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Sample records for cryst liq cryst

  1. Comment on "Experimental study of the orientation dependence of indium incorporation in GaInN" [J. Cryst. Growth 433 (2016) 7-12

    Science.gov (United States)

    Monavarian, Morteza

    2016-07-01

    The authors of the title paper (J. Cryst. Growth 433 (2016) 7-12) reported on experimental comparison of indium incorporation efficiency in wide variety of orientations tilted from the basal plane toward a-plane (a-family planes) or m-plane (m-family planes) and some mixed planes. Despite a good investigation and useful information reported in this manuscript, some points of criticism, concerning the inclination angle calculations, optical characterizations of the layers, and the final conclusions are highlighted in this comment to consider.

  2. Seperation of CsCl from LiCl-CsCl molten salt by cold finger melt cryst allization

    Energy Technology Data Exchange (ETDEWEB)

    Versey, Joshua R. [Dept. of Chemical and Materials Engineering and Nuclear Engineering Program University of Idaho, Idaho (United States); Phongikaroon, Supathorn [Dept. of Mechanical and Nuclear Engineering Virginia Commonwealth University, Richmond (Korea, Republic of); Simpson, Michael F. [Dept. of Metallurgical Engineering University of Utah, Utah (Korea, Republic of)

    2014-06-15

    This study provides a fundamental understanding of a cold finger melt crystallization technique by exploring the heat and mass transfer processes of cold finger separation. A series of experiments were performed using a simplified LiCl-CsCl system by varying initial CsCl concentrations (1, 3, 5, and 7.5 wt%), cold finger cooling rates (7.4, 9.8, 12.3, and 14.9 L/min), and separation times (5, 10, 15, and 30 min). Results showed a potential recycling rate of 0.36 g/min with a purity of 0.33 wt% CsCl in LiCl. A CsCl concentrated drip formation was found to decrease crystal purity especially for smaller crystal formations. Dimensionless heat and mass transfer correlations showed that separation production is primarily influenced by convective transfer controlled by cooling gas flow rate, where correlations are more accurate for slower cooling gas flow rates.

  3. Two Beam Energy Exchange in Hybrid Liquid Crystal Cells with Photorefractive Field Controlled Boundary Conditions (Postprint)

    Science.gov (United States)

    2016-09-12

    axis modulation. © 2016 Author(s). All article content, except where otherwise noted, is licensed under a Creative Commons Attribution (CC BY) license...Miniewicz, Appl . Phys. Lett. 74, 2924 (1999). 6 S. Bartkiewicz, K. Matczyszyn, A. Miniewicz, and F. Kajzar, Opt. Commun. 187, 257 (2001). 7 G. P...1997). 9 H. Ono and N. Kawatsuki, J. Appl . Phys. 85, 2482 (1999). 10 G. Cook, J. L. Carns, M. A. Saleh, and D. R. Evans, Mol. Cryst. Liq. Cryst. 453

  4. The Ste locus, a component of the parasitic cry-Ste system of Drosophila melanogaster, encodes a protein that forms crystals in primary spermatocytes and mimics properties of the beta subunit of casein kinase 2

    DEFF Research Database (Denmark)

    Bozzetti, M P; Massari, S; Finelli, P

    1995-01-01

    Males of Drosophila melanogaster lacking the Y chromosome-linked crystal locus show multiple meiotic alterations including chromosome disorganization and prominent crystal formation in primary spermatocytes. These alterations are due to the derepression of the X chromosome-linked Stellate sequenc...

  5. 3,4,5-Tri-dodecyloxybenzoic acid: optimisation and scale-up of the synthesis

    NARCIS (Netherlands)

    Hersmis, M.C.; Spiering, A.J.H.; Waterval, R.J.M.; Meuldijk, J.; Vekemans, J.A.J.M.; Hulshof, L.A.

    2001-01-01

    The synthesis of tris-O-dodecyl-gallic acid [3,4,5-tris(dodecyloxy)benzoic acid] - a versatile building block for org. liq. cryst. materials - has been selected for fine chem. scale-up. A large-scale procedure of the alkylation of Me gallate with dodecyl bromide was optimized with exptl. design

  6. Liquid-crystalline side chain block copolymers - synthesis, morphology and LC behavior

    NARCIS (Netherlands)

    Arnold, M.; Poser, S.; Fischer, H.R.; Frank, W.; Utschick, H.

    1994-01-01

    Side-chain liq.-cryst. 2-hydroxyethyl methacrylate-styrene diblock copolymer (I) was prepd. by polymn. of 2-(trimethylsiloxy)ethyl methacrylate with styrene with further treatment with cholesteryl chloroformate. Morphol. and phase behavior of I were investigated. [on SciFinder (R)

  7. Structure/Property Relationships of Siloxane-Based Liquid Crystalline Materials

    Science.gov (United States)

    1992-05-01

    1974). (6) Goossens , N.J.,., Mol. Cryst. Liq. Cryst., 12,237-244(1971). (7) Gray, G.W. and Goodby, J.W.G., Smectic Liquid Crystals- Textures and...pp 30-105, (1989). 42 (59) Richards , R.D.C., Hawthorne, W.D., Hill, J.S., White, M.S., Lacey, D., Semlyen, J.A., Gray, G.W., and Kendrick, T.C., J...946(1985). (30) Davidson, P. and Levelut, A.M., J. Phys., 49, 689-695(1988). (31) Richards , R.D.C., Hawthorne, W.D., Hill, J.S., White, M.S., Lacey

  8. Bubble point pressures of the selected model system for CatLiq® bio-oil process

    DEFF Research Database (Denmark)

    Toor, Saqib Sohail; Rosendahl, Lasse; Baig, Muhammad Noman

    2010-01-01

    . In this work, the bubble point pressures of a selected model mixture (CO2 + H2O + Ethanol + Acetic acid + Octanoic acid) were measured to investigate the phase boundaries of the CatLiq® process. The bubble points were measured in the JEFRI-DBR high pressure PVT phase behavior system. The experimental results......The CatLiq® process is a second generation catalytic liquefaction process for the production of bio-oil from WDGS (Wet Distillers Grains with Solubles) at subcritical conditions (280-350 oC and 225-250 bar) in the presence of a homogeneous alkaline and a heterogeneous Zirconia catalyst...

  9. Environmental Management Plan for the Chemical Engineering Laboratory (LIQ) of the National University of Colombia, Bogotá

    OpenAIRE

    Javier Gama Chávez; Martha Lozano García; Paulo César Narváez Rincón; Óscar Javier Suárez Medina

    2004-01-01

    An Enviromental Management Plan was formulated with the objective of improving the environmental performance of the Chemical Engineering Laboratory (LIQ). The plan was supported on the principles established by the ISO 140001 standard. In a first step, an environmental politic was proposed. Next, by means of an initial review of the laboratory, the most significant impacts related to the activities developed in the Laboratory were identified: dangerous chemical wastes accumulation, water cont...

  10. Environmental Management Plan for the Chemical Engineering Laboratory (LIQ of the National University of Colombia, Bogotá

    Directory of Open Access Journals (Sweden)

    Javier Gama Chávez

    2004-01-01

    Full Text Available An Enviromental Management Plan was formulated with the objective of improving the environmental performance of the Chemical Engineering Laboratory (LIQ. The plan was supported on the principles established by the ISO 140001 standard. In a first step, an environmental politic was proposed. Next, by means of an initial review of the laboratory, the most significant impacts related to the activities developed in the Laboratory were identified: dangerous chemical wastes accumulation, water contamination by effusions generation and air contamination. These impacts were the base for formulating following and control programs, furthermire, a training an communication program was done. All the programs, including the requiered documents and procedures, were published in the Environmental Management Plan and the Environmental Procedures Manual.

  11. A Concise Li/liq. NH{sub 3} Mediated Synthesis of (4E,10Z)-Tetradeca-4,10-dienyl Acetate: The Major Sex Pheromone of Apple Leafminer Moth, Phyllonorycter ringoniella

    Energy Technology Data Exchange (ETDEWEB)

    Prem Kumar, B.; Vijaykumar, B. V. D.; Harshavardhan, S. J.; Jung, Haedong; Xie, Yongsheng; Shin, Dongsoo; Jang, Kiwan [Changwon National Univ., Changwon (Korea, Republic of); Lee, Dong Ha [Hanbat National Univ., Daejeon (Korea, Republic of); Yoon, Yongjin [Gyeongsang National Univ., Jinju (Korea, Republic of)

    2014-01-15

    We have accomplished a protection free, concise, Li/liq. NH3 mediated and gram scale synthesis of (4E,10Z)-tetradeca-4,10-dienyl acetate (1), the major sex pheromone of apple leafminer moth, Phyllonorycter ringoniella starting from commercially available 1-pentyne, 1,4- dibromobutane and 4-petyne-1-ol in 24% overall yield. The Li/liq. NH3 based mono-alkynylation of dibromobutane has been introduced for the first time. The stereoselective formation of 10(Z) and 4(E) olefins are accomplished by partial hydrogenation (Lindlar's catalyst) and birch reduction respectively. The economy, efficiency, simplicity and high stereo chemical purity of this synthesis allow the potential use of pheromone 1 in integrated field studies to understand the behavioral responses of male apple leaf miner moth.

  12. Director gliding in a nematic liquid crystal layer: Quantitative comparison with experiments

    Science.gov (United States)

    Mema, E.; Kondic, L.; Cummings, L. J.

    2018-03-01

    The interaction between nematic liquid crystals and polymer-coated substrates may lead to slow reorientation of the easy axis (so-called "director gliding") when a prolonged external field is applied. We consider the experimental evidence of zenithal gliding observed by Joly et al. [Phys. Rev. E 70, 050701 (2004), 10.1103/PhysRevE.70.050701] and Buluy et al. [J. Soc. Inf. Disp. 14, 603 (2006), 10.1889/1.2235686] as well as azimuthal gliding observed by S. Faetti and P. Marianelli [Liq. Cryst. 33, 327 (2006), 10.1080/02678290500512227], and we present a simple, physically motivated model that captures the slow dynamics of gliding, both in the presence of an electric field and after the electric field is turned off. We make a quantitative comparison of our model results and the experimental data and conclude that our model explains the gliding evolution very well.

  13. Advances in membrane protein crystallography: in situ and in meso data collection

    International Nuclear Information System (INIS)

    Weyand, Simone; Tate, Christopher G.

    2015-01-01

    Membrane protein structural biology has made tremendous advances over the last decade but there are still many challenges associated with crystallization, data collection and structure determination. Two independent groups, Axford et al. [(2015), Acta Cryst. D71, 1228–1237] and Huang et al. [(2015), Acta Cryst. D71, 1238–1256], have published methods that make a major contribution to addressing these challenges

  14. Advances in membrane protein crystallography: in situ and in meso data collection

    Energy Technology Data Exchange (ETDEWEB)

    Weyand, Simone, E-mail: sw644@cam.ac.uk [Department of Biochemistry, University of Cambridge, 80 Tennis Court Road, Cambridge CB2 1GA (United Kingdom); Tate, Christopher G., E-mail: sw644@cam.ac.uk [MRC Laboratory of Molecular Biology, Cambridge Biomedical Campus, Francis Crick Avenue, Cambridge CB2 0QH (United Kingdom)

    2015-05-23

    Membrane protein structural biology has made tremendous advances over the last decade but there are still many challenges associated with crystallization, data collection and structure determination. Two independent groups, Axford et al. [(2015), Acta Cryst. D71, 1228–1237] and Huang et al. [(2015), Acta Cryst. D71, 1238–1256], have published methods that make a major contribution to addressing these challenges.

  15. A facile synthesis of 1,2,3-triazolyl indole hybrids via SbCl3 ...

    Indian Academy of Sciences (India)

    Ponnuswamy A and Jagatheesan R 2011 Acta Cryst. E67 o2707. 27. Fun H K, Hemamalini M, Shanmugavelan P,. Ponnuswamy A and Jagatheesan R 2011 Acta Cryst. E67 o2776. 28. Sundberg R J 1996 The Chemistry of Indoles, New York: Academic Press 113. 29. (a) Saxton J E 1997 Nat. Prod. Rep. 14 559; (b) Toyota.

  16. Comparative Studies on Optical and Electronic Behavior of ...

    Indian Academy of Sciences (India)

    Prabu Mani

    2018-05-29

    May 29, 2018 ... And these dodecahedrons are connected through chelidamic acid ligand ... acid based lanthanide coordination polymers. ...... 3-carboxylate and oxalate ligands Dalton Trans. ... dicarboxylic acid and oxalic acid ligands Cryst.

  17. Nucleobase assemblies supported by uranyl cation coordination ...

    Indian Academy of Sciences (India)

    organic hybrid materials using smaller building blocks, which can be ..... nucleobase analogs, in addition to the presence of car- boxylate ... R 2004 Cryst. Eng. Comm. .... Sheldrick G M 2000 SADABS 2.0 (Germany: University of Göttingen). 76.

