require physically isolated structures, such as suspended beams, cantilevers, and membranes. For nanophotonics, elements like waveguides and photonic crystal cavities rely on light confinement provided by total internal reflection or distributed Bragg reflection, both of which require refractive index contrast between the device and surrounding medium (often air). Such suspended nanostructures are typically fabricated in a heterolayer structure, comprising of device (top) and sacrificial (middle) layers supported by a substrate (bottom), using standard surface nanomachining techniques. A selective, isotropic etch is then used to remove the sacrificial layer, resulting in free-standing devices. While high-quality, crystalline, thin film heterolayer structures are readily available for silicon (as silicon-on-insulator (SOI)) or III-V semiconductors (i.e. GaAs/AlGaAs), there remains an extensive list of materials with attractive electro-optic, piezoelectric, quantum optical, and other properties for which high quality single-crystal thin film heterolayer structures are not available. These include complex metal oxides like lithium niobate (LiNbO3), silicon-based compounds such as silicon carbide (SiC), III-V nitrides including gallium nitride (GaN), and inert single-crystals such as diamond. Diamond is especially attractive for a variety of nanoscale technologies due to its exceptional physical and chemical properties, including high mechanical hardness, stiffness, and thermal conductivity. Optically, it is transparent over a wide wavelength range (from 220 nm to the far infrared), has a high refractive index (n ~ 2.4), and is host to a vast

Synthesis, growth, crystal structure, optical and third order nonlinear optical properties of quinolinium derivative single crystal: PNQI

Science.gov (United States)

Karthigha, S.; Krishnamoorthi, C.

2018-03-01

An organic quinolinium derivative nonlinear optical (NLO) crystal, 1-ethyl-2-[2-(4-nitro-phenyl)-vinyl]-quinolinium iodide (PNQI) was synthesized and successfully grown by slow evaporation solution growth technique. Formation of a crystalline compound was confirmed by single crystal X-ray diffraction. The quinolinium compound PNQI crystallizes in the triclinic crystal system with a centrosymmetric space group of P-1 symmetry. The molecular structure of PNQI was confirmed by 1H NMR and 13C NMR spectral studies. The thermal properties of the crystal have been investigated by thermogravimetric (TG) and differential scanning calorimetry (DSC) studies. The optical characteristics obtained from UV-Vis-NIR spectral data were described and the cut-off wavelength observed at 506 nm. The etching study was performed to analyse the growth features of PNQI single crystal. The third order NLO properties such as nonlinear refractive index (n2), nonlinear absorption coefficient (β) and nonlinear susceptibility (χ (3)) of the crystal were investigated using Z-scan technique at 632.8 nm of Hesbnd Ne laser.

Effect of crystal structure on optical properties of sol–gel derived zirconia thin films

Energy Technology Data Exchange (ETDEWEB)

Wang, Xiaodong, E-mail: xiaodong_wang@tongji.edu.cn [Pohl Institute of Solid State Physics, Shanghai Key Laboratory of Special Artificial Microstructure Materials and Technology, Tongji University, Shanghai 200092 (China); Wu, Guangming; Zhou, Bin [Pohl Institute of Solid State Physics, Shanghai Key Laboratory of Special Artificial Microstructure Materials and Technology, Tongji University, Shanghai 200092 (China); Shen, Jun, E-mail: shenjun67@tongji.edu.cn [Pohl Institute of Solid State Physics, Shanghai Key Laboratory of Special Artificial Microstructure Materials and Technology, Tongji University, Shanghai 200092 (China)

2013-04-15

Highlights: ► ZrO{sub 2} films were deposited by sol–gel method. ► Crystal structures of the films were tuned by different thermal annealing methods. ► The refractive indices vary with the crystal structures of the films. ► Lattice-mismatch was found to reduce the refractive index of ZrO{sub 2} films. -- Abstract: The optical properties of sol–gel derived zirconia thin films and their relation to the crystal structure are studied in this paper. ZrO{sub 2} films were deposited on quartz glass and silicon wafer substrates by sol–gel method with conventional furnace annealing (CFA) and rapid thermal annealing (RTA). Crystal structures of the films were analyzed by X-ray diffraction (XRD) and Raman spectroscopy, while refractive indices of the films were determined from the reflectance and transmittance spectra. The refractive indices vary with the function of crystal structure and density of the films, which depends on annealing temperature and annealing technique. Lattice-mismatch between monoclinic phase and tetragonal phase was found to reduce the refractive index of ZrO{sub 2} films.

Elastic properties of Ti-24Nb-4Zr-8Sn single crystals with bcc crystal structure

International Nuclear Information System (INIS)

Zhang, Y.W.; Li, S.J.; Obbard, E.G.; Wang, H.; Wang, S.C.; Hao, Y.L.; Yang, R.

2011-01-01

Research highlights: → The single crystals of Ti2448 alloy with the bcc crystal structure were prepared. → The elastic moduli and constants were measured by several resonant methods. → The crystal shows significant elastic asymmetry in tension and compression. → The crystal exhibits weak nonlinear elasticity with large elastic strain ∼2.5%. → The crystal has weak atomic interactions against crystal distortion to low symmetry. - Abstract: Single crystals of Ti2448 alloy (Ti-24Nb-4Zr-8Sn in wt.%) were grown successfully using an optical floating-zone furnace. Several kinds of resonant methods gave consistent Young's moduli of 27.1, 56.3 and 88.1 GPa and shear moduli of 34.8, 11.0 and 14.6 GPa for the , and oriented single crystals, and C 11 , C 12 and C 44 of 57.2, 36.1 and 35.9 GPa respectively. Uniaxial testing revealed asymmetrical elastic behaviors of the crystals: tension caused elastic softening with a large reversible strain of ∼4% and a stress plateau of ∼250 MPa, whereas compression resulted in gradual elastic stiffening with much smaller reversible strain. The crystals exhibited weak nonlinear elasticity with a large elastic strain of ∼2.5% and a high strength, approaching ∼20% and ∼30% of its ideal shear and ideal tensile strength respectively. The crystals showed linear elasticity with a small elastic strain of ∼1%. These elastic deformation characteristics have been interpreted in terms of weakened atomic interactions against crystal distortion to low crystal symmetry under external applied stresses. These results are consistent with the properties of polycrystalline Ti2448, including high strength, low elastic modulus, large recoverable strain and weak strengthening effect due to grain refinement.

Band structures in Sierpinski triangle fractal porous phononic crystals

International Nuclear Information System (INIS)

Wang, Kai; Liu, Ying; Liang, Tianshu

2016-01-01

In this paper, the band structures in Sierpinski triangle fractal porous phononic crystals (FPPCs) are studied with the aim to clarify the effect of fractal hierarchy on the band structures. Firstly, one kind of FPPCs based on Sierpinski triangle routine is proposed. Then the influence of the porosity on the elastic wave dispersion in Sierpinski triangle FPPCs is investigated. The sensitivity of the band structures to the fractal hierarchy is discussed in detail. The results show that the increase of the hierarchy increases the sensitivity of ABG (Absolute band gap) central frequency to the porosity. But further increase of the fractal hierarchy weakens this sensitivity. On the same hierarchy, wider ABGs could be opened in Sierpinski equilateral triangle FPPC; whilst, a lower ABG could be opened at lower porosity in Sierpinski right-angled isosceles FPPCs. These results will provide a meaningful guidance in tuning band structures in porous phononic crystals by fractal design.

Band structures in Sierpinski triangle fractal porous phononic crystals

Energy Technology Data Exchange (ETDEWEB)

Wang, Kai; Liu, Ying, E-mail: yliu5@bjtu.edu.cn; Liang, Tianshu

2016-10-01

In this paper, the band structures in Sierpinski triangle fractal porous phononic crystals (FPPCs) are studied with the aim to clarify the effect of fractal hierarchy on the band structures. Firstly, one kind of FPPCs based on Sierpinski triangle routine is proposed. Then the influence of the porosity on the elastic wave dispersion in Sierpinski triangle FPPCs is investigated. The sensitivity of the band structures to the fractal hierarchy is discussed in detail. The results show that the increase of the hierarchy increases the sensitivity of ABG (Absolute band gap) central frequency to the porosity. But further increase of the fractal hierarchy weakens this sensitivity. On the same hierarchy, wider ABGs could be opened in Sierpinski equilateral triangle FPPC; whilst, a lower ABG could be opened at lower porosity in Sierpinski right-angled isosceles FPPCs. These results will provide a meaningful guidance in tuning band structures in porous phononic crystals by fractal design.

Synthesis and Crystal Structure of 1-Chloro-2-methyl-4-nitrobenzene

Directory of Open Access Journals (Sweden)

Jim Simpson

2012-03-01

Full Text Available The title compound (3 was prepared from 4-chloroaniline in good yield on successive oxidation and methylation and its crystal and molecular structure is reported. The compound crystallizes in the monoclinic space group P 21/n with unit cell dimensions a = 13.5698(8, b = 3.7195 (3, c = 13.5967 (8 Å, ß = 91.703(3 °, V = 685.96 (10 Å3. The molecule is essentially planar with a dihedral angle of 6.2(3 ° between the nitro group and the phenyl ring. The crystal structure is stabilised by π...π contacts between adjacent benzene rings together with C–H...O hydrogen bonds and close Cl...O contacts.

Structure of single-chain single crystals of isotactic polystyrene and their radiation resistance

International Nuclear Information System (INIS)

Bu Haishan; Cao Jie; Xu Shengyong; Zhang Ze

1997-01-01

The structure of the single-chain single crystals of isotactic polystyrene (i-PS) was investigated by electron diffraction (ED) and high resolution electron microscopy (HREM). The nano-scale single-chain single crystals were found to be very stable to electron irradiation. According to the unit cell of i-PS crystals, the reflection rings in ED pattern and the lattice fringes in HREM images could be indexed, but the lower-index diffractions were not found. It is proposed that the single-chain single crystals are very small, thus secondary electrons may be allowed to escape and radiation damage is highly reduced, and that there are less lower-index lattice planes in the single-chain single crystals to provide sufficient diffraction intensity for recording. HREM images can be achieved at room temperature in the case of single-chain single crystals because of its stability to electron irradiation, therefore, this might be a novel experimental approach to the study of crystal structure of macromolecules

Crystal Structure of Tetragonal Form of La2NiO4+x

Science.gov (United States)

Kajitani, Tsuyoshi; Hosoya, Syoichi; Hirabayashi, Makoto; Fukuda, Tsuguo; Onozuka, Takashi

1989-10-01

The crystal structure of the title oxide was studied by means of the X-ray and neutron single crystal diffraction measurements. At room temperature, the tetragonal crystal structure is P42/ncm-type (No. 138), which is one of the subgroup of the space group I4/mmm. The lattice parameters of a sample annealed and slowly cooled in oxygen atmosphere from 673 K are a{=}b{=}5.4640(1) Å and c{=}12.6719(2) Å, while the oxygen content, x{=}0.10(4), was determined from obtained neutron data. The title oxide undergoes a tetragonal (P42/ncm)/tetragonal (I4/mmm) phase transition at about 560 K. The transition temperature is almost identical both in the annealed and as-grown crystals.