  18. The alignment of smectic A liquid crystals with director tilt on the boundaries

    International Nuclear Information System (INIS)

    Stewart, I W

    2007-01-01

    Equilibrium solutions are presented for smectic A liquid crystals in which the usual director n and unit layer normal a do not necessarily coincide. Previous applications often equate n with a; the model in this paper allows n and a to differ and has been motivated by the recent investigations of Auernhammer et al (2000 Rheol. Acta 39 215-22, 2002 Phys. Rev. E 66 061707), Soddemann et al (2004 Eur. Phys. J. E 13 141-51) and Stewart (2007 Contin. Mech. Thermodyn. 18 343-60). The two experimental geometries studied consist of planar homeotropically aligned smectic layers and 'bookshelf' aligned layers. In both cases a director tilt at the boundaries will be imposed. Solutions to the fully nonlinear bookshelf problem where both the director and the layer normal can vary with an element of decoupling are presented and are particularly relevant to the experimental observations of Elston (1994 Liq. Cryst. 16 151-7); there are two boundary layer effects, as will be discussed, that are related to the biasing of the director towards the smectic A phase and the reorientation of the smectic layers themselves

  19. The alignment of smectic A liquid crystals with director tilt on the boundaries

    Energy Technology Data Exchange (ETDEWEB)

    Stewart, I W [Department of Mathematics, University of Strathclyde, Livingstone Tower, 26 Richmond Street, Glasgow, G1 1XH (United Kingdom)

    2007-05-18

    Equilibrium solutions are presented for smectic A liquid crystals in which the usual director n and unit layer normal a do not necessarily coincide. Previous applications often equate n with a; the model in this paper allows n and a to differ and has been motivated by the recent investigations of Auernhammer et al (2000 Rheol. Acta 39 215-22, 2002 Phys. Rev. E 66 061707), Soddemann et al (2004 Eur. Phys. J. E 13 141-51) and Stewart (2007 Contin. Mech. Thermodyn. 18 343-60). The two experimental geometries studied consist of planar homeotropically aligned smectic layers and 'bookshelf' aligned layers. In both cases a director tilt at the boundaries will be imposed. Solutions to the fully nonlinear bookshelf problem where both the director and the layer normal can vary with an element of decoupling are presented and are particularly relevant to the experimental observations of Elston (1994 Liq. Cryst. 16 151-7); there are two boundary layer effects, as will be discussed, that are related to the biasing of the director towards the smectic A phase and the reorientation of the smectic layers themselves.

  20. Ericksen number and Deborah number cascade predictions of a model for liquid crystalline polymers for simple shear flow

    Science.gov (United States)

    Klein, D. Harley; Leal, L. Gary; García-Cervera, Carlos J.; Ceniceros, Hector D.

    2007-02-01

    We consider the behavior of the Doi-Marrucci-Greco (DMG) model for nematic liquid crystalline polymers in planar shear flow. We found the DMG model to exhibit dynamics in both qualitative and quantitative agreement with experimental observations reported by Larson and Mead [Liq. Cryst. 15, 151 (1993)] for the Ericksen number and Deborah number cascades. For increasing shear rates within the Ericksen number cascade, the DMG model displays three distinct regimes: stable simple shear, stable roll cells, and irregular structure accompanied by disclination formation. In accordance with experimental observations, the model predicts both ±1 and ±1/2 disclinations. Although ±1 defects form via the ridge-splitting mechanism first identified by Feng, Tao, and Leal [J. Fluid Mech. 449, 179 (2001)], a new mechanism is identified for the formation of ±1/2 defects. Within the Deborah number cascade, with increasing Deborah number, the DMG model exhibits a streamwise banded texture, in the absence of disclinations and roll cells, followed by a monodomain wherein the mean orientation lies within the shear plane throughout the domain.

  1. Characterization and H2-O2 reactivity of noble nano-metal tailored single wall nano-carbons

    International Nuclear Information System (INIS)

    K Kaneko; T Itoh; E Bekyarova; H Kanoh; S Utsumi; H Tanaka; M Yudasaka; S Iijima; S Iijima

    2005-01-01

    Phys. Chem.B. 108 17775, 2004. [5] H. Tanaka et al, Mol. Cryst. Liq. Cryst. 388, 429, 2002. [6] E. Bekyarova, et al, J. Phys. Chem. 107, 1468, 2003. [7] K. Murata et al., J. Phys. Chem. 106, 12668, 2002. [8] J. Phys. Chem. 106, 11132-11138 (20002). [9] H. Tanaka, et al, J. Amer. Chem.Soc. in press. [10] H. Tanaka et al. J. Phys. Chem. In press. [11] E. Bekyarova et al. J. Phys. Chem. In press

  2. Piezoelectric and Electrostrictive Materials for Transducer Applications. Volume 2.

    Science.gov (United States)

    1988-03-01

    Dariington, J. Appi. Phys. 43, 4951 (1972).I 17Z. Ujina and J. Handerek, Acta Physica Polonica A53, 665 (1978). 18Z. Q. Zhuang, M. J. Haun, S. J...Solution System. Part V: Theoretical Calculations." J. Appi. Phys. (submritted). 5 A. M. Glazer, S. A. Mabud, and R. Clarke, Acta Cryst. B34, 1060 (1978...Clarke, Acta Cryst.. B34, 1060 (1978). 12A. Amrin. R. E. Newham, and L. E. Cross, J. Solid State Chemissry 37, 248 (198 1). 13 M. j. Haun, E

  3. Definite existence of subphases with eight- and ten-layer unit cells as studied by complementary methods, electric-field-induced birefringence and microbeam resonant x-ray scattering.

    Science.gov (United States)

    Feng, Zhengyu; Chandani Perera, A D L; Fukuda, Atsuo; Vij, Jagdish K; Ishikawa, Ken; Iida, Atsuo; Takanishi, Yoichi

    2017-07-01

    A mixture of two selenium-containing compounds, 80 wt. % AS657 and 20 wt. % AS620, are studied with two complementary methods, electric-field-induced birefringence (EFIB) and microbeam resonant x-ray scattering (μRXS). The mixture shows the typical phase sequence of Sm-C_{A}^{*}-1/3-1/2-Sm-C^{*}-Sm-C_{α}^{*}-Sm-A, where 1/3 and 1/2 are two prototypal ferrielectric and antiferroelectric subphases with three- and four-layer unit cells, respectively. Here we designate the subphase as its q_{T} number defined by the ratio of [F]/([F]+[A]), where [F] and [A] are the numbers of synclinic ferroelectric and anticlinic antiferroelectric orderings in the unit cell, respectively. The electric field vs temperature phase diagram with EFIB contours indicates the emergence of three additional subphases, an antiferroelectric one between Sm-C_{A}^{*} and 1/3 and antiferroelectric and apparently ferrielectric ones between 1/3 and 1/2. The simplest probable q_{T}'s for these additional subphases are 1/4, 2/5, and 3/7, respectively, in the order of increasing temperature. The μRXS profiles indicate that antiferroelectric 1/4 and 2/5 approximately have the eight-layer (FAAAFAAA) and ten-layer (FAFAAFAFAA) Ising unit cells, respectively. The remaining subphase may be ferrielectric 3/7 with a seven-layer unit cell, although the evidence is partial. These experimental results are compared with the phenomenological Landau model [P. V. Dolganov and E. I. Kats, Liq. Cryst. Rev. 1, 127 (2014)2168-039610.1080/21680396.2013.869667] and the quasimolecular model [A. V. Emelyanenko and M. A. Osipov, Phys. Rev. E 68, 051703 (2003)1063-651X10.1103/PhysRevE.68.051703].

  4. Systematic Modelling and Crystal Size Distribution Control for Batch Crystallization Processes

    DEFF Research Database (Denmark)

    Abdul Samad, Noor Asma Fazli; Singh, Ravendra; Sin, Gürkan

    Crystallization processes form an important class of separation methods that are frequently used in the chemical, the pharmaceutical and the food industry. The specifications of the crystal product are usually given in terms of crystal size, shape and purity. In order to predict the desired cryst...

  5. Integration of Generic Multi-dimensional Model and Operational Policies for Batch Cooling Crystallization

    DEFF Research Database (Denmark)

    Abdul Samad, Noor Asma Fazli; Singh, Ravendra; Sin, Gürkan

    2011-01-01

    Crystallization processes form an important class of separation methods that are frequently used in the chemical, the pharmaceutical and the food industry. The specifications of the crystal product are usually given in terms of crystal size, shape and purity. In order to predict the desired cryst...

  6. Recent studies of point defects by Huang scattering of x rays

    International Nuclear Information System (INIS)

    Maeta, Hiroshi

    1977-01-01

    Huang scattering allows the measurements of the symmetry and strength of point defects produced by irradiations and constitutes a very sensitive method for observing the clustering that occurs during irradiations or annealings. In the present review, the principles and characteristics of the Huang scattering and recent investigations using this technique are described. [J.Cryst.Soc.Japan 19,231(1977)] (auth.)

  7. Introduction of an electron push-pull system yields a planar Red ...

    Indian Academy of Sciences (India)

    form a one-dimensional chain-like structure (figure S2). Molecule III crystallized in a ... value for the laplacian22 ( ρbcp) supports a closed shell. C=O...π interaction .... Nishio M, Umezawa Y, Honda K, Tsuboyama S and. Suezawa H 2009 Cryst ...

  8. Role of Steric Hindrance in the Crystal Packing of Z′ = 4 Superstructure of Trimethyltin Hydroxide

    KAUST Repository

    Dey, S.; Schö nleber, A.; Mondal, S.; Ali, S. I.; van Smaalen, S.

    2018-01-01

    The roomerature crystal structure of trimethyltin hydroxide, (CH)SnOH, has been described by Anderson et al. [Cryst. Growth Des. 2011, 11, 820-826] as a 2a × 2b × 8c, 32-fold superstructure. We report a a × b × 8c, eight-fold superstructure

  9. Influence of crystal–melt interface shape on self-seeding and single ...

    Indian Academy of Sciences (India)

    Unknown

    Self-seeding; orientation; interface shape; antimonide crystals; VDS technique. 1. Introduction ... fundamental characteristics of source materials, various crystal growth models ... to the temperature 50°C above the melting temperature of the crystals ..... Gadkari D B, Lal K B, Shah A P and Arora B M 1997 J. Cryst. Growth 173 ...

  10. Measurement of Refractive Indices of CdSiP2 at Temperatures from 90 to 450 K (Postprint)

    Science.gov (United States)

    2018-01-05

    Highway, Suite 1204, Arlington, VA 22202-4302. Respondents should be aware that notwithstanding any other provision of law, no person shall be subject...crystals,” J. Cryst. Growth 312(8), 1127–1132 (2010). 4. P. Brand , B. Boulanger, P. Segonds, V. Kemlin, P. G. Schunemann, K. T. Zawilski, B. Ménaert

  11. Significance of calculated cluster conformations of benzene: comment on a publication by D. E. Williams

    NARCIS (Netherlands)

    van de Waal, B.W.

    1981-01-01

    Results of potential-energy minimization, applied to clusters of benzene molecules, have been reported recently by Williams [Acta Cryst. (1980), A36, 715-723]. Two stable tridecamer clusters were found and compared with a 13-molecule fragment from crystalline orthorhombic benzene. In this comment

  12. Ab initio work function of elemental metals

    DEFF Research Database (Denmark)

    Skriver, Hans Lomholt; Rosengaard, N. M.

    1992-01-01

    We have used a recently developed self-consistent Green’s-function technique based on tight-binding linear-muffin-tin-orbital theory to calculate the work function for the close-packed surfaces of 37 elemental metals. The results agree with the limited experimental data obtained from single cryst...

  13. C9H14N

    Indian Academy of Sciences (India)

    J. Chem. Sci. Vol. 128, No. 7, July 2016, pp. 1037–1045. c Indian Academy of ..... Teraski O, Barry J C and Thomas J M 1987 Nature ... Betteridge P W, Carruthers J R, Cooper R I, Prout K and ... Clegg W and Watson D G 2007 Acta Cryst.

  14. Polynuclear and one-dimensional cyanide-bridged heterobimetallic ...

    Indian Academy of Sciences (India)

    JINGWEN SHI

    2018-02-07

    Feb 7, 2018 ... complexes: synthesis, crystal structures and magnetic properties. JINGWEN ... Introduction. In the recent past decades, many effective strategies have ..... organization of single molecule magnets on surfaces. Chem. Soc. Rev. ... Spin Crossover Coordination Polymer Cryst. Growth. Des. 17 2736. 17. Kaneko ...

  15. Structural study of nanosized yttrium-doped CaMnO3 perovskites

    Indian Academy of Sciences (India)

    Administrator

    Mater. 10 2461. Rodriguez-Carvajal J 1990 Collected abstract of powder di- ffraction meeting, Toulouse, p. 127. Shannon R D 1976 Acta Cryst. A32 751. Woodward P M, Vogt T, Cox D E, Arulraj A, Rao C N R,. Karen P and Cheetham A K 1998 Chem. Mater. 10 3652. Wunderlich F, Leisegang T and Weissbach T 2010 Phys.