Thermal decomposition of rhenium (5) complexes with 1,2,4-triazole

International Nuclear Information System (INIS)

Amindzhanov, A.A.; Gagieva, S.Ch.; Kotegov, K.V.

1991-01-01

Processes of thermal decomposition of rhenium (5) complexes with 1,2,4-triazole were studied. Thermolysis products were identified on the basis of data of the element analysis, IR spectra, conductometry and other methods. It is ascertained that at the first stage of thermolysis of hydroxyl-containing monomer complexes removal of water molecules occurs, and at the second one - dimerization process with formation of Re-O-Re group. It is shown that the nature of halide ion practically does not affect the temperature of the start of intensive thermal decomposition of the complexes

The analysis of mechanism of rhenium-coated tools' wear-resistance rising

Directory of Open Access Journals (Sweden)

Daniel Petrosyan

2017-06-01

Full Text Available It is proposed to obtain wear-resistant layers on the hard-alloy materials by thermochemical treatment. In the different field of production – mechanical engineering, metallurgy and military technologies, with machine parts demanding high wearproof and corrosion-proof machinery parts on the surfaces of syntheses of diamonds, with metal surface thermal-diffusion with rhenium, to receive diffusion wearing layers for the first time. A method for thermochemical treatment of hard alloy plates has been investigated, allowing to raise the wear-resistance of cutting and mining tools.

Machine learning for the structure-energy-property landscapes of molecular crystals.

Science.gov (United States)

Musil, Félix; De, Sandip; Yang, Jack; Campbell, Joshua E; Day, Graeme M; Ceriotti, Michele

2018-02-07

Molecular crystals play an important role in several fields of science and technology. They frequently crystallize in different polymorphs with substantially different physical properties. To help guide the synthesis of candidate materials, atomic-scale modelling can be used to enumerate the stable polymorphs and to predict their properties, as well as to propose heuristic rules to rationalize the correlations between crystal structure and materials properties. Here we show how a recently-developed machine-learning (ML) framework can be used to achieve inexpensive and accurate predictions of the stability and properties of polymorphs, and a data-driven classification that is less biased and more flexible than typical heuristic rules. We discuss, as examples, the lattice energy and property landscapes of pentacene and two azapentacene isomers that are of interest as organic semiconductor materials. We show that we can estimate force field or DFT lattice energies with sub-kJ mol -1 accuracy, using only a few hundred reference configurations, and reduce by a factor of ten the computational effort needed to predict charge mobility in the crystal structures. The automatic structural classification of the polymorphs reveals a more detailed picture of molecular packing than that provided by conventional heuristics, and helps disentangle the role of hydrogen bonded and π-stacking interactions in determining molecular self-assembly. This observation demonstrates that ML is not just a black-box scheme to interpolate between reference calculations, but can also be used as a tool to gain intuitive insights into structure-property relations in molecular crystal engineering.

High-brightness tapered laser diodes with photonic crystal structures

Science.gov (United States)

Li, Yi; Du, Weichuan; Kun, Zhou; Gao, Songxin; Ma, Yi; Tang, Chun

2018-02-01

Beam quality of tapered laser diodes is limited by higher order lateral mode. On purpose of optimizing the brightness of tapered laser diodes, we developed a novel design of tapered diodes. This devices based on InGaAs/AlGaAs asymmetry epitaxial structure, containing higher order lateral mode filtering schemes especially photonic crystal structures, which fabricated cost effectively by using standard photolithography and dry etch processes. Meanwhile, the effects of photonic crystal structures on mode control are also investigated theoretically by FDBPM (Finite-Difference Beam Propagation Method) calculation. We achieved a CW optical output power of 6.9W at 940nm for a single emitter with 4 mm cavity length. A nearly diffraction limited beam of M2 ≍1.9 @ 0.5W has been demonstrated, and a highest brightness of β =75MW/(cm2 ·sr) was reached.

Solving crystal structures from neutron diffraction data

International Nuclear Information System (INIS)

Wilson, C.C.

1987-07-01

In order to pursue crystal structure determination using neutron diffraction data, and given the wide experience available of solving structures using X-ray data, the codes used in X-ray structural analysis should be adapted to the different requirements of a neutron experiment. Modifications have been made to a direct methods program MITHRIL and to a Patterson methods program PATMET to incorporate into these the features of neutron rather than X-ray diffraction. While to date these modifications have been fairly straightforward and many sophistications remain to be exploited, results obtained from the neutron versions of both programs are promising. (author)

CRYSTAL AND MOLECULAR STRUCTURE OF 5-NITROPIRIDINE PIPERIDINE-SULFENAMIDE

OpenAIRE

Brito, Iván; León, Yasna; Arias, Mauricio; Vargas, Danitza; Carmona, Francisco; Ramírez, Eduardo; Restovic, Ambrosio; Cárdenas, Alejandro; Wittke, Oscar; López-Rodríguez, Matías

2002-01-01

The crystal and molecular structure of 5-nitropiridine piperidine-sulfenamide, C10H13N3O2 S is described and compared with other sulfenamides and with other similar compounds. This structure belongs to a type of divalent sulphur compound and crystallizes in the orthorhombic space group Pnma with a= 27.810(4), b=6.797(1), c=6.110(1)Å, and Dx =1.376 g cm-3 with Z=4. The S-N bond distance of 1.699(4) Å is shorter than a single S-N bond [1.74 Å]. The NO2-(C6H3N)-S-N(C 5H10) molecule lies on a cry...

Protein crystal growth on board Shenzhou 3: a concerted effort improves crystal diffraction quality and facilitates structure determination

International Nuclear Information System (INIS)

Han, Y.; Cang, H.-X.; Zhou, J.-X.; Wang, Y.-P.; Bi, R.-C.; Colelesage, J.; Delbaere, L.T.J.; Nahoum, V.; Shi, R.; Zhou, M.; Zhu, D.-W.; Lin, S.-X.

2004-01-01

The crystallization of 16 proteins was carried out using 60 wells on board Shenzhou 3 in 2002. Although the mission was only 7 days, careful and concerted planning at all stages made it possible to obtain crystals of improved quality compared to their ground controls for some of the proteins. Significantly improved resolutions were obtained from diffracted crystals of 4 proteins. A complete data set from a space crystal of the PEP carboxykinase yielded significantly higher resolution (1.46 A vs. 1.87 A), I/sigma (22.4 vs. 15.5), and a lower average temperature factor (29.2 A 2 vs. 42.9 A 2 ) than the best ground-based control crystal. The 3-D structure of the enzyme is well improved with significant ligand density. It has been postulated that the reduced convection and absence of macromolecule sedimentation under microgravity have advantages/benefits for protein crystal growth. Improvements in experimental design for protein crystal growth in microgravity are ongoing

Oxidation of iridium coating on rhenium coated graphite at elevated temperature in stagnated air

International Nuclear Information System (INIS)

Huang, Yongle; Bai, Shuxin; Zhang, Hong; Ye, Yicong

2015-01-01

Highlights: • Continuous and dense Ir coatings were prepared on graphite by electrodepostion. • The purification of the as-prepared Ir coating was higher than about 99.98%. • The Ir/Re/C specimen kept integrity without significant failures after oxidation. • The average oxidation rate of the Ir coating was about 0.219 mg/(cm 2 min). • Penetrating holes at gains boundaries resulted in the failure of the Ir coating. - Abstract: Continuous and dense iridium coatings were prepared on the rhenium coated graphite specimens by electrodeposition. The iridium/rhenium coated graphite (Ir/Re/C) specimens were oxidized at elevated temperatures in stagnated air for 3600 s. The purification of the as-prepared Ir coating was higher than about 99.98% with the main impurity elements Si, Al, Fe and Ru. After oxidation, the Ir/Re/C specimens kept integrity without significant failures and the average oxidation rate was about 0.219 mg/(cm 2 min). Pores were found at the grain boundaries and concentrated to penetrating holes with the growth of Ir grains, which resulted in disastrous failures of the Ir coating

Oxidation of iridium coating on rhenium coated graphite at elevated temperature in stagnated air

Energy Technology Data Exchange (ETDEWEB)

Huang, Yongle; Bai, Shuxin, E-mail: NUDT_MSE_501@163.com; Zhang, Hong; Ye, Yicong

2015-02-15

Highlights: • Continuous and dense Ir coatings were prepared on graphite by electrodepostion. • The purification of the as-prepared Ir coating was higher than about 99.98%. • The Ir/Re/C specimen kept integrity without significant failures after oxidation. • The average oxidation rate of the Ir coating was about 0.219 mg/(cm{sup 2} min). • Penetrating holes at gains boundaries resulted in the failure of the Ir coating. - Abstract: Continuous and dense iridium coatings were prepared on the rhenium coated graphite specimens by electrodeposition. The iridium/rhenium coated graphite (Ir/Re/C) specimens were oxidized at elevated temperatures in stagnated air for 3600 s. The purification of the as-prepared Ir coating was higher than about 99.98% with the main impurity elements Si, Al, Fe and Ru. After oxidation, the Ir/Re/C specimens kept integrity without significant failures and the average oxidation rate was about 0.219 mg/(cm{sup 2} min). Pores were found at the grain boundaries and concentrated to penetrating holes with the growth of Ir grains, which resulted in disastrous failures of the Ir coating.

High-resolution metallic magnetic calorimeters for β-spectroscopy on 187rhenium and position resolved X-ray spectroscopy

International Nuclear Information System (INIS)

Porst, Jan-Patrick

2011-01-01

This thesis describes the development of metallic magnetic calorimeters (MMCs) for high resolution spectroscopy. MMCs are energy dispersive particle detectors based on the calorimetric principle which are typically operated at temperatures below 100 mK. The detectors make use of a paramagnetic temperature sensor to transform the temperature rise upon the absorption of a particle in the detector into a measurable magnetic flux change in a dc-SQUID. The application of MMCs for neutrino mass measurements and their advantages with respect to other approaches are discussed. In view of this application the development of an MMC optimized for β-endpoint spectroscopy on 187 rhenium is presented. A fully micro-fabricated X-ray detector is characterized and performs close to design values. Furthermore, a new technique to more efficiently couple rhenium absorbers mechanically and thermally to the sensor was developed and successfully tested. By employing a metallic contact, signal rise times faster than 5 μs could be observed with superconducting rhenium absorbers. In addition to the single pixel detectors, an alternative approach of reading out multiple pixels was developed in this work, too. Here, the individual absorbers have a different thermal coupling to only one temperature sensor resulting in a distribution of different pulse shapes. Straightforward position discrimination by means of rise time analysis is demonstrated for a four pixel MMC and a thermal model of the detector is provided. Unprecedented so far, an energy resolution of less than ΔE FWHM <5 eV for 5.9 keV X-rays was achieved across all absorbers. (orig.)

Parallelization for X-ray crystal structural analysis program

Energy Technology Data Exchange (ETDEWEB)

Watanabe, Hiroshi [Japan Atomic Energy Research Inst., Tokyo (Japan); Minami, Masayuki; Yamamoto, Akiji

1997-10-01

In this report we study vectorization and parallelization for X-ray crystal structural analysis program. The target machine is NEC SX-4 which is a distributed/shared memory type vector parallel supercomputer. X-ray crystal structural analysis is surveyed, and a new multi-dimensional discrete Fourier transform method is proposed. The new method is designed to have a very long vector length, so that it enables to obtain the 12.0 times higher performance result that the original code. Besides the above-mentioned vectorization, the parallelization by micro-task functions on SX-4 reaches 13.7 times acceleration in the part of multi-dimensional discrete Fourier transform with 14 CPUs, and 3.0 times acceleration in the whole program. Totally 35.9 times acceleration to the original 1CPU scalar version is achieved with vectorization and parallelization on SX-4. (author)

Re-investigation of the crystal structure of enstatite under high-pressure conditions

DEFF Research Database (Denmark)

Periotto, Benedetta; Balic Zunic, Tonci; Nestola, Fabrizio

2012-01-01

A synthetic single crystal of pure orthoenstatite (MgSiO3, space group Pbca) has been investigated at high pressure for structural determinations by in situ single-crystal X‑ray diffraction using a diamond-anvil cell. Ten complete intensity data collections were performed up to 9.36 GPa. This study...... with different compositions. The structural evolution determined in this work confirms the high-pressure evolution found previously for other orthopyroxenes and removes some ambiguities originating from the less accurate published data on the MgSiO3 structure at high pressure. The structural compression...

Magnetic structure of URhSi single crystal

Czech Academy of Sciences Publication Activity Database

Prokeš, K.; Andreev, Alexander V.; Honda, F.; Sechovský, V.

2003-01-01

Roč. 261, - (2003), s. 131-138 ISSN 0304-8853 R&D Projects: GA ČR GA202/02/0739 Institutional research plan: CEZ:AV0Z1010914 Keywords : URhSi single crystal * magnetization * neutron diffraction * magnetic structure determination Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.910, year: 2003

Rhenium (5) and molybdenum (5) complexes with 4',4''(5'')-ditretbutyldibenzo-24-crown-8. Kompleksnye soedineniya reniya (5) i molibdena (5) s 4',4''(5'')-ditretbutildibenzo-24-kraun-8

Energy Technology Data Exchange (ETDEWEB)

Ashurova, N Kh; Yakubov, K G; Basitova, S M; Tashmukhamedova, A K; Sajfullina, N Zh [Tadzhikskij Gosudarstvennyj Univ., Dushanbe (USSR)

1989-10-01

Rhenium and molybdenum complexes in +5 oxidation degree with 4',4''(5'')-ditretbutyldibenzo-24-crown-8 (L) are synthesized with 75-95 % yield. Composition and structure of compounds produced are investigated using element analysis, conductometry, IR spectroscopy, thermogravimetry methods. Oxidation degree of complexer metal is determined. It is ascertained that the compound composition corresponds to the MOLX{sub 3} formula, where M-Re, Mo; X-Cl{sup -}, Br{sup -}.

Band structures of two dimensional solid/air hierarchical phononic crystals

International Nuclear Information System (INIS)

Xu, Y.L.; Tian, X.G.; Chen, C.Q.

2012-01-01

The hierarchical phononic crystals to be considered show a two-order “hierarchical” feature, which consists of square array arranged macroscopic periodic unit cells with each unit cell itself including four sub-units. Propagation of acoustic wave in such two dimensional solid/air phononic crystals is investigated by the finite element method (FEM) with the Bloch theory. Their band structure, wave filtering property, and the physical mechanism responsible for the broadened band gap are explored. The corresponding ordinary phononic crystal without hierarchical feature is used for comparison. Obtained results show that the solid/air hierarchical phononic crystals possess tunable outstanding band gap features, which are favorable for applications such as sound insulation and vibration attenuation.

Band structures of two dimensional solid/air hierarchical phononic crystals

Energy Technology Data Exchange (ETDEWEB)

Xu, Y.L.; Tian, X.G. [State Key Laboratory for Mechanical Structure Strength and Vibration, Xi' an Jiaotong University, Xi' an 710049 (China); Chen, C.Q., E-mail: chencq@tsinghua.edu.cn [Department of Engineering Mechanics, AML and CNMM, Tsinghua University, Beijing 100084 (China)

2012-06-15

The hierarchical phononic crystals to be considered show a two-order 'hierarchical' feature, which consists of square array arranged macroscopic periodic unit cells with each unit cell itself including four sub-units. Propagation of acoustic wave in such two dimensional solid/air phononic crystals is investigated by the finite element method (FEM) with the Bloch theory. Their band structure, wave filtering property, and the physical mechanism responsible for the broadened band gap are explored. The corresponding ordinary phononic crystal without hierarchical feature is used for comparison. Obtained results show that the solid/air hierarchical phononic crystals possess tunable outstanding band gap features, which are favorable for applications such as sound insulation and vibration attenuation.

Crystallization and preliminary X-ray structural studies of adeno-associated virus serotype 6

International Nuclear Information System (INIS)

Xie, Qing; Ongley, Heather M.; Hare, Joan; Chapman, Michael S.

2008-01-01

Adeno-associated virus type 6, a human DNA virus that is being developed as a vector for gene therapy, has been crystallized in a form suitable for structure determination at about 3.2 Å resolution. Adeno-associated viruses are being developed as vectors for gene therapy and have been used in a number of clinical trials. Vectors to date have been based on the type species AAV-2, the structure of which was published in 2002. There is growing interest in modulating the cellular tropism and immune neutralization of AAV-2 with variants inspired by the properties of other serotypes. Towards the determination of a structure for AAV type 6, this paper reports the high-yield production, purification, crystallization and preliminary diffraction studies of infectious AAV-6 virions. The crystals diffracted to 3.2 Å resolution using synchrotron radiation. The most promising crystal form belonged to space group R3 and appeared to be suitable for initial structure determination

Crystal Structure of Cocosin, A Potential Food Allergen from Coconut (Cocos nucifera).

Science.gov (United States)

Jin, Tengchuan; Wang, Cheng; Zhang, Caiying; Wang, Yang; Chen, Yu-Wei; Guo, Feng; Howard, Andrew; Cao, Min-Jie; Fu, Tong-Jen; McHugh, Tara H; Zhang, Yuzhu

2017-08-30

Coconut (Cocos nucifera) is an important palm tree. Coconut fruit is widely consumed. The most abundant storage protein in coconut fruit is cocosin (a likely food allergen), which belongs to the 11S globulin family. Cocosin was crystallized near a century ago, but its structure remains unknown. By optimizing crystallization conditions and cryoprotectant solutions, we were able to obtain cocosin crystals that diffracted to 1.85 Å. The cocosin gene was cloned from genomic DNA isolated from dry coconut tissue. The protein sequence deduced from the predicted cocosin coding sequence was used to guide model building and structure refinement. The structure of cocosin was determined for the first time, and it revealed a typical 11S globulin feature of a double layer doughnut-shaped hexamer.

Low-Temperature Crystal Structures of the Hard Core Square Shoulder Model

Directory of Open Access Journals (Sweden)

Alexander Gabriëlse

2017-11-01

Full Text Available In many cases, the stability of complex structures in colloidal systems is enhanced by a competition between different length scales. Inspired by recent experiments on nanoparticles coated with polymers, we use Monte Carlo simulations to explore the types of crystal structures that can form in a simple hard-core square shoulder model that explicitly incorporates two favored distances between the particles. To this end, we combine Monte Carlo-based crystal structure finding algorithms with free energies obtained using a mean-field cell theory approach, and draw phase diagrams for two different values of the square shoulder width as a function of the density and temperature. Moreover, we map out the zero-temperature phase diagram for a broad range of shoulder widths. Our results show the stability of a rich variety of crystal phases, such as body-centered orthogonal (BCO lattices not previously considered for the square shoulder model.