  16. ORF Alignment: NC_000917 [GENIUS II[Archive

    Lifescience Database Archive (English)

    Full Text Available ... Template pdb|1SZ1|B Chain B, Mechanism Of Cca-Adding ... Enzymes Specificity Revealed By Cryst...al Structures Of ... Ternary Complexes pdb|1SZ1|A Chain A, Mechanism Of ... Cca-Adding Enzym...es Specificity Revealed By Crystal ... Structures Of Ternary Complexes pdb|1

  17. Dynamic quantum crystallography

    DEFF Research Database (Denmark)

    Hoser, Anna A.; Madsen, Anders Østergaard

    2017-01-01

    In the first paper of this series [Hoser & Madsen (2016). Acta Cryst. A72, 206-214], a new approach was introduced which enables the refinement of frequencies of normal modes obtained from ab initio periodic computations against single-crystal diffraction data. In this contribution, the performance...

  18. A third monoclinic polymorph of 3,4,5-trihydroxybenzoic acid monohydrate

    Directory of Open Access Journals (Sweden)

    Güneş Demirtaş

    2011-06-01

    Full Text Available The title compound, C7H6O5·H2O, is a new polymorph of the structures reported by Jiang et al. (2000 [Acta Cryst. C56, 594–595] and Okabe et al. (2001 [Acta Cryst. E57, o764–o766]. The gallic acid molecule is essentially planar (r.m.s. deviation = 0.550 Å. An intramolecular O—H...O hydrogen bond occurs in the gallic acid molecule, which is linked to the water molecule by a further O—H...O hydrogen bond. In the crystal, the components are linked by O—H...O hydrogen bonds. The hydrogen-bonding pattern differs from those reported for the previous polymorphs.

  19. A nanoscale characterisation of extended defects in glassy-like As2Se3 semiconductors with PAL technique

    International Nuclear Information System (INIS)

    Shpotyuk, O.; Kovalskiy, A.; Filipecki, J.; Hyla, M.; Kozdras, A.

    2003-01-01

    A meaningful interpretation of positron lifetime characteristics for glassy-like g-As 2 Se 3 is developed taking into account calculations of Jensen et al. (J. Non-Cryst. Solids 170 (1994) 57) for positrons trapped by free-volume extended defects in orthorhombic As 2 Se 3 and void volume distribution for 146-atoms layer-biased model of amorphous As 2 Se 3 presented by Popescu (J. Non-Cryst. Solids 35-36 (1980) 549). The obtained results are compared for samples having different thermal pre-history. Two groups of experimental results with close lifetime characteristics are distinguished for each of the investigated samples. This feature is explained in terms of average positron lifetime by applying two-state positron trapping model for mathematical treatment of the obtained spectra

  20. A nanoscale characterisation of extended defects in glassy-like As{sub 2}Se{sub 3} semiconductors with PAL technique

    Energy Technology Data Exchange (ETDEWEB)

    Shpotyuk, O.; Kovalskiy, A.; Filipecki, J.; Hyla, M.; Kozdras, A

    2003-12-31

    A meaningful interpretation of positron lifetime characteristics for glassy-like g-As{sub 2}Se{sub 3} is developed taking into account calculations of Jensen et al. (J. Non-Cryst. Solids 170 (1994) 57) for positrons trapped by free-volume extended defects in orthorhombic As{sub 2}Se{sub 3} and void volume distribution for 146-atoms layer-biased model of amorphous As{sub 2}Se{sub 3} presented by Popescu (J. Non-Cryst. Solids 35-36 (1980) 549). The obtained results are compared for samples having different thermal pre-history. Two groups of experimental results with close lifetime characteristics are distinguished for each of the investigated samples. This feature is explained in terms of average positron lifetime by applying two-state positron trapping model for mathematical treatment of the obtained spectra.

  1. Irreversible altering of crystalline phase of phase-change Ge-Sb thin films

    International Nuclear Information System (INIS)

    Krusin-Elbaum, L.; Shakhvorostov, D.; Cabral, C. Jr.; Raoux, S.; Jordan-Sweet, J. L.

    2010-01-01

    The stability of the crystalline phase of binary phase-change Ge x Sb 1-x films is investigated over a wide range of Ge content. From Raman spectroscopy we find the Ge-Sb crystalline structure irreversibly altered after exposure to a laser beam. We show that with increasing beam intensity/temperature Ge agglomerates and precipitates out in the amount growing with x. A simple empirical relation links Ge precipitation temperature T Ge p to the rate of change dT cryst /dx of crystallization, with the precipitation easiest on the mid-range x plateau, where T cryst is nearly constant. Our findings point to a preferable 15% < or approx. x < 50% window, that may achieve the desired cycling/archival properties of a phase-change cell.

  2. 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}.

  3. 2-Vinylpyridine–tris(pentafluorophenylborane hexane monosolvate

    Directory of Open Access Journals (Sweden)

    Marcus Klahn

    2012-04-01

    Full Text Available The title compound, C7H7N·B(C6F53·C6H14, was obtained by the stoichiometric reaction of 2-vinylpyridine and tris(pentafluorophenylborane in toluene. The formed adduct exhibits a restricted rotation along the B—N bond resulting in an asymmetry, which can be also observed in the 19F NMR spectra. The B—N distance is equivalent to the distances found for 2-methylpyridine and 2-ethylpyridine B(C6F53 adducts. For the final refinement, the contributions of disordered solvent molecules were removed from the diffraction data with SQUEEZE in PLATON [van der Sluis & Spek (1990. Acta Cryst. A46, 194–201; Spek (2009. Acta Cryst. D65, 148–155].

  4. Crystallographic data processing for free-electron laser sources

    International Nuclear Information System (INIS)

    White, Thomas A.; Barty, Anton; Stellato, Francesco; Holton, James M.; Kirian, Richard A.; Zatsepin, Nadia A.; Chapman, Henry N.

    2013-01-01

    A processing pipeline for diffraction data acquired using the ‘serial crystallography’ methodology with a free-electron laser source is described with reference to the crystallographic analysis suite CrystFEL and the pre-processing program Cheetah. A processing pipeline for diffraction data acquired using the ‘serial crystallography’ methodology with a free-electron laser source is described with reference to the crystallographic analysis suite CrystFEL and the pre-processing program Cheetah. A detailed analysis of the nature and impact of indexing ambiguities is presented. Simulations of the Monte Carlo integration scheme, which accounts for the partially recorded nature of the diffraction intensities, are presented and show that the integration of partial reflections could be made to converge more quickly if the bandwidth of the X-rays were to be increased by a small amount or if a slight convergence angle were introduced into the incident beam

  5. Crystallographic data processing for free-electron laser sources

    Energy Technology Data Exchange (ETDEWEB)

    White, Thomas A., E-mail: taw@physics.org; Barty, Anton; Stellato, Francesco [DESY, Notkestrasse 85, 22607 Hamburg (Germany); Holton, James M. [University of California, San Francisco, CA 94158 (United States); Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Kirian, Richard A. [DESY, Notkestrasse 85, 22607 Hamburg (Germany); Arizona State University, Tempe, AZ 85287 (United States); Zatsepin, Nadia A. [Arizona State University, Tempe, AZ 85287 (United States); Chapman, Henry N. [DESY, Notkestrasse 85, 22607 Hamburg (Germany); University of Hamburg, Luruper Chaussee 149, 22761 Hamburg (Germany)

    2013-07-01

    A processing pipeline for diffraction data acquired using the ‘serial crystallography’ methodology with a free-electron laser source is described with reference to the crystallographic analysis suite CrystFEL and the pre-processing program Cheetah. A processing pipeline for diffraction data acquired using the ‘serial crystallography’ methodology with a free-electron laser source is described with reference to the crystallographic analysis suite CrystFEL and the pre-processing program Cheetah. A detailed analysis of the nature and impact of indexing ambiguities is presented. Simulations of the Monte Carlo integration scheme, which accounts for the partially recorded nature of the diffraction intensities, are presented and show that the integration of partial reflections could be made to converge more quickly if the bandwidth of the X-rays were to be increased by a small amount or if a slight convergence angle were introduced into the incident beam.

  6. Targeted Basic Studies of Ferroelectric and Ferroelastic Materials for Piezoelectric Transducer Applications.

    Science.gov (United States)

    1983-03-01

    Ann . Freq. Control Symp., Atlantic City, NJ, 110 (1979). 2.12 L. Bohaty and S. Haussühl, Acta Cryst. A33, 114 (1977). 2.13 B.J. Luymes, Ph.D. Thesis...Maas. (1967). 6. J. van Men Boomgaard, DJL Terrell , RJU. Bom sad HS JX Ciller, J. Mat. Set«, 1705(1974). 7. AJ4J.G. van Run. DJt. Terrell

  7. Skin permeability and pharmacokinetics of diclofenac epolamine administered by dermal patch in Yorkshire-Landrace pigs

    OpenAIRE

    Tse S; Powell KD; MacLennan SJ; Moorman AR; Paterson C; Bell RR

    2012-01-01

    Susanna Tse,1 Kendall D Powell,2 Stephen MacLennan,3 Allan R Moorman,4 Craig Paterson,5 Rosonald R Bell11Pfizer Inc, Groton, CT, USA; 2Tandem Labs, Durham, NC, USA; 3BioCryst Pharmaceuticals Inc, Durham, NC, USA; 4Alta Vetta Pharmaceutical Consulting LLC, Durham, NC, USA; 5Salix Pharmaceuticals Inc, Raleigh, NC, USAPurpose: This study compared the pharmacokinetic profile, and systemic and local absorption of diclofenac, following dermal patch application and oral administration in Yorkshire- ...

  8. mu-crystallin is a mammalian homologue of Agrobacterium ornithine cyclodeaminase and is expressed in human retina.

    OpenAIRE

    Kim, R Y; Gasser, R; Wistow, G J

    1992-01-01

    mu-Crystallin is the major component of the eye lens in several Australian marsupials. The complete sequence of kangaroo mu-crystallin has now been obtained by cDNA cloning. The predicted amino acid sequence shows similarity with ornithine cyclodeaminases encoded by the tumor-inducing (Ti) plasmids of Agrobacterium tumefaciens. Until now, neither ornithine cyclodeaminase nor any structurally related enzymes have been observed in eukaryotes. RNA analysis of kangaroo tissues shows that mu-cryst...

  9. Sm , Bi phosphors with high efficiency white-light-emittin

    Indian Academy of Sciences (India)

    2017-08-29

    Aug 29, 2017 ... Therefore, researches on high efficiency red phos- phors are very important. So far ..... ing concentration and reached a maximum at y = 8 mol%. A .... [10] Xue L P, Wang Y J, Lv P W, Chen D G, Lin Z, Liang J K et al. 2009 Crystal ... [28] Liu J, Xu B, Song C, Luo H, Zou X, Han L et al 2012 Cryst-. EngComm.

  10. Hydrothermal growth of ZnO nanoflowers and their photocatalyst ...

    Indian Academy of Sciences (India)

    JINCHENG FAN1,∗, TENGFEI LI1 and HANG HENG2,3. 1School of Materials ... In this paper, the fabrication of ZnO nanoflowers on Si substrate by the ..... [21] Bae J, Han J B, Zhang X-M, Wei M, Duan X, Zhang Y and. Wang Z L 2009 J. ... 142 570. [31] Sun Y J, Wang L, Yu X G and Chen K Z 2012 CrystEngComm. 14 3199.

  11. Analysis of Cl…Cl and C–H…Cl intermolecular interactions ...

    Indian Academy of Sciences (India)

    Administrator

    Rae A D and Desiraju G R 1993 J. Chem. Soc. Perkin. Trans. 2 2353. 7. Choudhury A R and Row T N G 2004 Cryst. Growth. Des. 4 47; Thalladi V R, Weiss H-C, Blдser D, Boese. R, Nangia A and Desiraju G R 1998 J. Am. Chem. Soc. 120 8702. 8. Chopra D, Cameron T S, Ferrara J D and Row T N G. 2006 J. Phys. Chem.

  12. Untitled

    Indian Academy of Sciences (India)

    3, Garrido, J. . . C.R. Acad. Sci., 1950, 230, 1878. 4. Guan Ya-Siyan, Simonov, Docklady Acad. Sci., USSR, 1963, 149, 146. V.I., and Belov, N. V.. 5. Hoppe, W. . . Acta Cryst., 1963, 16, 1056,. 6. Main, D. and Woolfson, Ibid., 1963, 16, 1046. : M. M.. 7. McLachlan, D. and Proc. Nat. Acad. Sei, USA, 1957, 37, 846,. Harker, D. 8.

  13. Structure of Hordeum vulgare NADPH-dependent thioredoxin reductase 2. Unwinding the reaction mechanism

    DEFF Research Database (Denmark)

    Kirkensgaard, Kristine Groth; Hägglund, Per; Finnie, Christine

    2009-01-01

    to the active form. Here, the first crystal structure of a cereal NTR, HvNTR2 from Hordeum vulgare (barley), is presented, which is also the first structure of a monocot plant NTR. The structure was determined at 2.6 A resolution and refined to an R (cryst) of 19.0% and an R (free) of 23.8%. The dimeric protein...

  14. Redetermination of 1,4-dimethoxybenzene

    OpenAIRE

    David M. Grant; Ronald J. Pugmire; James K. Harper; Atta M. Arif; Cody L. Hoop; Robbie Iuliucci

    2009-01-01

    The structure of the centrosymmetric title compound, C8H10O2, originally determined by Goodwin et al. [Acta Cryst.(1950), 3, 279–284], has been redetermined to modern standards of precision to aid in its use as a model compound for 13C chemical-shift tensor measurements in single-crystal NMR studies. In the crystal structure, a C—H...O interaction helps to establish the packing.

  15. HIGHLY ENERGY EFFICIENT D-GLU (DIRECTED-GREEN LIQ-UOR UTILIZATION) PULPING

    Energy Technology Data Exchange (ETDEWEB)

    Lucia, Lucian A

    2013-04-19

    Purpose: The purpose of the project was to retrofit the front end (pulp house) of a commercial kraft pulping mill to accommodate a mill green liquor (GL) impregna-tion/soak/exposure and accrue downstream physical and chemical benefits while prin-cipally reducing the energy footprint of the mill. A major player in the mill contrib-uting to excessive energy costs is the lime kiln. The project was intended to offload the energy (oil or natural gas) demands of the kiln by by-passing the causticization/slaking site in the recovery area and directly using green liquor as a pulping medium for wood. Scope: The project was run in two distinct, yet mutually compatible, phases: Phase 1 was the pre-commercial or laboratory phase in which NC State University and the Insti-tute of Paper Science and Technology (at the Georgia Institute of Technology) ran the pulping and associated experiments, while Phase 2 was the mill scale trial. The first tri-al was run at the now defunct Evergreen Pulp Mill in Samoa, CA and lead to a partial retrofit of the mill that was not completed because it went bankrupt and the work was no longer the low-hanging fruit on the tree for the new management. The second trial was run at the MeadWestvaco Pulp Mill in Evedale, TX which for all intents and pur-poses was a success. They were able to fully retrofit the mill, ran the trial, studied the pulp properties, and gave us conclusions.

  16. Density- and wavefunction-normalized Cartesian spherical harmonics for l ≤ 20.

    Science.gov (United States)

    Michael, J Robert; Volkov, Anatoliy

    2015-03-01

    The widely used pseudoatom formalism [Stewart (1976). Acta Cryst. A32, 565-574; Hansen & Coppens (1978). Acta Cryst. A34, 909-921] in experimental X-ray charge-density studies makes use of real spherical harmonics when describing the angular component of aspherical deformations of the atomic electron density in molecules and crystals. The analytical form of the density-normalized Cartesian spherical harmonic functions for up to l ≤ 7 and the corresponding normalization coefficients were reported previously by Paturle & Coppens [Acta Cryst. (1988), A44, 6-7]. It was shown that the analytical form for normalization coefficients is available primarily for l ≤ 4 [Hansen & Coppens, 1978; Paturle & Coppens, 1988; Coppens (1992). International Tables for Crystallography, Vol. B, Reciprocal space, 1st ed., edited by U. Shmueli, ch. 1.2. Dordrecht: Kluwer Academic Publishers; Coppens (1997). X-ray Charge Densities and Chemical Bonding. New York: Oxford University Press]. Only in very special cases it is possible to derive an analytical representation of the normalization coefficients for 4 4 the density normalization coefficients were calculated numerically to within seven significant figures. In this study we review the literature on the density-normalized spherical harmonics, clarify the existing notations, use the Paturle-Coppens (Paturle & Coppens, 1988) method in the Wolfram Mathematica software to derive the Cartesian spherical harmonics for l ≤ 20 and determine the density normalization coefficients to 35 significant figures, and computer-generate a Fortran90 code. The article primarily targets researchers who work in the field of experimental X-ray electron density, but may be of some use to all who are interested in Cartesian spherical harmonics.

  17. Fundamental Studies in the OM-CVD Growth of Ga-In-As-Sb.

    Science.gov (United States)

    1987-05-01

    greater than one ’T. Fukui and Y. Horkoshi. Jpn. 1. Appl. Phys. 19. L53 19801.tG. Nataf and C. Vene. J. Cryst. Growth 55. 87 11981.volt, the tunneling...350 *C. The BEP of In, Sb, and As was kept at ’T. Fukui and Y. Horikoshi, Jpn. J. Appl. Phys. 19, L53 (1980). 3 X 10’ , 3.1 X 10- 7, and 1.3 X 10...substrate and a Gas mask. Rat"" feedtM2, l The experimental setup is shown in Fig. 1. The rf heated td u susceptor is made of graphite coated with silicon

  18. Encyclopedia of Explosives and Related Items. Volume 9

    Science.gov (United States)

    1980-01-01

    NA), HNO. In the method used before WWII, NA was prepd Ammontol. A castable HE mixt of AN 50, by heating Na nitrate ( Chile saltpeter) with TNT 38...as an igniting charge in Pb Azide detonators Torpedos. Accdg to Gonzilez (Ref 11, p 76), torpedos can be used on land (tierra) or in water (en el agua ...sumergidos (Tetryl). Described in Ref 6, p 294; Ref 9, pp en agua ) after being waterproofed 21 & 139; and Ref 19, p 335. Lt-yel crysts; d 1.73g/cc

  19. Thermally induced nano-structural and optical changes of nc-Si:H deposited by hot-wire CVD

    CSIR Research Space (South Africa)

    Arendse, CJ

    2009-04-01

    Full Text Available 55 56 57 58 59 60 61 62 63 64 65 15 [26] D. Stryahilev, F. Diehl, B. Schroeder, J. Non-Cryst. Solids 266–269, 166 (2000) [27] M. H. Brodsky, M. Cardona, and J. J. Cuomo, Phys. Rev. B 16. 3556 (1977) [28] H. Shanks, C. J. Fang, L. Ley... stream_source_info Arendse_d1_2009.pdf.txt stream_content_type text/plain stream_size 28527 Content-Encoding UTF-8 stream_name Arendse_d1_2009.pdf.txt Content-Type text/plain; charset=UTF-8...

  20. Neutron time-of-flight techniques for investigation of the extinction effect

    International Nuclear Information System (INIS)

    Niimura, N.; Tomiyoshi, S.; Takahashi, J.; Harada, J.

    1975-01-01

    An application of the time-of-flight neutron diffraction technique to an investigation of the nature of the extinction effect in a single-crystal specimen is given. It is shown that the wavelength dependence of the extinction can be easily obtained by changing the scattering angle. An estimation of the extinction factor for a CuCl single crystal is given as an example and a comparison of the results with recent extinction theory [Becker and Coppens. Acta Cryst.(1974). A30, 129-147; 148-153] is made. (Auth.)

  1. Tetraammineplatinum(II dichloride ammonia tetrasolvate

    Directory of Open Access Journals (Sweden)

    Tobias Grassl

    2014-07-01

    Full Text Available The title compound, [Pt(NH34]Cl2·4NH3, was crystallized in liquid ammonia from the salt PtCl2. The platinum cation is coordinated by four ammonia molecules, forming a square-planar complex. The chloride anions are surrounded by nine ammonia molecules, either bound within the platinum complex or solvent molecules. The solvent ammonia molecules are packed in such a way that an extended network of N—H...N and N—H...Cl hydrogen bonds is formed. The structure is isotypic with [Pd(NH34]Cl2·4NH3 [Grassl & Korber (2014. Acta Cryst. E70, i32].

  2. Redetermination of 3-methylisoquinoline at 150 K

    Directory of Open Access Journals (Sweden)

    Andrew D. Bond

    2010-11-01

    Full Text Available The structure of the title compound, C19H9O, has been redetermined at 150 K. The redetermination is of significantly higher precision than a previous room-temperature structure [Ribar et al. (1974. Cryst. Struct. Commun. 3, 323–325]. The C—N bond lengths for this redetermination are much closer to those observed in comparable structures, and the orientation of the methyl group with respect to the isoquinoline plane is clarified. Intermolecular weak C—H...N contacts are present in the crystal.

  3. International Conference on Millimeter Wave and Far-Infrared Technology (1st) Held in Beijing, China, August 17-21, 1992

    Science.gov (United States)

    1993-03-01

    exist in this wavelength range. Reliable observations have to be performed from satellites, rockets, stratospheric balloon gondolas or aircraft . Far...tan6 SiO, aerogel Si0) glass 10" Sio, cryst Fig. 6 The ,phase portrait* of the paper 104 letter aR* registered by radiation 100 300 500 700 with A = i...5 num. v.GHz 4.7 Fig. S SBMM absorption of quartz in three different states - single crystal, glass and aerogel . S’ and absorptivity. The abrupt

  4. Accelerated Exploration of Multi-principal Element Alloys for Structural Applications (Postprint)

    Science.gov (United States)

    2015-04-27

    S. Ranganathan, High Entropy Alloys, Butterworth-Hei- nemann, London, UK, 2014. [6] B. Cantor , I.T.H. Chang, P. Knight, A.J.B. Vincent, Mater. Sci...Kristallogr.-Cryst. Mater. 230 (2015) 55–68. [14] B. Cantor , Entropy 16 (2014) 4749–4768. [15] O.N. Senkov, C. Woodward, D.B. Miracle, JOM. 66 (2014...2014) 1973–1983. [21] F. Otto, Y. Yang, H. Bei, E.P. George , Acta Mater. 61 (2013) 2628–2638. [22] K.Y. Tsai, M.H. Tsai, J.W. Yeh, Acta Mater. 61

  5. Bis{μ-cis-1,3-bis[(di-tert-butylphosphanyloxy]cyclohexane-κ2P:P′}bis[carbonylnickel(0] including an unknown solvent molecule

    Directory of Open Access Journals (Sweden)

    Klara J. Jonasson

    2014-05-01

    Full Text Available The title compound, [Ni2(C22H46P2O22(CO2], is located about a centre of inversion with the Ni0 atom within a distorted trigonal–planar geometry. The cyclohexyl rings are in the usual chair conformation with the 1,3-cis substituents equatorially oriented. No specific intermolecular interactions are noted in the crystal packing. A region of disordered electron density, most probably a disordered deuterobenzene solvent molecule, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Its formula mass and unit-cell characteristics were not taken into account during refinement.

  6. Abacavir methanol 2.5-solvate

    Directory of Open Access Journals (Sweden)

    Phuong-Truc T. Pham

    2009-08-01

    Full Text Available The structure of abacavir (systematic name: {(1S,4R-4-[2-amino-6-(cyclopropylamino-9H-purin-9-yl]cyclopent-2-en-1-yl}methanol, C14H18N6O·2.5CH3OH, consists of hydrogen-bonded ribbons which are further held together by additional hydrogen bonds involving the hydroxyl group and two N atoms on an adjacent purine. The asymmetric unit also contains 2.5 molecules of methanol solvate which were grossly disordered and were excluded using SQUEEZE subroutine in PLATON [Spek, (2009. Acta Cryst. D65, 148–155].

  7. Redetermination and absolute configuration of atalaphylline

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2010-02-01

    Full Text Available The title acridone alkaloid [systematic name: 1,3,5-trihydroxy-2,4-bis(3-methylbut-2-enylacridin-9(10H-one], C23H25NO4, has previously been reported as crystallizing in the chiral orthorhombic space group P212121 [Chantrapromma et al. (2010. Acta Cryst. E66, o81–o82] but the absolute configuration could not be determined from data collected with Mo radiation. The absolute configuration has now been determined by refinement of the Flack parameter with data collected using Cu radiation. All features of the molecule and its crystal packing are similar to those previously described.

  8. Redetermination of tetrakis(N,N-diethyldithiocarbamatotin(IV

    Directory of Open Access Journals (Sweden)

    Coco K. Y. A. Okio

    2009-06-01

    Full Text Available The crystal structure of the title compound, [Sn(C5H10NS24], was originally determined by Harreld & Schlemper [Acta Cryst. (1971, B27, 1964–1969] using intensity data estimated from Weissenberg films. In comparison with the previous refinement, the current redetermination reveals anisotropic displacement parameters for all non-H atoms, localization of the H atoms, and higher precision of lattice parameters and interatomic distances. The complex features a distorted S6 octahedral coordination geometry for tin and a cis disposition of the monodentate dithiocarbamate ligands.

  9. Redetermination of 1-naphthaleneacetic acid

    Directory of Open Access Journals (Sweden)

    Li-Jian Liu

    2008-12-01

    Full Text Available The crystal structure of the title compound, C12H10O2, was originally determined by Rajan [Acta Cryst. (1978. B34, 998–1000] using intensity data estimated from Weissenberg films. This redetermination provides a structure with significantly improved precision with respect to the geometric parameters. In the crystal structure, intermolecular O—H...O hydrogen bonds, weak C—H...O hydrogen bonds and C—H...π interactions link the molecules into a two-dimensional sheet lying parallel to (100.