Use of a new tandem cation/anion exchange system with clinical-scale generators provides high specific volume solutions of technetium-99m and rhenium-188

International Nuclear Information System (INIS)

Knapp, F.R. Jr.; Beets, A.L.; Mirzadeh, S.; Guhlke, S.; Univ. of Bonn

1998-03-01

In this paper the authors describe the first application of a simple and inexpensive post elution tandem cation-anion exchange column system which is based on generator elution with salts of weak acids such as ammonium acetate instead of saline solution to provide very high specific volume solutions of technetium-99m and rhenium-188 from clinical scale molybdenum-99/technetium-99m generator prepared from low specific activity (n,y) molybdenum-99, and tungsten-188/rhenium-188 generators, respectively. Initial passage of the bolus through a strong cation exchange cartridge converts the ammonium acetate to acetic acid which is essentially not ionized at the acidic pH, allowing specific subsequent amine type (QMA SepPak trademark) anion exchange cartridge column trapping of the microscopic levels of the pertechnetate or perrhenate. Subsequent elution of the anion cartridge with a small volume ( 500 mCi/mL) from the alumina-based tungsten-188/rhenium-188 generator

Magnetic interactions in rhenium-containing rare earth double perovskites Sr{sub 2}LnReO{sub 6} (Ln=rare earths)

Energy Technology Data Exchange (ETDEWEB)

Nishiyama, Atsuhide; Doi, Yoshihiro; Hinatsu, Yukio, E-mail: hinatsu@sci.hokudai.ac.jp

2017-04-15

The perovskite-type compounds containing both rare earth and rhenium Sr{sub 2}LnReO{sub 6} (Ln=Y, Tb-Lu) have been prepared. Powder X-ray diffraction measurements and Rietveld analysis show that Ln{sup 3+} and Re{sup 5+} ions are structurally ordered at the B site of the perovskite SrBO{sub 3}. Magnetic anomalies are found in their magnetic susceptibility and specific heat measurements at 2.6–20 K for Ln=Y, Tb, Dy, Yb, Lu compounds. They are due to magnetic interactions between Re{sup 5+} ions. The results of the magnetic hysteresis and remnant magnetization measurements for Sr{sub 2}YReO{sub 6} and Sr{sub 2}LuReO{sub 6} indicate that the antiferromagnetic interactions between Re{sup 5+} ions below transition temperatures have a weak ferromagnetic component. The analysis of the magnetic specific heat data for Sr{sub 2}YbReO{sub 6} shows that both the Yb{sup 3+} and Re{sup 5+} ions magnetically order at 20 K. For the case of Sr{sub 2}DyReO{sub 6}, magnetic ordering of the Re{sup 5+} moments occurs at 93 K, and with decreasing temperature, the moments of Dy{sup 3+} ferromagnetically order at 5 K from the measurements of magnetic susceptibility and specific heat. - Graphical abstract: Crystal structure of double perovskite Sr{sub 2}LnReO{sub 6}. Red and black lines show cubic and monoclinic unit cells, respectively. - Highlights: • Double perovskites Sr{sub 2}LnReO{sub 6} (Ln=rare earths) were prepared. • They show an antiferromagnetic transition at 2.6–20 K. • In Sr{sub 2}DyReO{sub 6}, Dy and Re moments magnetically order at 5 and 93 K, respectively.

X-ray crystal structure and small-angle X-ray scattering of sheep liver sorbitol dehydrogenase

DEFF Research Database (Denmark)

Yennawar, Hemant; Møller, Magda; Gillilan, Richard

2011-01-01

The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer...

Photonic guiding structures in lithium niobate crystals produced by energetic ion beams

Science.gov (United States)

Chen, Feng

2009-10-01

A range of ion beam techniques have been used to fabricate a variety of photonic guiding structures in the well-known lithium niobate (LiNbO3 or LN) crystals that are of great importance in integrated photonics/optics. This paper reviews the up-to-date research progress of ion-beam-processed LiNbO3 photonic structures and reports on their fabrication, characterization, and applications. Ion beams are being used with this material in a wide range of techniques, as exemplified by the following examples. Ion beam milling/etching can remove the selected surface regions of LiNbO3 crystals via the sputtering effects. Ion implantation and swift ion irradiation can form optical waveguide structures by modifying the surface refractive indices of the LiNbO3 wafers. Crystal ion slicing has been used to obtain bulk-quality LiNbO3 single-crystalline thin films or membranes by exfoliating the implanted layer from the original substrate. Focused ion beams can either generate small structures of micron or submicron dimensions, to realize photonic bandgap crystals in LiNbO3, or directly write surface waveguides or other guiding devices in the crystal. Ion beam-enhanced etching has been extensively applied for micro- or nanostructuring of LiNbO3 surfaces. Methods developed to fabricate a range of photonic guiding structures in LiNbO3 are introduced. Modifications of LiNbO3 through the use of various energetic ion beams, including changes in refractive index and properties related to the photonic guiding structures as well as to the materials (i.e., electro-optic, nonlinear optic, luminescent, and photorefractive features), are overviewed in detail. The application of these LiNbO3 photonic guiding structures in both micro- and nanophotonics are briefly summarized.

Coefficient of crystal lattice matching as a parameter of substrate - crystal structure compatibility in silumins

Directory of Open Access Journals (Sweden)

J. Piątkowski

2009-07-01

Full Text Available Adding high-melting point elements (Mo, Nb, Ni, Ti, W to complex silumins results in hardening of the latter ones, owing to the formation of new intermetallic phases of the AlxMey type, with refinement of dendrites in α solution and crystals in β phase. The hardening is also due to the effect of various inoculants. An addition of the inoculant is expected to form substrates, the crystal lattice of which, or some (privileged lattice planes and interatomic spaces should bear a strong resemblance to the crystal nucleus. To verify this statement, using binary phase equilibria systems, the coefficient of crystal lattice matching, being one of the measures of the crystallographic similarity, was calculated. A compatibility of this parameter (up to 20% may decide about the structure compatibility between the substrate and crystal which, in turn, is responsible for the effectiveness of alloy modification. Investigations have proved that, given the temperature range of their formation, the density, the lattice type, and the lattice parameter, some intermetallic phases of the AlxMey type can act as substrates for the crystallisation of aluminium and silicon, and some of the silumin hardening phases.

Synthesis, characterization and crystal structure of a ...

African Journals Online (AJOL)

The Mo atom in the complex is in octahedral coordination. Thermal stability of the complex has also been studied. KEY WORDS: Molybdenum complex, Hydrazone ligand, Crystal structure, X-ray diffraction, Thermal property. Bull. Chem. Soc. Ethiop. 2014, 28(3), 409-414. DOI: http://dx.doi.org/10.4314/bcse.v28i3.10 ...

Crystal structure of ethyl 2,4-dichloroquinoline-3-carboxylate

Directory of Open Access Journals (Sweden)

Alberto Cabrera

2015-12-01

Full Text Available In the crystal structure of the title compound, C12H9Cl2NO2, the mean planes through the quinoline and carboxylate groups have r.m.s. deviations of 0.006 and 0.021 Å, respectively, and form a dihedral angle of 87.06 (19°. In the crystal, molecules are linked via very weak C—H...O hydrogen bonds, forming chains, which propagate along the c-axis direction.

Chalcogenhalide cluster rhenium- and molybdenum complexes

International Nuclear Information System (INIS)

Fedin, V.P.; Gubin, S.P.; Mishchenko, A.V.; Fedorov, V.E.

1984-01-01

The interaction of rhenium- and molybdenum chalcogenhalides with n-donor ligands (L) is studied. At heating Re 3 X 2 Hal 5 complexes up to 100 deg in DMSO in the L presence obtained are the complexes of the 1-6 composition Re 3 X 2 Hal 5 -x Lx DMSO (X=Se, Hal=Cl, L=Et 3 N(1); X=Se, Hal=Cl, L=Bipy(2); X=Se, Hal=Br, L=Et 3 N(3); X=Se, Hal=Br, L=Bipy(4); X=Te, Hal=Br, L=Et 3 N(5); X=Te, Hal=Br, L=(Me 2 NCH 2 ) 2 (6). In the course of boiling of Mo 3 S 7 Hal 4 with PPh 3 in MeCN the Mo 3 S 7 Hal 4 2PPh 3 complexes (Hal=Cl(7); Br(8)) are obtained. For 1 through 8 complexes the chemical analysis data and IR spectra are given. For 4 and 8 complexes the molecular mass is measured. A possible method of obtaining molecular trinuclear clusters from polymer clusters is discussed

The crystal structure of bøgvadite (Na2SrBa2Al4F20)

DEFF Research Database (Denmark)

Balic Zunic, Tonci

2014-01-01

The crystal structure of bøgvadite, Na2SrBa2Al4F20, has been solved and refined to a R1 factor of 4.4% from single-crystal data (MoKα X-ray diffraction, CCD area detector) on a sample from the cryolite deposit at Ivittuut, SW Greenland. Bøgvadite is monoclinic, P21/n space group, with unit cell...... parameters a= 7.134(1), b= 19.996(3) and c= 5.3440(8) Å, β = 90.02(1)o. A close proximity of the crystal structure to an orthorhombic symmetry and the presence of the two twin components in a nearly 1:1 ratio suggest that the investigated bøgvadite crystal has originally formed as a high......-temperature orthorhombic polymorph which on cooling transformed to the stable low temperature monoclinic structure. The bøgvadite crystal structure has groupings of cation-fluoride coordination polyhedra similar to those found in the crystal structures of the genetically closely associated minerals jarlite...

Synthesis, Crystal Structure, and DFT Calculations of 1,3-Diisobutyl Thiourea

Directory of Open Access Journals (Sweden)

Ataf A. Altaf

2015-01-01

Full Text Available 1,3-Diisobutyl thiourea was synthesized and characterized by single crystal X-ray diffraction. It gives a monoclinic (α = γ = 90 and β  ≠ 90 structure with the space group P21/c. The unit cell dimensions are a = 11.5131 (4 Å, b = 9.2355 (3 Å, c = 11.3093 (5 Å, α = 90°, β = 99.569° (2, γ = 90°, V = 1185.78 (8 Å3, and Z = 4. The crystal packing is stabilized by intermolecular (N–H⋯S hydrogen bonding in the molecules. The optimized geometry and Mullikan's charges of the said molecule calculated with the help of DFT using B3LYP-6-311G model support the crystal structure.