  10. 1-[2,2-Bis(1,3-benzimidazol-1-ylmethyl-3-bromopropyl]-1,3-benzimidazole

    Directory of Open Access Journals (Sweden)

    Tai-Bao Wei

    2011-07-01

    Full Text Available The title compound, C26H23BrN6, has been synthesized as a potential ligand for the construction of metal–organic frameworks. The three benzimidazolyl groups present three potential coordination nodes. The dihedral angles between the benzimidazole ring systems are 74.03 (10, 66.49 (9 and 74.09 (9°. The structure contains large voids, which contain highly disordered solvent molecules that may be CH3CH2OH. Since the solvent molecules could not be located, the PLATON/SQUEEZE procedure [Spek (2009. Acta Cryst. D65, 148–155] was used.

  11. Structural basis for basal activity and autoactivation of abscisic acid (ABA) signaling SnRK2 kinases

    OpenAIRE

    Ng, Ley-Moy; Soon, Fen-Fen; Zhou, X. Edward; West, Graham M.; Kovach, Amanda; Suino-Powell, Kelly M.; Chalmers, Michael J.; Li, Jun; Yong, Eu-Leong; Zhu, Jian-Kang; Griffin, Patrick R.; Melcher, Karsten; Xu, H. Eric

    2011-01-01

    Abscisic acid (ABA) is an essential hormone that controls plant growth, development, and responses to abiotic stresses. Central for ABA signaling is the ABA-mediated autoactivation of three monomeric Snf1-related kinases (SnRK2.2, -2.3, and -2.6). In the absence of ABA, SnRK2s are kept in an inactive state by forming physical complexes with type 2C protein phosphatases (PP2Cs). Upon relief of this inhibition, SnRK2 kinases can autoactivate through unknown mechanisms. Here, we report the cryst...

  12. The XChemExplorer graphical workflow tool for routine or large-scale protein–ligand structure determination

    Science.gov (United States)

    Krojer, Tobias; Talon, Romain; Pearce, Nicholas; Douangamath, Alice; Brandao-Neto, Jose; Dias, Alexandre; Marsden, Brian

    2017-01-01

    XChemExplorer (XCE) is a data-management and workflow tool to support large-scale simultaneous analysis of protein–ligand complexes during structure-based ligand discovery (SBLD). The user interfaces of established crystallo­graphic software packages such as CCP4 [Winn et al. (2011 ▸), Acta Cryst. D67, 235–242] or PHENIX [Adams et al. (2010 ▸), Acta Cryst. D66, 213–221] have entrenched the paradigm that a ‘project’ is concerned with solving one structure. This does not hold for SBLD, where many almost identical structures need to be solved and analysed quickly in one batch of work. Functionality to track progress and annotate structures is essential. XCE provides an intuitive graphical user interface which guides the user from data processing, initial map calculation, ligand identification and refinement up until data dissemination. It provides multiple entry points depending on the need of each project, enables batch processing of multiple data sets and records metadata, progress and annotations in an SQLite database. XCE is freely available and works on any Linux and Mac OS X system, and the only dependency is to have the latest version of CCP4 installed. The design and usage of this tool are described here, and its usefulness is demonstrated in the context of fragment-screening campaigns at the Diamond Light Source. It is routinely used to analyse projects comprising 1000 data sets or more, and therefore scales well to even very large ligand-design projects. PMID:28291762

  13. The XChemExplorer graphical workflow tool for routine or large-scale protein-ligand structure determination.

    Science.gov (United States)

    Krojer, Tobias; Talon, Romain; Pearce, Nicholas; Collins, Patrick; Douangamath, Alice; Brandao-Neto, Jose; Dias, Alexandre; Marsden, Brian; von Delft, Frank

    2017-03-01

    XChemExplorer (XCE) is a data-management and workflow tool to support large-scale simultaneous analysis of protein-ligand complexes during structure-based ligand discovery (SBLD). The user interfaces of established crystallographic software packages such as CCP4 [Winn et al. (2011), Acta Cryst. D67, 235-242] or PHENIX [Adams et al. (2010), Acta Cryst. D66, 213-221] have entrenched the paradigm that a `project' is concerned with solving one structure. This does not hold for SBLD, where many almost identical structures need to be solved and analysed quickly in one batch of work. Functionality to track progress and annotate structures is essential. XCE provides an intuitive graphical user interface which guides the user from data processing, initial map calculation, ligand identification and refinement up until data dissemination. It provides multiple entry points depending on the need of each project, enables batch processing of multiple data sets and records metadata, progress and annotations in an SQLite database. XCE is freely available and works on any Linux and Mac OS X system, and the only dependency is to have the latest version of CCP4 installed. The design and usage of this tool are described here, and its usefulness is demonstrated in the context of fragment-screening campaigns at the Diamond Light Source. It is routinely used to analyse projects comprising 1000 data sets or more, and therefore scales well to even very large ligand-design projects.

  14. Effect of impurities and post-experimental purification in SAD phasing with serial femtosecond crystallography data.

    Science.gov (United States)

    Zhang, Tao; Gu, Yuanxin; Fan, Haifu

    2016-06-01

    In serial crystallography (SX) with either an X-ray free-electron laser (XFEL) or synchrotron radiation as the light source, huge numbers of micrometre-sized crystals are used in diffraction data collection. For a SAD experiment using a derivative with introduced heavy atoms, it is difficult to completely exclude crystals of the native protein from the sample. In this paper, simulations were performed to study how the inclusion of native crystals in the derivative sample could affect the result of SAD phasing and how the post-experimental purification proposed by Zhang et al. [(2015), Acta Cryst. D71, 2513-2518] could be used to remove the impurities. A gadolinium derivative of lysozyme and the corresponding native protein were used in the test. Serial femtosecond crystallography (SFX) diffraction snapshots were generated by CrystFEL. SHELXC/D, Phaser, DM, ARP/wARP and REFMAC were used for automatic structure solution. It is shown that a small amount of impurities (snapshots from native crystals) in the set of derivative snapshots can strongly affect the SAD phasing results. On the other hand, post-experimental purification can efficiently remove the impurities, leading to results similar to those from a pure sample.

  15. Geochemistry of radioactive elements in the process of weathering of carbonatites, acidic and alkali rocks

    International Nuclear Information System (INIS)

    Zhmodik, S.M.

    1984-01-01

    Geochemical peculiarities of uranium and thorium behaviour under formation of area crusts of weathering of granitoids, alkali rocks and carbonatites of certain areas of East Siberia are considered. The presented crysts of weathering have been formed under different climatic conditions, they have different age (in the limit of upper Cretaceous period - Neogene up to Quaternary time), chemical and mineral composition. Factors determining and controlling the level of uranium and thorium concentrations in weathering products are disclosed on the basis of facts using the methods of neutron-fragmentary radiography and by-fractional balances. Uranium and thorium distribution in granulometric fractions of crysts of weathering is considered in detail. Data on change in forms of radioactive elements under weathering, effect of fine-dispersed hypergene minerals (kaolinite, montmorillonite, goethite, etc.) on the character of uranium and thorium distribution in eluvial products as well as on sources of migrating uranium in crusts of weathering are presented. Scales of uranium and thorium redistribution under weathering are revealed. Supposition on the source of uranium and throium in sediments is made

  16. Crystal structure of a second triclinic polymorph of 2-methylpyridinium picrate

    Directory of Open Access Journals (Sweden)

    Jeganathan Gomathi

    2015-11-01

    Full Text Available The title molecular salt, C6H8N+·C6H2N3O7− (systematic name: 2-methylpyridinium 2,4,6-trinitrophenolate, crystallizes with two cations and two anions in the asymmetric unit. In the crystal, the cations are linked to the anions via bifurcated N—H...(O,O hydrogen bonds, generating R12(6 graph-set motifs. Numerous C—H...O hydrogen bonds are observed between these cation–anion pairs, which result in a three-dimensional network. In addition, weak aromatic π–π stacking between the 2-methylpyridinium rings [inter-centroid distance = 3.8334 (19 Å] and very weak stacking [inter-centroid distance = 4.0281 (16 Å] between inversion-related pairs of picrate anions is observed. The title salt is a second triclinic polymorph of the structure (also with Z′ = 2 reported earlier [Anita et al. (2006. Acta Cryst. C62, o567–o570; Chan et al. (2014. CrystEngComm, 16, 4508–4538]. In the title compound, the cations and anions display a chequerboard arrangement when viewed down [100], whereas in the first polymorph, (010 layers of alternating cations and anions are apparent in a [100] view. It is interesting that the unit-cell lengths are almost identical for the two polymorphs, although the inter-axial angles are quite different.

  17. 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

  18. Covariance and correlation estimation in electron-density maps.

    Science.gov (United States)

    Altomare, Angela; Cuocci, Corrado; Giacovazzo, Carmelo; Moliterni, Anna; Rizzi, Rosanna

    2012-03-01

    Quite recently two papers have been published [Giacovazzo & Mazzone (2011). Acta Cryst. A67, 210-218; Giacovazzo et al. (2011). Acta Cryst. A67, 368-382] which calculate the variance in any point of an electron-density map at any stage of the phasing process. The main aim of the papers was to associate a standard deviation to each pixel of the map, in order to obtain a better estimate of the map reliability. This paper deals with the covariance estimate between points of an electron-density map in any space group, centrosymmetric or non-centrosymmetric, no matter the correlation between the model and target structures. The aim is as follows: to verify if the electron density in one point of the map is amplified or depressed as an effect of the electron density in one or more other points of the map. High values of the covariances are usually connected with undesired features of the map. The phases are the primitive random variables of our probabilistic model; the covariance changes with the quality of the model and therefore with the quality of the phases. The conclusive formulas show that the covariance is also influenced by the Patterson map. Uncertainty on measurements may influence the covariance, particularly in the final stages of the structure refinement; a general formula is obtained taking into account both phase and measurement uncertainty, valid at any stage of the crystal structure solution.

  19. Possiblités de mesure quantitative avec un appareillage de réflectométrie X utilisant le mode angulaire dispersif

    Science.gov (United States)

    Chihab, J.; Naudon, A.

    1992-12-01

    A normalization procedure for reflectivity curves obtained with a new apparatus using the angle-resolved dispersive mode (J. Appl. Cryst., 1989) is described here. Simulation of spectra with the optical theory of X-rays is then possible. It allows to determine with a good accuracy the density, thickness and interfacial rugosities of layers when their thicknesses are less than about 200 nm. In order to check the normalization procedure a bulk silicon sample and a layer of evaporated nickel are analysed. Dans cet article nous présentons une procédure pour la normalisation des courbes de réflectivité obtenues par un nouvel appareillage de réflectométrie X utilisant le mode angulaire dispersif (J. Appl. Cryst., 1989). La simulation de ces courbes, dans le cadre de la théorie optique, devient alors possible. Pour les dépôts d'épaisseur inférieure à environ 200 nm, elle permet de déterminer précisément l'épaisseur, les rugosités interfaciales et la compacité. Afin de vérifier la validité de notre procédure de normalisation, nous analysons à titre d'exemples le cas d'un échantillon massif de silicium, et celui d'une couche mince de nickel évaporée sur un support en silicium.

  20. Interactive comparison and remediation of collections of macromolecular structures.

    Science.gov (United States)

    Moriarty, Nigel W; Liebschner, Dorothee; Klei, Herbert E; Echols, Nathaniel; Afonine, Pavel V; Headd, Jeffrey J; Poon, Billy K; Adams, Paul D

    2018-01-01

    Often similar structures need to be compared to reveal local differences throughout the entire model or between related copies within the model. Therefore, a program to compare multiple structures and enable correction any differences not supported by the density map was written within the Phenix framework (Adams et al., Acta Cryst 2010; D66:213-221). This program, called Structure Comparison, can also be used for structures with multiple copies of the same protein chain in the asymmetric unit, that is, as a result of non-crystallographic symmetry (NCS). Structure Comparison was designed to interface with Coot(Emsley et al., Acta Cryst 2010; D66:486-501) and PyMOL(DeLano, PyMOL 0.99; 2002) to facilitate comparison of large numbers of related structures. Structure Comparison analyzes collections of protein structures using several metrics, such as the rotamer conformation of equivalent residues, displays the results in tabular form and allows superimposed protein chains and density maps to be quickly inspected and edited (via the tools in Coot) for consistency, completeness and correctness. © 2017 The Protein Society.

  1. Symmetry of semi-reduced lattices.

    Science.gov (United States)

    Stróż, Kazimierz

    2015-05-01

    The main result of this work is extension of the famous characterization of Bravais lattices according to their metrical, algebraic and geometric properties onto a wide class of primitive lattices (including Buerger-reduced, nearly Buerger-reduced and a substantial part of Delaunay-reduced) related to low-restricted semi-reduced descriptions (s.r.d.'s). While the `geometric' operations in Bravais lattices map the basis vectors into themselves, the `arithmetic' operators in s.r.d. transform the basis vectors into cell vectors (basis vectors, face or space diagonals) and are represented by matrices from the set {\\bb V} of all 960 matrices with the determinant ±1 and elements {0, ±1} of the matrix powers. A lattice is in s.r.d. if the moduli of off-diagonal elements in both the metric tensors M and M(-1) are smaller than corresponding diagonal elements sharing the same column or row. Such lattices are split into 379 s.r.d. types relative to the arithmetic holohedries. Metrical criteria for each type do not need to be explicitly given but may be modelled as linear derivatives {\\bb M}(p,q,r), where {\\bb M} denotes the set of 39 highest-symmetry metric tensors, and p,q,r describe changes of appropriate interplanar distances. A sole filtering of {\\bb V} according to an experimental s.r.d. metric and subsequent geometric interpretation of the filtered matrices lead to mathematically stable and rich information on the Bravais-lattice symmetry and deviations from the exact symmetry. The emphasis on the crystallographic features of lattices was obtained by shifting the focus (i) from analysis of a lattice metric to analysis of symmetry matrices [Himes & Mighell (1987). Acta Cryst. A43, 375-384], (ii) from the isometric approach and invariant subspaces to the orthogonality concept {some ideas in Le Page [J. Appl. Cryst. (1982), 15, 255-259]} and splitting indices [Stróż (2011). Acta Cryst. A67, 421-429] and (iii) from fixed cell transformations to transformations

  2. Single-electron-capture processes in collisions of He2+, Liq+ (q=1,2,3), C6+, and O8+ ions with helium

    International Nuclear Information System (INIS)

    Samanta, R.; Purkait, M.; Mandal, C. R.

    2011-01-01

    Cross sections for single-electron capture in collisions of He 2+ , Li q+ (q = 1,2,3), C 6+ , and O 8+ ions with helium atoms at incident energy ranging from 50 to 5000 keV/amu have been calculated in the framework of four-body boundary-corrected continuum intermediate state (BCCIS-4B) approximation in both prior and post forms. In this formalism, distortion in the final channel related to the Coulomb continuum states of the projectile ion and the active electron in the field of residual target ion are included. In all cases, total single-electron-capture cross sections have been calculated by summing over all contributions up to n = 3 shells and subshells, respectively. It has been observed that the contribution of the capture cross section into the excited states is significant for asymmetric collision (Z P >Z T ) and is insignificant for symmetric collision. Numerical results for the total cross sections show good agreement with the available experimental findings, particularly in the post form. Post-prior discrepancy has been found to be within 30% except for Li + + He interactions below 150 keV/amu.

  3. EDM-DEDM and protein crystal structure solution.

    Science.gov (United States)

    Caliandro, Rocco; Carrozzini, Benedetta; Cascarano, Giovanni Luca; Giacovazzo, Carmelo; Mazzone, Anna Maria; Siliqi, Dritan

    2009-05-01

    Electron-density modification (EDM) procedures are the classical tool for driving model phases closer to those of the target structure. They are often combined with automated model-building programs to provide a correct protein model. The task is not always performed, mostly because of the large initial phase error. A recently proposed procedure combined EDM with DEDM (difference electron-density modification); the method was applied to the refinement of phases obtained by molecular replacement, ab initio or SAD phasing [Caliandro, Carrozzini, Cascarano, Giacovazzo, Mazzone & Siliqi (2009), Acta Cryst. D65, 249-256] and was more effective in improving phases than EDM alone. In this paper, a novel fully automated protocol for protein structure refinement based on the iterative application of automated model-building programs combined with the additional power derived from the EDM-DEDM algorithm is presented. The cyclic procedure was successfully tested on challenging cases for which all other approaches had failed.

  4. Computational and instrumental methods in EPR

    CERN Document Server

    Bender, Christopher J

    2006-01-01

    Computational and Instrumental Methods in EPR Prof. Bender, Fordham University Prof. Lawrence J. Berliner, University of Denver Electron magnetic resonance has been greatly facilitated by the introduction of advances in instrumentation and better computational tools, such as the increasingly widespread use of the density matrix formalism. This volume is devoted to both instrumentation and computation aspects of EPR, while addressing applications such as spin relaxation time measurements, the measurement of hyperfine interaction parameters, and the recovery of Mn(II) spin Hamiltonian parameters via spectral simulation. Key features: Microwave Amplitude Modulation Technique to Measure Spin-Lattice (T1) and Spin-Spin (T2) Relaxation Times Improvement in the Measurement of Spin-Lattice Relaxation Time in Electron Paramagnetic Resonance Quantitative Measurement of Magnetic Hyperfine Parameters and the Physical Organic Chemistry of Supramolecular Systems New Methods of Simulation of Mn(II) EPR Spectra: Single Cryst...

  5. Expanding the structural landscape of niclosamide: a high Z ' polymorph, two new solvates and monohydrate HA

    DEFF Research Database (Denmark)

    Sovago, Ioana; Bond, Andrew D.

    2015-01-01

    to be twinned by twofold rotation around that axis. The acetonitrile molecules occupy channels in the structure. A complete structure is provided for niclosamide monohydrate, C13H8Cl2N2O4·H2O, polymorph HA, obtained by Rietveld refinement against laboratory powder X-ray diffraction data. It has been suggested...... that this compound is related to the methanol solvate of niclosamide [Harriss, Wilson & Radosevljevic Evans (2014). Acta Cryst. C70, 758-763], but it is found that the two are not fully isostructural: they contain isostructural two-dimensional layers, but the layers are arranged differently in the two structures....... This suggests that HA may have the potential for polytypism, and features in the Rietveld difference curve indicate that a polytype fully isostructural with the methanol solvate might be present....

  6. Structural redetermination of the ThNi phase

    International Nuclear Information System (INIS)

    Fornasini, M.L.

    1983-01-01

    Msub(r) = 290.8, orthorhombic, Pnma, a = 14.146(6), b = 4.286(3), c = 5.702(3) A, V = 345.7 A 3 , Z = 8, Dsub(x) = 11.17 Mg m - 3 , F(000) = 944, room temperature, lambda (Mo Kα) = 0.71069 A, μ(Mo Kα) = 138 mm - 1 , final R = 0.049 for 306 observed reflections. Contrary to the report of Florio, Baenziger and Rundle [Acta Cryst. (1956), 9, 367-372], ThNi was found to crystallize in a stacking variant of the CrB-FeB types with trigonal-prismatic coordination of the Ni atoms, and recognized to be isotypic with the SrAg phase, having stacking code (hc) 2 . (Auth.)

  7. Entropic vs. elastic models of fragility of glass-forming liquids: Two sides of the same coin?

    Science.gov (United States)

    Sen, Sabyasachi

    2012-10-01

    The two most influential atomistic models that have been proposed in the literature to explain the temperature dependent activation energy of viscous flow of a glass-forming liquid, i.e., its fragility, are the configurational entropy model of Adam and Gibbs [J. Chem. Phys. 43, 139 (1965), 10.1063/1.1696442] and the elastic "shoving" model of Dyre et al. [J. Non-Cryst. Solids 352, 4635 (2006), 10.1016/j.jnoncrysol.2006.02.173]. Here we demonstrate a qualitative equivalence between these two models starting from the well-established general relationships between the interatomic potentials, elastic constants, structural rearrangement, and entropy in amorphous materials. The unification of these two models provides important predictions that are consistent with experimental observations and shed new light into the problem of glass transition.

  8. PCDDB: the Protein Circular Dichroism Data Bank, a repository for circular dichroism spectral and metadata.

    Science.gov (United States)

    Whitmore, Lee; Woollett, Benjamin; Miles, Andrew John; Klose, D P; Janes, Robert W; Wallace, B A

    2011-01-01

    The Protein Circular Dichroism Data Bank (PCDDB) is a public repository that archives and freely distributes circular dichroism (CD) and synchrotron radiation CD (SRCD) spectral data and their associated experimental metadata. All entries undergo validation and curation procedures to ensure completeness, consistency and quality of the data included. A web-based interface enables users to browse and query sample types, sample conditions, experimental parameters and provides spectra in both graphical display format and as downloadable text files. The entries are linked, when appropriate, to primary sequence (UniProt) and structural (PDB) databases, as well as to secondary databases such as the Enzyme Commission functional classification database and the CATH fold classification database, as well as to literature citations. The PCDDB is available at: http://pcddb.cryst.bbk.ac.uk.

  9. The protein circular dichroism data bank, a Web-based site for access to circular dichroism spectroscopic data.

    Science.gov (United States)

    Whitmore, Lee; Woollett, Benjamin; Miles, Andrew J; Janes, Robert W; Wallace, B A

    2010-10-13

    The Protein Circular Dichroism Data Bank (PCDDB) is a newly released resource for structural biology. It is a web-accessible (http://pcddb.cryst.bbk.ac.uk) data bank for circular dichroism (CD) and synchrotron radiation circular dichroism (SRCD) spectra and their associated experimental and secondary metadata, with links to protein sequence and structure data banks. It is designed to provide a public repository for CD spectroscopic data on macromolecules, to parallel the Protein Data Bank (PDB) for crystallographic, electron microscopic, and nuclear magnetic resonance spectroscopic data. Similarly to the PDB, it includes validation checking procedures to ensure good practice and the integrity of the deposited data. This paper reports on the first public release of the PCDDB, which provides access to spectral data that comprise standard reference datasets. Copyright © 2010 Elsevier Ltd. All rights reserved.

  10. Disorder effects in Mn(12)-acetate at 83 K.

    Science.gov (United States)

    Cornia, Andrea; Fabretti, Antonio Costantino; Sessoli, Roberta; Sorace, Lorenzo; Gatteschi, Dante; Barra, Anne-Laure; Daiguebonne, Carole; Roisnel, Thierry

    2002-07-01

    The structure of hexadeca-mu-acetato-tetraaquadodeca-mu(3)-oxo-dodecamanganese bis(acetic acid) tetrahydrate, [Mn(12)O(12)(CH(3)COO)(16)(H(2)O)(4)] x 2CH(3)COOH x 4H(2)O, known as Mn(12)-acetate, has been determined at 83 (2) K by X-ray diffraction methods. The fourfold (S(4)) molecular symmetry is disrupted by a strong hydrogen-bonding interaction with the disordered acetic acid molecule of solvation, which displaces one of the acetate ligands in the cluster. Up to six Mn(12) isomers are potentially present in the crystal lattice, which differ in the number and arrangement of hydrogen-bonded acetic acid molecules. These results considerably improve the structural information available on this molecular nanomagnet, which was first synthesized and characterized by Lis [Acta Cryst. (1980), B36, 2042-2046].

  11. Tetraamminepalladium(II dichloride ammonia tetrasolvate

    Directory of Open Access Journals (Sweden)

    Tobias Grassl

    2014-07-01

    Full Text Available The title compound, [Pd(NH34]Cl2·4NH3, was crystallized in liquid ammonia from the salt Pd(enCl2 (en is ethylenediamine and is isotypic with [Pt(NH34]Cl2·4NH3 [Grassl & Korber (2014. Acta Cryst. E70, i31]. The Pd2+ cation is coordinated by four ammonia molecules, exhibiting a square-planar geometry. The chloride anions are surrounded by nine ammonia molecules. These are either bound in the palladium complex or solvent molecules. The packing of the ammonia solvent molecules enables the formation of an extended network of N—H...N and N—H...Cl interactions with nearly ideal hydrogen-bonding geometry.

  12. Crystal structure of rubidium peroxide ammonia disolvate

    Directory of Open Access Journals (Sweden)

    Tobias Grassl

    2017-02-01

    Full Text Available The title compound, Rb2O2·2NH3, has been obtained as a reaction product of rubidium metal dissolved in liquid ammonia and glucuronic acid. As a result of the low-temperature crystallization, a disolvate was formed. To our knowledge, only one other solvate of an alkali metal peroxide is known: Na2O2·8H2O has been reported by Grehl et al. [Acta Cryst. (1995, C51, 1038–1040]. We determined the peroxide bond length to be 1.530 (11 Å, which is in accordance with the length reported by Bremm & Jansen [Z. Anorg. Allg. Chem. (1992, 610, 64–66]. One of the ammonia solvate molecules is disordered relative to a mirror plane, with 0.5 occupancy for the corresponding nitrogen atom.

  13. Holographic recording in thiophene-based polyester

    DEFF Research Database (Denmark)

    Matharu, Avtar Singh; Chambers-Asman, David; Jeeva, Shehzad

    2008-01-01

    The synthesis and optical data storage properties of a side-chain thiophene-phenyl azopolyester ThPhAzoP.ol is reported. The polyester is derived from diphenyl tetradecanedioate and a thiophenebased liquid crystalline diol which exhibits a short-lived enantiotropic SmA phase (Cryst 177.7 SmA 180.......4 I). The polyester ThPhAzoPol exhibits amorphous (Tg, 78.6 DC), crystalline and liquid crystalline character as evidenced by differential scanning calorimetry and thermal polarising microscopy. A grainy texture, which is thermally reversible, with increasing birefringence on cooling from...... the isotropic melt is observed. The polyester is amenable to optical data storage, showing efficient induced anisotropy, which is stable at room temperature. Polarisation gratings can be inscribed using orthogonally.linear and circularly polarised light to good effect (>10/0) and surface relief gratings...