The crystal structures of three pyrazine-2,5-dicarboxamides: three-dimensional supramolecular structures

Directory of Open Access Journals (Sweden)

Dilovan S. Cati

2017-05-01

Full Text Available The complete molecules of the title compounds, N2,N5-bis(pyridin-2-ylmethylpyrazine-2,5-dicarboxamide, C18H16N6O2 (I, 3,6-dimethyl-N2,N5-bis(pyridin-2-ylmethylpyrazine-2,5-dicarboxamide, C20H20N6O2 (II, and N2,N5-bis(pyridin-4-ylmethylpyrazine-2,5-dicarboxamide, C18H16N6O2 (III, are generated by inversion symmetry, with the pyrazine rings being located about centres of inversion. Each molecule has an extended conformation with the pyridine rings inclined to the pyrazine ring by 89.17 (7° in (I, 75.83 (8° in (II and by 82.71 (6° in (III. In the crystal of (I, molecules are linked by N—H...N hydrogen bonds, forming layers lying parallel to the bc plane. The layers are linked by C—H...O hydrogen bonds, forming a three-dimensional supramolecular structure. In the crystal of (II, molecules are also linked by N—H...N hydrogen bonds, forming layers lying parallel to the (10-1 plane. As in (I, the layers are linked by C—H...O hydrogen bonds, forming a three-dimensional supramolecular structure. In the crystal of (III, molecules are again linked by N—H...N hydrogen bonds, but here form corrugated sheets lying parallel to the bc plane. Within the sheets, neighbouring pyridine rings are linked by offset π–π interactions [intercentroid distance = 3.739 (1 Å]. The sheets are linked by C—H...O hydrogen bonds, forming a three-dimensional supramolecular structure. Compound (I crystallizes in the monoclinic space group P21/c. Another monoclinic polymorph, space group C2/c, has been reported on by Cockriel et al. [Inorg. Chem. Commun. (2008, 11, 1–4]. The molecular structures of the two polymorphs are compared.

Crystal structure of natural phaeosphaeride A

Directory of Open Access Journals (Sweden)

Victoria V. Abzianidze

2015-08-01

Full Text Available The asymmetric unit of the title compound, C15H23NO5, contains two independent molecules. Phaeosphaeride A contains two primary sections, an alkyl chain consisting of five C atoms and a cyclic system consisting of fused five- and six-membered rings with attached substituents. In the crystal, the molecules form layered structures. Nearly planar sheets, parallel to the (001 plane, form bilayers of two-dimensional hydrogen-bonded networks with the hydroxy groups located on the interior of the bilayer sheets. The network is constructed primarily of four O—H...O hydrogen bonds, which form a zigzag pattern in the (001 plane. The butyl chains interdigitate with the butyl chains on adjacent sheets. The crystal was twinned by a twofold rotation about the c axis, with refined major–minor occupancy fractions of 0.718 (6:0.282 (6.

Molecular complex of lumiflavin and 2-aminobenzoic acid: crystal structure, crystal spectra, and solution properties.

Science.gov (United States)

Shieh, H S; Ghisla, S; Hanson, L K; Ludwig, M L; Nordman, C E

1981-08-04

The molecular complex lumiflavin-2-aminobenzoic acid monohydrate (C13H12N4O2.C7H7NO2.H2O) crystallizes from from aqueous solution as red triclinic prisms. The space group is P1 with cell dimensions a = 9.660 A, b = 14.866 A, c = 7.045 A, alpha = 95.44 degrees , beta = 95.86 degrees, and gamma = 105.66 degrees . The crystal structure was solved by direct methods and refined by block-diagonal least-squares procedures to an R value of 0.050 on the basis of 1338 observed reflections. The structure is composed of stacks of alternating lumiflavin adn un-ionized (neutral) 2-aminobenzoic acid molecules. Two different modes of stacking interaction are observed. In one, 2-aminobenzoic acid overlaps all three of the isoalloxazine rings, at a mean distance of 3.36 A; in the other, 2-aminobenzoic acid interacts distance of 3.36 A; in the other, 2-aminobenzoic acid interacts with the pyrazine and dimethylbenzene moieties, at a distance of 3.42 A. Perpendicular to the stacking direction, the molecules form a continuous sheet. Each flavin is hydrogen bonded via O(2) and NH(3) to two symmetrically related aminobenzoates; the water of crystallization forms three hydrogen bonds, bridging two flavins, via O(4) and N(5), and one aminobenzoic acid. The red color of the crystals results from a charge-transfer transition involving stacked flavin and 2-aminobenzoic acid. The red color of the crystals results from a charge-transfer transition involving stacked flavin and 2-aminobenzoic acid molecules. Measurements of the polarized optical absorption spectra of crystals show that the transition moment direction for the long wavelength absorbance (beyond 530 nm) contains an out-of-plane component which can only arise from a charge-transfer interaction. Since the amino N does not make exceptionally close interactions with isoalloxazine atoms in either stacking mode (minimum interatomic distance 3.52 A), the charge transfer is presumed to involve pi orbitals of the 2-aminobenzoic acid donor.

On the crystal structure of Z-phase Cr(V,Nb)N

DEFF Research Database (Denmark)

Danielsen, Hilmar Kjartansson; Hald, John; Grumsen, Flemming Bjerg

2006-01-01

The Z-phase Cr(YNb)N particles in various 9 to 12 pct Cr creep-resistant steels were investigated with electron diffraction, energy dispersive spectroscopy (EDS), and electron energy loss spectroscopy(EELS). In addition to the well-known tetragonal crystal structure for Z phase, a cubic crystal s...

One dimensional coordination polymers: Synthesis, crystal structures and spectroscopic properties

Science.gov (United States)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

2016-11-01

Two new one dimensional (1D) cyanide complexes, namely [M(4-aepy)2(H2O)2][Pt(CN)4], (4-aepy = 4-(2-aminoethyl)pyridine M = Cu(II) (1) or Zn(II) (2)), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. The crystallographic analyses reveal that 1 and 2 are isomorphous and isostructural, and crystallize in the monoclinic system and C2 space group. The Pt(II) ions are coordinated by four cyanide-carbon atoms in the square-planar geometry and the [Pt(CN)4]2- ions act as a counter ion. The M(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4-aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. The crystal structures of 1 and 2 are similar each other and linked via intermolecular hydrogen bonding, Pt⋯π interactions to form 3D supramolecular network. Vibration assignments of all the observed bands are given and the spectral features also supported to the crystal structures of the complexes.

Probing Zeolite Crystal Architecture and Structural Imperfections using Differently Sized Fluorescent Organic Probe Molecules.

Science.gov (United States)

Hendriks, Frank C; Schmidt, Joel E; Rombouts, Jeroen A; Lammertsma, Koop; Bruijnincx, Pieter C A; Weckhuysen, Bert M

2017-05-05

A micro-spectroscopic method has been developed to probe the accessibility of zeolite crystals using a series of fluorescent 4-(4-diethylaminostyryl)-1-methylpyridinium iodide (DAMPI) probes of increasing molecular size. Staining large zeolite crystals with MFI (ZSM-5) topology and subsequent mapping of the resulting fluorescence using confocal fluorescence microscopy reveal differences in structural integrity: the 90° intergrowth sections of MFI crystals are prone to develop structural imperfections, which act as entrance routes for the probes into the zeolite crystal. Polarization-dependent measurements provide evidence for the probe molecule's alignment within the MFI zeolite pore system. The developed method was extended to BEA (Beta) crystals, showing that the previously observed hourglass pattern is a general feature of BEA crystals with this morphology. Furthermore, the probes can accurately identify at which crystal faces of BEA straight or sinusoidal pores open to the surface. The results show this method can spatially resolve the architecture-dependent internal pore structure of microporous materials, which is difficult to assess using other characterization techniques such as X-ray diffraction. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

Band structure and optical properties of opal photonic crystals

Science.gov (United States)

Pavarini, E.; Andreani, L. C.; Soci, C.; Galli, M.; Marabelli, F.; Comoretto, D.

2005-07-01

A theoretical approach for the interpretation of reflectance spectra of opal photonic crystals with fcc structure and (111) surface orientation is presented. It is based on the calculation of photonic bands and density of states corresponding to a specified angle of incidence in air. The results yield a clear distinction between diffraction in the direction of light propagation by (111) family planes (leading to the formation of a stop band) and diffraction in other directions by higher-order planes (corresponding to the excitation of photonic modes in the crystal). Reflectance measurements on artificial opals made of self-assembled polystyrene spheres are analyzed according to the theoretical scheme and give evidence of diffraction by higher-order crystalline planes in the photonic structure.

Crystals structure of Na3Li(TiF6)2

International Nuclear Information System (INIS)

Popov, D.Yu.; Antokhina, T.F.; Gerasimenko, A.V.; Kajdalova, T.A.; Sergienko, V.I.

2004-01-01

Crystals of Na 3 Li(TiF 6 ) 2 (1) were synthesized in aqueous solution and characterized by the elementary and X-ray phase analysis methods. According to X-ray diffraction analysis data compound 1 is crystallized in a tetragonal crystal system with the following parameters: a=5.130(1), c=18.046(4) A, Z=2, space group P4-bar2 1 c. Alternating layers on the basis of dimers made up by octahedrons of TiF 6 and Na(1)F 6 constitute the frame of compound 1 crystal structure. The dimer layers are joined in a continuous frame by Na(2) and Li cations. Coordination polyhedron of Li atom is tetrahedron (Li-F 1.898(3) A) [ru

CCDC 963856: Experimental Crystal Structure Determination : catena-[bis(mu2-2-methylimidazole)-zinc

KAUST Repository

Shekhah, Osama; Swaidan, Raja; Belmabkhout, Youssef; du Plessis, Marike; Jacobs, Tia; Barbour, Leonard J.; Pinnau, Ingo; Eddaoudi, Mohamed

2014-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1477679: Experimental Crystal Structure Determination : (1,3-dimesitylimidazolidin-2-ylidene)-trimethyl-indium

KAUST Repository

Wu, Melissa M.; Gill, Arran M.; Yunpeng, Lu; Yongxin, Li; Ganguly, Rakesh; Falivene, Laura; Garcí a, Felipe

2017-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1477678: Experimental Crystal Structure Determination : (1,3-dimesitylimidazolidin-2-ylidene)-trimethyl-gallium

KAUST Repository

Wu, Melissa M.; Gill, Arran M.; Yunpeng, Lu; Yongxin, Li; Ganguly, Rakesh; Falivene, Laura; Garcí a, Felipe

2017-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1059905: Experimental Crystal Structure Determination : 7,13-dimesitylindeno[1,2-b]thioxanthene

KAUST Repository

Shi, Xueliang; Kueh, Weixiang; Zheng, Bin; Huang, Kuo-Wei; Chi, Chunyan

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 844302: Experimental Crystal Structure Determination : N-1-Naphthyl-P,P-diphenylphosphinoselenoic amide

KAUST Repository

Al-Masri, H.T.; Emwas, Abdul-Hamid M.; Al-Talla, Zeyad; Al Kordi, Mohamed

2012-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1010350: Experimental Crystal Structure Determination : dichloro-(methylenebis(di-t-butylphosphine))-palladium(ii)

KAUST Repository

Roesle, Philipp; Caporaso, Lucia; Schnitte, Manuel; Goldbach, Verena; Cavallo, Luigi; Mecking, Stefan

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 721713: Experimental Crystal Structure Determination : Dichloro-(ethyl phenylalaninate)-tris(pyridine)-ruthenium(ii)

KAUST Repository

Reiner, Thomas; Jantke, Dominik; Miao, Xiao-He; Marziale, Alexander N.; Kiefer, Florian J.; Eppinger, Jö rg

2013-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 713130: Experimental Crystal Structure Determination : bis(2,5-Dihydrobenzylammonium) hexachloro-osmium(iv)

KAUST Repository

Reiner, T.