  14. Potassium tetracyanidoaurate(III monohydrate: a redetermination

    Directory of Open Access Journals (Sweden)

    Nobuyuki Matsushita

    2017-03-01

    Full Text Available The structure of the title metal complex salt, K[Au(CN4]·H2O, has been redetermined using X-ray diffraction data at 173 K in order to improve the precision. The previous determination was based on neutron diffraction data [Bertinotti & Bertinotti (1970. Acta Cryst. B26, 422–428]. The title compound crystallizes in the space group P212121 with one potassium cation, one [Au(CN4]− anion and one water molecule in the asymmetric unit. The AuIII atom lies on a general position and has an almost square-planar coordination sphere defined by four cyanide ligands. Interactions between the potassium cation and N atoms of the complex anion, as well as O—H...N hydrogen bonds, lead to the formation of a three-dimensional framework structure.

  15. On the correlation between hydrogen bonding and melting points in the inositols

    DEFF Research Database (Denmark)

    Bekö, Sándor L; Alig, Edith; Schmidt, Martin U

    2014-01-01

    Inositol, 1,2,3,4,5,6-hexahydroxycyclohexane, exists in nine stereoisomers with different crystal structures and melting points. In a previous paper on the relationship between the melting points of the inositols and the hydrogen-bonding patterns in their crystal structures [Simperler et al. (2006...... ▶). CrystEngComm 8, 589], it was noted that although all inositol crystal structures known at that time contained 12 hydrogen bonds per molecule, their melting points span a large range of about 170 °C. Our preliminary investigations suggested that the highest melting point must be corrected for the effect...... ordered phases could be determined, of which seven were obtained from laboratory X-ray powder diffraction data. Five additional phases turned out to be rotator phases and only their unit cells could be determined. Two previously unknown melting points were measured, as well as most enthalpies of melting...

  16. Statistical mechanics and the physics of fluids

    CERN Document Server

    Tosi, Mario

    This volume collects the lecture notes of a course on statistical mechanics, held at Scuola Normale Superiore di Pisa for third-to-fifth year students in physics and chemistry. Three main themes are covered in the book. The first part gives a compact presentation of the foundations of statistical mechanics and their connections with thermodynamics. Applications to ideal gases of material particles and of excitation quanta are followed by a brief introduction to a real classical gas and to a weakly coupled classical plasma, and by a broad overview on the three states of matter.The second part is devoted to fluctuations around equilibrium and their correlations. Coverage of liquid structure and critical phenomena is followed by a discussion of irreversible processes as exemplified by diffusive motions and by the dynamics of density and heat fluctuations. Finally, the third part is an introduction to some advanced themes: supercooling and the glassy state, non-Newtonian fluids including polymers and liquid cryst...

  17. Crystal structures of 2,6-dibromo-4-methylbenzonitrile and 2,6-dibromo-4-methylphenyl isocyanide

    Directory of Open Access Journals (Sweden)

    Wayland E. Noland

    2017-12-01

    Full Text Available In the title crystals, C8H5Br2N, which are isomorphous, the steric bulk of the methyl group causes neighboring molecules to become mutually inclined. This prevents the formation of planar or nearly planar sheets, which were observed in the trichloro and tribromo analogs. Instead of CN/NC...Br contacts, tetrameric Br...Br contacts are observed. These contacts form tetragonally puckered sheets parallel to (001. The CN/NC and methyl groups are grouped at the peaks and troughs. Both molecules lie across crystallographic mirror planes; thus, the methyl H atoms are disordered over two sets of sites with equal occupancy. The title nitrile is a redetermination. The refinement converged at R[F2 > 2σ(F2] = 0.020, whereas the original determination [Gleason & Britton, (1976. Cryst. Struct. Commun. 5, 229–232] had R = 0.112.

  18. Chromium isotope fractionation during coprecipitation with calcium carbonate

    DEFF Research Database (Denmark)

    Rodler, Alexandra; Sánchez-Pastor, Nuria; Fernández-Díaz, Lurdes

    The chromium (Cr) isotopic composition of carbonates can potentially be used as a paleoclimate proxy to elucidate past fluctuations of oxygen contents in atmosphere and hydrosphere. The use of Cr isotopes to track paleoenvironmental changes, for example related to the rise of oxygen during the Ar...... et al., 2007, Water Air Soil Poll. 179, 381-390. [2] Sánchez-Pastor et al., 2011, Cryst. Growth Des. 11, 3081-3089.......The chromium (Cr) isotopic composition of carbonates can potentially be used as a paleoclimate proxy to elucidate past fluctuations of oxygen contents in atmosphere and hydrosphere. The use of Cr isotopes to track paleoenvironmental changes, for example related to the rise of oxygen during...... the Archaean and Protoerozoic, needs careful assessment of the signal robustness and necessitates a thorough understanding of the Cr cycle in Earth system processes. We conducted experiments testing the incorporation and isotopic fractionation of chromate into the calcite lattice. Our experiments indicate...

  19. Orthorhombic polymorph of 4-[(1H-benzimidazol-1-ylmethyl]benzoic acid

    Directory of Open Access Journals (Sweden)

    Hai-Wei Kuai

    2011-11-01

    Full Text Available We reported recently the first polymorph of the title compound [Kuai & Cheng (2011a. Acta Cryst., E67, o2787]. A second polymorph of the title compound, C15H12N2O2, was unexpectedly obtained by the hydrothermal reaction of the title compound with manganese chloride in the presence of potassium hydroxide at 413 K. The benzimidazole ring system is almost planar, with a maximum deviation from the mean plane of 0.015 (2 Å. The benzimidazole and benzene rings are inclined at a dihedral angle of 79.00 (1°. In the crystal, adjacent molecules are connected through O—H...N hydrogen bonds into a one-dimensional chain along the [001] direction.

  20. Differential thermal analysis of the glassy system AsSe-AsTe

    International Nuclear Information System (INIS)

    El Den, M.B.; El Mously, M.K.

    1986-11-01

    Thermal induced phase transformation for the system AsSe-AsTe has been studied using DTA. The dependence of the characteristic temperature Tg, Tc and Tm on the ratio of Se/Tc has been determined. The increase of Te content leads to the decrease of both Tg and Tc, i.e. tellurium enhances the crystallization process in these glasses exactly as in the case of AsSe 3/2-x Te x and AsSe 5/2-x Te x . The kinetic calculations have also been tried. Reasonable results have been obtained for two compositions only AsSe 0.5 Te 0.5 and AsSe 0.1 Te 0.9 with E cryst equal to 31.0 kcal/mole for the first and 45 and 65 kcal/mole for the second. The other compositions either do not crystallize completely or have complicated and overlapped peaks. (author)

  1. 4′,5-Dihydroxy-7-methoxyflavanone dihydrate

    Directory of Open Access Journals (Sweden)

    Iván Brito

    2012-01-01

    Full Text Available The title compound, C16H14O5·2H2O [systematic name: 5-hydroxy-2-(4-hydroxyphenyl-7-methoxychroman-4-one dihydrate], is a natural phytoalexin flavone isolated from the native chilean species Heliotropium taltalense and crystallizes with an organic molecule and two water molecules in the asymmetric unit. The 5-hydroxy group forms a strong intramolecular hydrogen bond with the carbonyl group, resulting in a six-membered ring. In the crystal, the components are linked by O—H...O hydrogen bonds, forming a three-dimensional network. The 4-hydroxyphenyl benzene ring is bonded equatorially to the pyrone ring, which adopts a slightly distorted sofa conformation. The title compound is the hydrated form of a previously reported structure [Shoja (1990. Acta Cryst. C46, 1969–1971]. There are only slight variations in the molecular geometry between the two compounds.

  2. Thermal diffuse scattering in angular-dispersive neutron diffraction

    International Nuclear Information System (INIS)

    Popa, N.C.; Willis, B.T.M.

    1998-01-01

    The theoretical treatment of one-phonon thermal diffuse scattering (TDS) in single-crystal neutron diffraction at fixed incident wavelength is reanalysed in the light of the analysis given by Popa and Willis [Acta Cryst. (1994), (1997)] for the time-of-flight method. Isotropic propagation of sound with different velocities for the longitudinal and transverse modes is assumed. As in time-of-flight diffraction, there exists, for certain scanning variables, a forbidden range in the one-phonon TDS of slower-than-sound neutrons, and this permits the determination of the sound velocity in the crystal. A fast algorithm is given for the TDS correction of neutron diffraction data collected at a fixed wavelength: this algorithm is similar to that reported earlier for the time-of-flight case. (orig.)

  3. 10,21-Dimethyl-2,7,13,18-tetraphenyl-3,6,14,17-tetraazatricyclo[17.3.1.18,12]tetracosa-1(23,2,6,8(24,9,11,13,17,19,21-decaene-23,24-diol cyclohexane 0.33-solvate

    Directory of Open Access Journals (Sweden)

    Sushil K. Gupta

    2011-10-01

    Full Text Available The title compound, C46H40N4O2·0.33C6H12, was obtained unintentionally as a product of an attempted synthesis of a cadmium(II complex of the [2,6-{PhSe(CH22N=CPh}2C6H2(4-Me(OH] ligand. The full tetraiminodiphenol macrocyclic ligand is generated by the application of an inversion centre. The macrocyclic ligand features strong intramolecular O—H...N hydrogen bonds. The dihedral angles formed between the phenyl ring incorporated within the macrocycle and the peripheral phenyl rings are 82.99 (8 and 88.20 (8°. The cyclohexane solvent molecule lies about a site of overline{3} symmetry. Other solvent within the lattice was disordered and was treated with the SQUEEZE routine [Spek (2009. Acta Cryst. D65, 148–155].

  4. Crystal structure of [(E-({2-[3-(2-{(1E-[(carbamothioylaminoimino]methyl}phenoxypropoxy]phenyl}methylideneamino]thiourea with an unknown solvate

    Directory of Open Access Journals (Sweden)

    Joel T. Mague

    2015-07-01

    Full Text Available The title molecule, C19H22N6O2S2, has crystallographically imposed C2 symmetry, with the central C atom lying on the rotation axis. The O—C—C—C torsion angle for the central chain is −59.22 (16° and the dihedral angle between the planes of the benzene rings is 75.20 (7°. In the crystal, N—H...O and N—H...S interactions link the molecules, forming a three-dimensional network encompassing channels running parallel to the c axis, which account for about 20% of the unit-cell volume. The contribution to the scattering from the highly disordered solvent molecules in these channels was removed with the SQUEEZE routine [Spek (2015. Acta Cryst. C71, 9–18] in PLATON. The stated crystal data for Mr, μ etc. do not take these into account.

  5. Trimesic acid dimethyl sulfoxide solvate: space group revision

    Directory of Open Access Journals (Sweden)

    Sylvain Bernès

    2008-07-01

    Full Text Available The structure of the title solvate, C9H6O6·C2H6OS, was determined 30 years ago [Herbstein, Kapon & Wasserman (1978. Acta Cryst. B34, 1613–1617], with data collected at room temperature, and refined in the space group P21. The present redetermination, based on high-resolution diffraction data, shows that the actual space group is more likely to be P21/m. The crystal structure contains layers of trimesic acid molecules lying on mirror planes. A mirror plane also passes through the S and O atoms of the solvent molecule. The molecules in each layer are interconnected through strong O—H...O hydrogen bonds, forming a two-dimensional supramolecular network within each layer. The donor groups are the hydroxyls of the trimesic acid molecules, while the acceptors are the carbonyl or the sulfoxide O atoms.

  6. 2-(5-Iodo-2-oxoindolin-3-ylidenehydrazinecarbothioamide including an unknown solvate

    Directory of Open Access Journals (Sweden)

    Viviane Conceição Duarte de Bittencourt

    2014-06-01

    Full Text Available The molecule of the title compound, C9H7IN4OS, is almost planar (r.m.s. deviation = 0.0373 Å. In the molecule, N—H...N and N—H...O hydrogen bonds generate, respectively, S(5 and S(6 ring motifs. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming chains propagating along [010]. These chains are linked via S...I contacts [3.4915 (16 Å], forming sheets lying parallel to (100. A region of disordered electron density, probably a disordered tetrahydrofuran solvent molecule, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. The formula mass and unit-cell characteristics were not taken into account during refinement.

  7. 5′′-(4-Nitrobenzylidene-7′-(4-nitrophenyl-1′′-methyl-1′,3′,5′,6′,7′,7a′-hexahydrodispiro[acenaphthylene-1,5′-pyrrolo[1,2-c][1,3]thiazole-6′,3′′-piperidine]-2,4′′(1H-dione including an unknown solvate

    Directory of Open Access Journals (Sweden)

    P. L. Nilantha Lakshman

    2013-08-01

    Full Text Available The title compound, C35H28N4O6S, crystallizes with two molecules in the asymmetric unit. In both molecules, the piperidine ring adopts a shallow-chair conformation, the thiazole ring adopts a twisted conformation about the Cm—N bond (m = methine and the pyrrole ring adopts an envelope conformation with the C atom shared with the thiazole ring as the flap. In the crystal, inversion dimers linked by pairs of C—H...O interactions generate R22(34 loops for one of the asymmetric molecules. Further C—H...O links also involving the other molecule lead to a three-dimesional network. The contribution of the highly disordered solvent to the scattering was removed with SQUEEZE option of PLATON [Spek (2009. Acta Cryst. D65, 148–155]. The solvent contribution is not included in the reported molecular weight and density.