2011-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1420581: Experimental Crystal Structure Determination : catena-[(mu-4,4'-sulfonyldibenzoato)-calcium ethylene

KAUST Repository

Plonka, Anna M.

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1420582: Experimental Crystal Structure Determination : catena-[(mu-4,4'-sulfonyldibenzoato)-calcium ethane

KAUST Repository

Plonka, Anna M.

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1420580: Experimental Crystal Structure Determination : catena-[(mu-4,4'-sulfonyldibenzoato)-calcium acetylene

KAUST Repository

Plonka, Anna M.

2016-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

CCDC 1048729: Experimental Crystal Structure Determination : bis(2-(hydroxyimino)-3-phenylpropanoato)-tin(ii)

KAUST Repository

Khanderi, Jayaprakash

2015-01-01

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

Effect of antimony incorporation on structural properties of CuInS2 crystals

International Nuclear Information System (INIS)

Ben Rabeh, M.; Chaglabou, N.; Kanzari, M.

2010-01-01

CuInS 2 (CIS) single crystals doped with 1, 2, 3 and 4 atomic percent (at.%) of antimony (Sb) were grown by the horizontal Bridgman method. The effect of Sb doping on the structural properties of CIS crystal was studied by means of X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM) and PL measurements. X-ray diffraction data suggests that the doping of Sb in the CIS single crystals does not affect the tetragonal (chalcopyrite) crystal structure and exhibited a (1 1 2) preferred orientation. In addition, with increasing Sb concentration, the X-ray diffraction analysis show that Sb doped CIS crystals are more crystallized and the diffraction peaks of the CuInS 2 phase were more pronounced in particular the (1 1 2) plane. EDAX study revealed that Sb atoms can occupy the indium site and/or occupying the sulfur site to make an acceptor. PL spectra of undoped and Sb doped CIS crystals show two emission peaks at 1.52 and 1.62 eV, respectively which decreased with increasing atomic percent antimony. Sb doped CIS crystals show p-type conductivity.

Crystal structures of two eukaryotic nucleases involved in RNA metabolism

DEFF Research Database (Denmark)

Jonstrup, Anette Thyssen; Midtgaard, Søren Fuglsang; Van, Lan Bich

RNA serves a number of functions in the cell: mRNAs are the carriers of information between gene and protein, tRNAs and rRNAs are involved in the synthesis of proteins, whereas a number of additional RNA species are responsible for other functions in the cell. The quality of the different RNAs...... RNAs. We have solved the structures of two nucleases involved in 3'-5' degradation of RNA; the S. pombe Pop2p and the S. cerevisiae Rrp6p. Pop2p is part of the main cytoplasmatic deadenylation complex in yeast, which also contains the nuclease Ccr4p. Deadenylation, where the poly(A)-tail is removed...... specific transcripts. Here, we present the crystal structure of the S. pombe Pop2p protein to 1.4 Å resolution. The high resolution structure provides a clear picture of the active site architecture. Structural alignment of single nucleotides and poly(A)-oligonucleotides from earlier co-crystal structures...

Crystal structure, vibrational and DFT simulation studies of melaminium dihydrogen phosphite monohydrate

Science.gov (United States)

Arjunan, V.; Kalaivani, M.; Marchewka, M. K.; Mohan, S.

2013-08-01

The crystal structure investigations of melamine with phosphorous acid, namely melaminium dihydrogenphosphite monohydrate (C3N6H7·H2PO3·H2O) have been investigated by means of single crystal X-ray diffraction method. The title compound crystallizes in monoclinic crystal system, and the space group is P21/c with a = 10.069 Å, b = 21.592 Å, c = 12.409 Å and Z = 12. The vibrational assignments and analysis of melaminium dihydrogen phosphite monohydrate have also been performed by FTIR, FT-Raman and far-infrared spectral studies. The quantum chemical simulations were performed with DFT (B3LYP) method using 6-31G**, cc-pVTZ, and 6-311++G** basis sets to determine the energy, structural, thermodynamic parameters and vibrational frequencies of melaminium dihydrogen phosphite monohydrate. The hydrogen atom from phosphorous acid was transferred to the melamine molecule giving the singly protonated melaminium cation. The ability of ions to form spontaneous three-dimensional structure through weak Osbnd H···O and Nsbnd H···O hydrogen bonds shows notable vibrational effects.

Comparison of NMR and crystal structures for the proteins TM1112 and TM1367

International Nuclear Information System (INIS)

Mohanty, Biswaranjan; Serrano, Pedro; Pedrini, Bill; Jaudzems, Kristaps; Geralt, Michael; Horst, Reto; Herrmann, Torsten; Elsliger, Marc-André; Wilson, Ian A.; Wüthrich, Kurt

2010-01-01

NMR structures of the proteins TM1112 and TM1367 solved by the JCSG in solution at 298 K could be superimposed with the corresponding crystal structures at 100 K with r.m.s.d. values of <1.0 Å for the backbone heavy atoms. For both proteins the structural differences between multiple molecules in the asymmetric unit of the crystals correlated with structural variations within the bundles of conformers used to represent the NMR solution structures. A recently introduced JCSG NMR structure-determination protocol, which makes use of the software package UNIO for extensive automation, was further evaluated by comparison of the TM1112 structure obtained using these automated methods with another NMR structure that was independently solved in another PSI center, where a largely interactive approach was applied. The NMR structures of the TM1112 and TM1367 proteins from Thermotoga maritima in solution at 298 K were determined following a new protocol which uses the software package UNIO for extensive automation. The results obtained with this novel procedure were evaluated by comparison with the crystal structures solved by the JCSG at 100 K to 1.83 and 1.90 Å resolution, respectively. In addition, the TM1112 solution structure was compared with an NMR structure solved by the NESG using a conventional largely interactive methodology. For both proteins, the newly determined NMR structure could be superimposed with the crystal structure with r.m.s.d. values of <1.0 Å for the backbone heavy atoms, which provided a starting platform to investigate local structure variations, which may arise from either the methods used or from the different chemical environments in solution and in the crystal. Thereby, these comparative studies were further explored with the use of reference NMR and crystal structures, which were computed using the NMR software with input of upper-limit distance constraints derived from the molecular models that represent the results of structure

Crystal structures of two thiacalix[4]arene derivatives anchoring four ...

Indian Academy of Sciences (India)

Administrator

Abstract. The crystal structures of two thiacalixarene derivatives anchoring thiadiazole functional groups at lower rim, C60H72O4S12N8 (1), C64H80O4S12N8 (2), have been determined by single crystal X-ray diffraction. The thiacalix[4]arene framework in both 1 and 2 adopts the 1,3-alternate conformation. Com- pound 1 ...

Crystal chemistry of nephelines from ijolites and nepheline-rich pegmatites: influence of composition and genesis on the crystal structure investigated by X-ray diffraction

DEFF Research Database (Denmark)

Vulić, Predrag; Balić-Žunić, Tonči; Belmonte, Louise Josefine

2011-01-01

Ten nepheline single crystals from five different localities representing rocks from nepheline-syenite pegmatites to urtite, ijolite and cancrinite-ijolite were investigated chemically and structurally. The chemical compositions were determined by electron microprobe, whereas the crystal structur...

Crystal Structure of Rat Carnitine Palmitoyltransferase II (CPT-II)

Energy Technology Data Exchange (ETDEWEB)

Hsiao,Y.; Jogl, G.; Esser, V.; Tong, L.

2006-01-01

Carnitine palmitoyltransferase II (CPT-II) has a crucial role in the {beta}-oxidation of long-chain fatty acids in mitochondria. We report here the crystal structure of rat CPT-II at 1.9 Angstroms resolution. The overall structure shares strong similarity to those of short- and medium-chain carnitine acyltransferases, although detailed structural differences in the active site region have a significant impact on the substrate selectivity of CPT-II. Three aliphatic chains, possibly from a detergent that is used for the crystallization, were found in the structure. Two of them are located in the carnitine and CoA binding sites, respectively. The third aliphatic chain may mimic the long-chain acyl group in the substrate of CPT-II. The binding site for this aliphatic chain does not exist in the short- and medium-chain carnitine acyltransferases, due to conformational differences among the enzymes. A unique insert in CPT-II is positioned on the surface of the enzyme, with a highly hydrophobic surface. It is likely that this surface patch mediates the association of CPT-II with the inner membrane of the mitochondria.

X-ray absorption spectroscopy investigation of structurally modified lithium niobate crystals

International Nuclear Information System (INIS)

Vitova, Tonya

2008-02-01

The type and concentration of impurity centers in different valence states are crucial for tuning the photorefractive properties of doped Lithium Niobate (LN) crystals. X-ray Absorption Spectroscopy (XAS) is an appropriate tool for studying the local structure of impurity centers. XAS combined with absorption in UV/VIS/IR and High Resolution X-ray Emission Spectroscopy (HRXES) provide information about the valence state of the dopant ions in as-grown, reduced or oxidized doped LN crystals. Cu (Cu 1+ and Cu 2+ ) and Fe (Fe 2+ and Fe 3+ ) atoms are found in two different valence states, whereas there are indications for a third Mn valency, in addition to Mn 2+ and Mn 3+ in manganese-doped LN crystals. One of the charge compensation mechanisms during reduction of copper- doped LN crystals is outgassing of oxygen atoms. Cu ions in the reduced crystals have at least two different site symmetries: twofold (Cu 1+ ) and sixfold (Cu 2+ ) coordinated by O atoms. Fe and Mn atoms are coordinated by six O atoms. Cu and Fe ions are found to occupy only Li sites, whereas Mn ions are also incorporated into Li and Nb sites. The refractive index change in LN crystals irradiated with 3 He 2+ ions is caused by structurally disordered centers, where Nb atoms are displaced from normal crystallographic sites and Li or/and O vacancies are present. (orig.)

Shear effects on crystallization behaviors and structure transitions of isotactic poly-1-butene

DEFF Research Database (Denmark)

Li, Jingqing; Guan, Peipei; Zhang, Yao

2014-01-01

Different melt pre-shear conditions were applied to isotactic poly-1-butene (iP-1-B) and the effect on the crystallization behaviors and the crystalline structure transitions of iP-1-B were investigated. The polarized optical microscope observations during isothermal crystallization process...... revealed that the applied melt pre-shear within the experimental range could enhance the nucleation of crystal II and accelerate the diameter growth of the formed spherulites. If the applied melt pre-shear rate was large enough, Shish-Kebabs structure could be formed. After the isothermal crystallization...... was formed in the melt pre-sheared iP-1-B samples. Further investigations were applied with synchrotron radiation instruments. Wide angle X-ray scattering (WAXS) and small angle X-ray scattering (SAXS) after the crystal transition showed that the applied melt pre-shear could result in orientated fine...

Structural insights into the mycobacteria transcription initiation complex from analysis of X-ray crystal structures

Energy Technology Data Exchange (ETDEWEB)

Hubin, Elizabeth A.; Lilic, Mirjana; Darst, Seth A.; Campbell, Elizabeth A.

2017-07-13

The mycobacteria RNA polymerase (RNAP) is a target for antimicrobials against tuberculosis, motivating structure/function studies. Here we report a 3.2 Å-resolution crystal structure of a Mycobacterium smegmatis (Msm) open promoter complex (RPo), along with structural analysis of the Msm RPo and a previously reported 2.76 Å-resolution crystal structure of an Msm transcription initiation complex with a promoter DNA fragment. We observe the interaction of the Msm RNAP α-subunit C-terminal domain (αCTD) with DNA, and we provide evidence that the αCTD may play a role in Mtb transcription regulation. Our results reveal the structure of an Actinobacteria-unique insert of the RNAP β' subunit. Finally, our analysis reveals the disposition of the N-terminal segment of Msm σA, which may comprise an intrinsically disordered protein domain unique to mycobacteria. The clade-specific features of the mycobacteria RNAP provide clues to the profound instability of mycobacteria RPo compared with E. coli.

NATO Advanced Study Institute on Electronic Structure of Polymers and Molecular Crystals

CERN Document Server

Ladik, János

1975-01-01

The NATO Advanced Study Institute on "Electronic Structure of Polymers and Molecular Crystals" was held at the Facultes Universi­ taires de Namur (F.U.N.) from September 1st till September 14th, 1974. We wish to express our appreciation to the NATO Scientific Affairs Division whose generous support made this Institute possible and to the Facultes Universitaires de Namur and the Societe Chimique de Belgique which provided fellowships and travel grants to a number of students. This volume contains the main lectures about the basic principles of the field and about different recent developments of the theory of the electronic structure of polymers and molecular crystals. The school started with the presentation of the basic SCF-LCAO theory of the electronic structure of periodic polymers and molecular crystals (contributions by Ladik, Andre & Delhalle) showing how a combination of quantum chemical and solid state physical methods can provide band structures for these systems. The numerical aspects of these ...

High-throughput crystal-optimization strategies in the South Paris Yeast Structural Genomics Project: one size fits all?

Science.gov (United States)

Leulliot, Nicolas; Trésaugues, Lionel; Bremang, Michael; Sorel, Isabelle; Ulryck, Nathalie; Graille, Marc; Aboulfath, Ilham; Poupon, Anne; Liger, Dominique; Quevillon-Cheruel, Sophie; Janin, Joël; van Tilbeurgh, Herman

2005-06-01

Crystallization has long been regarded as one of the major bottlenecks in high-throughput structural determination by X-ray crystallography. Structural genomics projects have addressed this issue by using robots to set up automated crystal screens using nanodrop technology. This has moved the bottleneck from obtaining the first crystal hit to obtaining diffraction-quality crystals, as crystal optimization is a notoriously slow process that is difficult to automatize. This article describes the high-throughput optimization strategies used in the Yeast Structural Genomics project, with selected successful examples.

The crystal structure of human GDP-L-fucose synthase.

Science.gov (United States)

Zhou, Huan; Sun, Lihua; Li, Jian; Xu, Chunyan; Yu, Feng; Liu, Yahui; Ji, Chaoneng; He, Jianhua

2013-09-01

Human GDP-l-fucose synthase, also known as FX protein, synthesizes GDP-l-fucose from its substrate GDP-4-keto-6-deoxy-d-mannose. The reaction involves epimerization at both C-3 and C-5 followed by an NADPH-dependent reduction of the carbonyl at C-4. In this paper, the first crystal structure of human FX protein was determined at 2.37 Å resolution. The asymmetric unit of the crystal structure contains four molecules which form two homodimers. Each molecule consists of two domains, a Rossmann-fold NADPH-binding motif and a carboxyl terminal domain. Compared with the Escherichia coli GDP-l-fucose synthase, the overall structures of these two enzymes have four major differences. There are four loops in the structure of human FX protein corresponding to two α-helices and two β-sheets in that of the E. coli enzyme. Besides, there are seven different amino acid residues binding with NAPDH comparing human FX protein with that from E. coli. The structure of human FX reveals the key catalytic residues and could be useful for the design of drugs for the treatment of inflammation, auto-immune diseases, and possibly certain types of cancer.

Synthesis, crystal structure and electronic structure of the binary phase Rh{sub 2}Cd{sub 5}

Energy Technology Data Exchange (ETDEWEB)

Koley, Biplab [Department of Chemistry, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India); Chatterjee, S. [Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India); Jana, Partha P., E-mail: ppj@chem.iitkgp.ernet.in [Department of Chemistry, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India)

2017-02-15

A new phase in the Rh-Cd binary system - Rh{sub 2}Cd{sub 5} has been identified and characterized by single crystal X-ray diffraction and Energy dispersive X-ray analysis. The stoichiometric compound Rh{sub 2}Cd{sub 5} crystallizes with a unit cell containing 14 atoms, in the orthorhombic space group Pbam (55). The crystal structure of Rh{sub 2}Cd{sub 5} can be described as a defect form of the In{sub 3}Pd{sub 5} structure with ordered vacancies, formed of two 2D atomic layers with the stacking sequence: ABAB. The A type layers consist of (3.6.3.6)-Kagomé nets of Cd atoms while the B type layers consist of (3{sup 5}) (3{sup 7})- nets of both Cd and Rh atoms. The stability of this line phase is investigated by first principle electronic structure calculations on the model of ordered Rh{sub 2}Cd{sub 5}. - Graphical abstract: (3.6.3.6)-Kagomé nets of cadmium atoms (top) and (3{sup 5}) (3{sup 7})- nets of both cadmium and rhodium atoms (bottom) in the structure of Rh{sub 2}Cd{sub 5}.

Crystal structure of di-( N-methylmorpholine betaine)- L(+)-tartrate

Science.gov (United States)

Dega-Szafran, Z.; Dutkiewicz, G.; Kosturkiewicz, Z.; Szafran, M.

2002-11-01

The crystal structure of di-( N-methylmorpholine betaine)- L(+)-tartrate has been determined by X-ray diffraction method. Crystals are orthorhombic, space group P2 12 12 1, a=9.580(1), b=12.208(1), c=18.677(1) Å, Z=4, R=0.037. The molecule of L(+)-tartaric acid appears in the extended form with the hydroxyl groups as well as carboxyl groups in anti positions. The molecule is involved in a number of the intra- and intermolecular hydrogen bonds. The COOH groups of the tartaric acid link two non-equivalent N-methylmorpholine betaine molecules by a short, intermolecular O-H⋯O bonds of the lengths 2.456(1) and 2.510(1) Å. The OH groups form two different bifurcated hydrogen bonds, the intramolecular with the CO oxygen atoms (2.641(2) and 2.638(2) Å) and the intermolecular (2.919(2) and 3.084(2) Å) with neighbouring tartaric acid molecules, and link complexes in the zigzag ribbon parallel to the x-axis. The morpholine rings of both betaine molecules are in chair conformation with methyl groups in an axial position and CH 2COO - substituents in an equatorial one. In the crystals and the PM3-optimized structures there is no symmetry, both in the tartrate and N-methylmorpholine betaine moieties. FTIR spectrum confirms the complex structure of the investigated molecule.

Tunable alumina 2D photonic-crystal structures via biomineralization of peacock tail feathers

Science.gov (United States)

Jiang, Yonggang; Wang, Rui; Feng, Lin; Li, Jian; An, Zhonglie; Zhang, Deyuan

2018-04-01

Peacock tail feathers with subtle periodic nanostructures exhibit diverse striking brilliancy, which can be applied as natural templates to fabricate artificial photonic crystals (PhCs) via a biomineralization method. Alumina photonic-crystal structures are successfully synthesized via an immersion and two-step calcination process. The lattice constants of the artificial PhCs are greatly reduced compared to their natural matrices. The lattice constants are tunable by modifying the final annealing conditions in the biomineralization process. The reflection spectra of the alumina photonic-crystal structures are measured, which is related to their material and structural parameters. This work suggests a facile fabrication process to construct alumina PhCs with a high-temperature resistance.

Twinning structures in near-stoichiometric lithium niobate single crystals

International Nuclear Information System (INIS)

Yao, Shuhua; Chen, Yanfeng

2010-01-01

A near-stoichiometric lithium niobate single crystal has been grown by the Czochralski method in a hanging double crucible with a continuous powder supply system. Twins were found at one of the three characteristic growth ridges of the as-grown crystal. The twin structure was observed and analyzed by transmission synchrotron topography. The image shifts ΔX and ΔY in the transmission synchrotron topograph were calculated for the 3 anti 2 anti 12 and 0 anti 222 reflections based on results from high-resolution X-ray diffractometry. It is confirmed that one of the {01 anti 1 anti 2} m planes is the composition face of the twin and matrix crystals. The formation mechanism of these twins is discussed. (orig.)

Crystal structure and spin state of mixed-crystals of iron with zinc and cobalt for the assembled complexes bridged by 1,3-bis(4-pyridyl)propanes

Energy Technology Data Exchange (ETDEWEB)

Dote, Haruka [Hiroshima University, Graduate School of Science (Japan); Nakashima, Satoru, E-mail: snaka@hiroshima-u.ac.jp [Hiroshima University, Natural Science Center for Basic Research and Development (Japan)

2012-03-15

Mixed crystals of cobalt and zinc were synthesized using 1,3-bis(4-pyridyl)propane (bpp) as bridging ligand and NCS{sup - } as anion. Red crystals and blue crystals were obtained. Powder X-ray diffraction patterns showed that the former is in 2D interpenetrated structure, while the latter has the same structure with Zn(NCS){sub 2}(bpp). Iron ion was introduced both into the red crystals and blue crystals of the mixed crystals of cobalt with zinc. {sup 57}Fe Moessbauer spectrum of the red crystals showed a main doublet of Fe{sup II} high-spin state at 78 K, while the spectrum of blue crystals did not show Fe{sup II} high-spin state at 78 K.

Crystal structure and spin state of mixed-crystals of iron with zinc and cobalt for the assembled complexes bridged by 1,3-bis(4-pyridyl)propanes

International Nuclear Information System (INIS)

Dote, Haruka; Nakashima, Satoru

2012-01-01

Mixed crystals of cobalt and zinc were synthesized using 1,3–bis(4–pyridyl)propane (bpp) as bridging ligand and NCS  −  as anion. Red crystals and blue crystals were obtained. Powder X-ray diffraction patterns showed that the former is in 2D interpenetrated structure, while the latter has the same structure with Zn(NCS) 2 (bpp). Iron ion was introduced both into the red crystals and blue crystals of the mixed crystals of cobalt with zinc. 57 Fe Mössbauer spectrum of the red crystals showed a main doublet of Fe II high-spin state at 78 K, while the spectrum of blue crystals did not show Fe II high-spin state at 78 K.

Photonic crystals, light manipulation, and imaging in complex nematic structures

Science.gov (United States)

Ravnik, Miha; Å timulak, Mitja; Mur, Urban; Čančula, Miha; Čopar, Simon; Žumer, Slobodan

2016-03-01

Three selected approaches for manipulation of light by complex nematic colloidal and non-colloidal structures are presented using different own custom developed theoretical and modelling approaches. Photonic crystals bands of distorted cholesteric liquid crystal helix and of nematic colloidal opals are presented, also revealing distinct photonic modes and density of states. Light propagation along half-integer nematic disclinations is shown with changes in the light polarization of various winding numbers. As third, simulated light transmission polarization micrographs of nematic torons are shown, offering a new insight into the complex structure characterization. Finally, this work is a contribution towards using complex soft matter in optics and photonics for advanced light manipulation.

Domain Structures in Nematic Liquid Crystals on a Polycarbonate Surface

Directory of Open Access Journals (Sweden)

Vasily F. Shabanov

2013-08-01

Full Text Available Alignment of nematic liquid crystals on polycarbonate films obtained with the use of solvents with different solvations is studied. Domain structures occurring during the growth on the polymer surface against the background of the initial thread-like or schlieren texture are demonstrated. It is established by optical methods that the domains are stable formations visualizing the polymer surface structures. In nematic droplets, the temperature-induced transition from the domain structure with two extinction bands to the structure with four bands is observed. This transition is shown to be caused by reorientation of the nematic director in the liquid crystal volume from the planar alignment to the homeotropic state with the pronounced radial configuration of nematic molecules on the surface. The observed textures are compared with different combinations of the volume LC orientations and the radial distribution of the director field and the disclination lines at the polycarbonate surface.

The crystal structure of tris(thenoyltrifluoroacetonato)bis(triphenylphosphine oxide)neodymium(III)

International Nuclear Information System (INIS)

Leipoldt, J.G.; Bok, L.D.C.; Laubscher, A.E.; Basson, S.S.

1975-01-01

The crystal structure of tris(thenoyltrifluoroacetonato)bis= x (triphenylphosphine oxide)neodymium(III), (Nd(TTa) 3 .2TPPO), has been determined by single crystal X-ray diffraction. A total number of 5505 independent reflections was used for the structure determination. The complex crystallized in the triclinic space group P 1 - with two molecules in the unit cell. The cell dimensions are a = 23.64 A, b Z= 12.15 A, C 11.19 A, α = 109.4 0 , β = 104.2 0 , γ = 90.8 0 . The final calculated R vale is 8.4%. The molecule is monomeric and the neodymium atom is coordinated to eight oxygen atoms (six from the three thenoyltrifluoroacetone groups and two from the two triphenylphosphine groups) which form a dodecahedron. The average neodymium-oxygen bond length is 2.44 A. (author)

The effect of exchange-correlation on change and stability of crystal structure

International Nuclear Information System (INIS)

Yazdani, A.; Niazi, M.; Alimardan, V.

2007-01-01

Since exchange interaction energy has effect on band structure via polarization of spin of free electron, then can directly effects formation crystal structure. Therefore exchange-correlation is able to have an effect on determination of crystal structure or its change and stability. This energy is subject to fluctuation range of electrons between conduction band and valance band or density of electrons which due to increase the entropy of system, via Gibss Energy .We investigated these factors: 1) Size of ions 2) Density of States 3) Range of inter atomic and pair-potential.

Crystal structure of the Al2CuIr phase

International Nuclear Information System (INIS)

Meshi, L.; Ezersky, V.; Kapush, D.; Grushko, B.

2010-01-01

A new ternary Al 2 CuIr phase was revealed in the Al-Cu-Ir system. It is formed below 1063 o C from the β-phase (CsCl-type structure) extending at elevated temperatures from AlIr. The crystal structure of the Al 2 CuIr phase was determined using a combination of precession electron diffraction and X-ray powder diffraction techniques. The phase has an orthorhombic C-centered unit cell with lattice parameters a = 8.1196(7) A, b = 5.0646(2) A and c = 5.18513(3) A; its crystal symmetry can be described by the Cmme (no. 67) space group (Pearson symbol oC16). The unit cell of the new phase contains 8 Al, 4 Cu and 4 Ir atoms and exhibits a new structure type. The reliability factors characterizing the Rietveld refinement procedure are: R p = 4.45%, R wp = 6.45%, R B = 3.69% and R f = 2.41%.

Convenient synthesis of bis(alkoxy)rhenium(VII) complexes

Energy Technology Data Exchange (ETDEWEB)

Zhu, Z.; Al-Ajlouni, A.M.; Espenson, J.H. [Iowa State Univ., Ames, IA (United States)

1996-02-28

The study of high-oxidation-state organorhenium compounds has been a field of continuing activity, thanks to the success of methylrhenium trioxide (CH{sub 3}ReO{sub 3} or MTO) in catalytic processes. This catalyst is effective in oxidations, olefin metathesis, the olefination of aldehydes, and the preparation of other compounds with three-membered rings. The syntheses of some rhenium compounds derived form MTO have been reported. Epoxide formation is a key reaction, and it bears directly on these findings reported here. Re(VII) complexes containing a chelated bis(diolate) ligand can be synthesized by refluxing MTO with 2,3-dimethyl-2,3-diol. Here, the authors report a more convenient method for this preparation. A different series of related compounds consists of chelated bis(diolates) of the Cp*Re-oxo series, Cp*ReO-(diolate).

High-resolution metallic magnetic calorimeters for {beta}-spectroscopy on {sup 187}rhenium and position resolved X-ray spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Porst, Jan-Patrick

2011-02-01

This thesis describes the development of metallic magnetic calorimeters (MMCs) for high resolution spectroscopy. MMCs are energy dispersive particle detectors based on the calorimetric principle which are typically operated at temperatures below 100 mK. The detectors make use of a paramagnetic temperature sensor to transform the temperature rise upon the absorption of a particle in the detector into a measurable magnetic flux change in a dc-SQUID. The application of MMCs for neutrino mass measurements and their advantages with respect to other approaches are discussed. In view of this application the development of an MMC optimized for {beta}-endpoint spectroscopy on {sup 187}rhenium is presented. A fully micro-fabricated X-ray detector is characterized and performs close to design values. Furthermore, a new technique to more efficiently couple rhenium absorbers mechanically and thermally to the sensor was developed and successfully tested. By employing a metallic contact, signal rise times faster than 5 {mu}s could be observed with superconducting rhenium absorbers. In addition to the single pixel detectors, an alternative approach of reading out multiple pixels was developed in this work, too. Here, the individual absorbers have a different thermal coupling to only one temperature sensor resulting in a distribution of different pulse shapes. Straightforward position discrimination by means of rise time analysis is demonstrated for a four pixel MMC and a thermal model of the detector is provided. Unprecedented so far, an energy resolution of less than {delta}E{sub FWHM}<5 eV for 5.9 keV X-rays was achieved across all absorbers. (orig.)

On the crystal structure of colloidally prepared CsPbBr3 quantum dots.

Science.gov (United States)

Cottingham, Patrick; Brutchey, Richard L

2016-04-18

Colloidally synthesized quantum dots of CsPbBr3 are highly promising for light-emitting applications. Previous reports based on benchtop diffraction conflict as to the crystal structure of CsPbBr3 quantum dots. We present X-ray diffraction and PDF analysis of X-ray total scattering data that indicate that the crystal structure is unequivocally orthorhombic (Pnma).

Synthesis and crystal structure of two lead (II) complexes with 1,10-phenanthroline ligand

International Nuclear Information System (INIS)

Olivera, Fiorella L.; Santillan, Guillermo A.

2012-01-01

Two coordination complexes have been synthesized by the reaction of lead nitrate (II) with 1,10-phenanthroline in methanol/water. The crystals of these complexes were obtained by using the diffusion method and structurally characterized by X-ray single crystal diffraction. Both complexes crystallized in the monoclinic space group P2 1 /c. The analysis by crystal X-ray diffraction reveals that in both complexes the coordination around the lead (II) ion is a distorted octahedral structure where the ion is bonded to the heterocyclic nitrogen atoms of chelating ligand 1,10-phenanthroline, three oxygen atoms of three nitrate groups and one oxygen from the water molecule. The difference between the complexes lies in the way of nitrate ion in presence of carboxylic acid aromatics. In addition, the crystal structure of complexes can be regarded as a 3D coordination polymer through Pb-O weak interactions, hydrogen bonds and π-π stacking interactions. (author).

Crystal structure of new AsS2 compound

International Nuclear Information System (INIS)