  8. 1-Decyl-6-nitro-1H-benzimidazol-2(3H-one

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    Younes Ouzidan

    2011-11-01

    Full Text Available The title molecule, C17H25N3O3, is built up from fused six- and five-membered rings linked to a –C10H21 chain. The fused-ring system is essentially planar, the largest deviation from the mean plane being 0.009 (2 Å. The chain is roughly perpendicular to this plane, making a dihedral angle of 79.5 (2°. In the crystal, N—H...O hydrogen bonds build infinite chains along [010]. There are channels in the structure containing disordered hexane. The contribution of this solvent to the scattering power was suppressed using the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  9. 2-(2-Chlorophenyl-N-cyclohexyl-2-oxoacetamide

    Directory of Open Access Journals (Sweden)

    Xiu-Dan Jin

    2013-04-01

    Full Text Available In the title compound, C14H16ClNO2, the cyclohexyl ring has a chair conformation. The dihedral angle between the benzene ring and the mean plane of the four planar C atoms of the cyclohexyl ring is 45.2 (3°. The two carbonyl groups are trans to one another, with an O=C—C=O torsion angle of −137.1 (3°. In the crystal, molecules are linked by N—H...O hydrogen bonds forming chains propagating along [001]. A region of disordered electron density, situated near the unit-cell corners, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. It gave a solvent-accessible void of ca 400 Å3 for only 21 electrons. It is probably due to traces of the solvent of crystallization and was not taken into account during structure refinement.

  10. 3,10,14,21-Tetrakis(4-methoxyphenylpentacyclo[11.8.0.02,11.04,9.015,20]henicosa-1(21,2,4(9,5,7,10,13,15(20,16,18-decaen-12-one chloroform monosolvate

    Directory of Open Access Journals (Sweden)

    S. Gopinath

    2014-08-01

    Full Text Available The asymmetric unit of the title compound, C49H36O6·CHCl3, contains half an organic molecule, the complete molecule being generated by the operation of a crystallographic twofold rotation axis, and half a highly disordered chloroform molecule. The contribution to the diffraction pattern of the latter was removed using the program SQUEEZE in PLATON [Spek (2009. Acta Cryst. D65, 148–155]; the unit-cell characteristics take into account the presence of CHCl3. The dihedral angles between the planes of the naphthalene ring system and the methoxybenzene rings are 71.05 (7 (syn to the central C=O group and 57.27 (6° (anti to the central C=O group. In the crystal, molecules are linked by C—H...O interactions, generating C(12 chains running parallel to the b axis.

  11. 1,3,5-Tri-p-tolylpentane-1,5-diol

    Directory of Open Access Journals (Sweden)

    A. Thiruvalluvar

    2014-02-01

    Full Text Available In the title compound, C26H30O2, the central benzene ring forms dihedral angles of 14.85 (15 and 28.17 (14° with the terminal benzene rings. The dihedral angle between the terminal benzene rings is 32.14 (13°. The crystal packing exhibits two strong intermolecular O—H...O hydrogen bonds, forming directed four-membered co-operative rings. A region of disordered electron density, most probably disordered ethyl acetate solvent molecules, occupying voids of ca 519 Å3 for an electron count of 59, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Their formula mass and unit-cell characteristics were not taken into account during refinement. The structure was refined as an inversion twin [absolute structure parameter = −0.3 (4].

  12. Influence of Nd dopants on lattice parameters and thermal and elastic properties in YVO4 single crystals

    International Nuclear Information System (INIS)

    Kucytowski, J.; Wokulska, K.; Kazmierczak-Balata, A.; Bodzenta, J.; Lukasiewicz, T.; Hofman, B.; Pyka, M.

    2008-01-01

    The influence of neodymium doping on YVO 4 single crystals has been studied. The crystals were grown by the Czochralski method. One of them was pure YVO 4 and the others were doped with neodymium (YVO 4 :Nd) at various concentrations of Nd = 0.3-3.0 at.%. The changes of the lattice parameters were determined by the Bond's method [W.L. Bond, Acta Cryst. 13 (1960) 814]. The thermal diffusivity and the velocity of ultrasound using the photothermal method with mirage effect and the pulse echo method [J. Bodzenta, M. Pyka, J. Phys. IV France 137 (2006) 259] were measured. In the examined crystals, it was found that the lattice parameters increase while the thermal diffusivity decreases with increasing concentration of Nd atoms

  13. Redetermination of the borax structure from laboratory X-ray data at 145 K.

    Science.gov (United States)

    Gainsford, Graeme J; Kemmitt, Tim; Higham, Caleb

    2008-04-23

    THE TITLE COMPOUND, SODIUM TETRABORATE DECAHYDRATE (MINERAL NAME: borax), Na(2)[B(4)O(5)(OH)(4)]·8H(2)O, has been studied previously using X-ray [Morimoto (1956). Miner. J.2, 1-18] and neutron [Levy & Lisensky (1978). Acta Cryst. B34, 3502-3510] diffraction data. The structure contains tetra-borate anions [B(4)O(5)(OH)(4)](2-) with twofold rotation symmetry, which form hydrogen-bonded chains, and [Na(H(2)O)(6)] octa-hedra that form zigzag chains [Na(H(2)O)(4/2)(H(2)O)(2/1)]. The O-H bond distances obtained from the present redetermination at 145 K are shorter than those in the neutron study by an average of 0.127 (19) Å.

  14. Redetermination of the borax structure from laboratory X-ray data at 145 K

    Directory of Open Access Journals (Sweden)

    Caleb Higham

    2008-05-01

    Full Text Available The title compound, sodium tetraborate decahydrate (mineral name: borax, Na2[B4O5(OH4]·8H2O, has been studied previously using X-ray [Morimoto (1956. Miner. J. 2, 1–18] and neutron [Levy & Lisensky (1978. Acta Cryst. B34, 3502–3510] diffraction data. The structure contains tetraborate anions [B4O5(OH4]2− with twofold rotation symmetry, which form hydrogen-bonded chains, and [Na(H2O6] octahedra that form zigzag chains [Na(H2O4/2(H2O2/1]. The O—H bond distances obtained from the present redetermination at 145 K are shorter than those in the neutron study by an average of 0.127 (19 Å.

  15. ShelXle: a Qt graphical user interface for SHELXL.

    Science.gov (United States)

    Hübschle, Christian B; Sheldrick, George M; Dittrich, Birger

    2011-12-01

    ShelXle is a graphical user interface for SHELXL [Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122], currently the most widely used program for small-molecule structure refinement. It combines an editor with syntax highlighting for the SHELXL-associated .ins (input) and .res (output) files with an interactive graphical display for visualization of a three-dimensional structure including the electron density (F(o)) and difference density (F(o)-F(c)) maps. Special features of ShelXle include intuitive atom (re-)naming, a strongly coupled editor, structure visualization in various mono and stereo modes, and a novel way of displaying disorder extending over special positions. ShelXle is completely compatible with all features of SHELXL and is written entirely in C++ using the Qt4 and FFTW libraries. It is available at no cost for Windows, Linux and Mac-OS X and as source code.

  16. Diosgenin hemihydrate

    Directory of Open Access Journals (Sweden)

    María-Guadalupe Hernández Linares

    2012-08-01

    Full Text Available Diosgenin [or (22R,25R-spirost-5-en-3β-ol] is the starting material of the Marker degradation, a cheap semi-synthesis of progesterone, which has been designated as an International Historic Chemical Landmark. Thus far, a single X-ray structure for diosgenin is known, namely its dimethyl sulfoxide solvate [Zhang et al. (2005. Acta Cryst. E61, o2324–o2325]. We have now determined the structure of the hemihydrate, C27H42O3·0.5H2O. The asymmetric unit contains two diosgenin molecules, with quite similar conformations, and one water molecule. Hydroxy groups in steroids and water molecules form O—H...O hydrogen-bonded R54(10 ring motifs. Fused edge-sharing R(10 rings form a backbone oriented along [100], which aggregates the diosgenin molecules in the crystal structure.

  17. (η2,η2-Cycloocta-1,5-diene[2-(diphenylphosphanylmethylpyridine-κ2N,P]rhodium(I tetrafluoridoborate 1,2-dichloroethane monosolvate

    Directory of Open Access Journals (Sweden)

    Siping Wei

    2016-08-01

    Full Text Available The title compound, [Rh(C8H12(C18H16NP]BF4 has been prepared as a precatalyst for applications in rhodium-catalysed additions of carbocyclic acids to terminal alkynes leading to anti-Markovnikov Z-enol esters. Here the triclinic pseudopolymorph of the title compound is presented. In contrast to the earlier reported pseudopolymorph (orthorhombic space group [Wei et al. (2013. Chem. Eur. J. 19, 12067–12076], the triclinic polymorph contains half a molecule of dichloromethane as solvent in the asymmetric unit. The rhodium(I atom exhibits a square-planar coordination. The estimated diffraction contribution of the disordered solvent (a half molecule of dichloroethane per asymmetric unit was subtracted from the observed diffraction data using the SQUEEZE [Spek (2015. Acta Cryst. C71, 9–16] routine in PLATON. The given chemical formula and other crystal data do not take the solvent into account.

  18. Carbonyl{3,3′-di-tert-butyl-5,5′-dimethoxy-2,2′-bis[(4,4,5,5-tetramethyl-1,3,2-dioxaphospholan-2-yloxy]biphenyl-κ2P,P′}hydrido(triphenylphosphane-κPrhodium(I diethyl ether trisolvate

    Directory of Open Access Journals (Sweden)

    Detlef Selent

    2013-01-01

    Full Text Available In the title compound, [RhH(C74H68O8P2(C18H15P(CO]·3C4H10O, the CHP3 coordination set at the RhI ion is arranged in a distorted trigonal–bipyramidal geometry with the P atoms adopting equatorial coordination sites and the C atom of the carbonyl ligand as well as the H atom adopting the axial sites. The asymmetric unit contains two very similar molecules of the rhodium complex, two half-occupied diethyl ether molecules and further diethyl ether solvent molecules which could not be modelled successfully. Therefore contributions of the latter were removed from the diffraction data using the SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  19. A second monoclinic polymorph of 2-(3,5-dimethyl-1H-pyrazol-1-yl)-2-hy­droxy­imino-N′-[1-(pyridin-2-yl)ethyl­idene]acetohydrazide

    Science.gov (United States)

    Plutenko, Maxym O.; Lampeka, Rostislav D.; Haukka, Matti; Nordlander, Ebbe

    2013-01-01

    The title compound, C14H16N6O2, is a second monoclinic polymorph of 2-[1-(3,5-dimeth­yl)pyrazol­yl]-2-hy­droxy­imino-N′-[1-(2-pyrid­yl)ethyl­idene] acetohydrazide, with two crystallographically independent mol­ecules per asymmetric unit. The non-planar mol­ecules are chemically equal having similar geometric parameters. The previously reported polymorph [Plutenko et al. (2012 ▶). Acta Cryst. E68, o3281] was described in space group Cc (Z = 4). The oxime group and the O atom of the amide group are anti with respect to the C—C bond. In the crystal, mol­ecules are connected by N—H⋯N hydrogen bonds into zigzag chains extending along the b axis. PMID:23723911

  20. Study of viscosity of aluminum melt during glass transition by molecular dynamics and Green–Kubo formula

    International Nuclear Information System (INIS)

    Kirova, E M; Pisarev, V V

    2016-01-01

    Molecular dynamics study of shear viscosity behavior of liquid aluminum is performed. The embedded atom method potential is used at the simulation of isobaric cooling. The viscosity is calculated using the Green–Kubo formula. The stress autocorrelation functions are obtained in the range 300-1200 K. The calculated kinematic viscosity is in agreement with the experimental data for the temperatures above melting temperature. The steep change of the shear viscosity is found below 650 K which we associate with the glass transition and is in a good agreement with the temperature which is obtained using the calorimetric criterion Kolotova et al (2015 J. Non-Cryst. Solids 429 98). The viscosity coefficient can not be calculated using the direct atomistic simulations below that temperature. (paper)

  1. Estimated H-atom anisotropic displacement parameters: a comparison between different methods and with neutron diffraction results

    DEFF Research Database (Denmark)

    Munshi, Parthapratim; Madsen, Anders Ø; Spackman, Mark A

    2008-01-01

    systems and identify systematic discrepancies for several atom types. A revised and extended library of internal H-atom mean-square displacements is presented for use with Madsen's SHADE web server [J. Appl. Cryst. (2006), 39, 757-758; http://shade.ki.ku.dk], and the improvement over the original SHADE...... in the agreement with neutron results. The SHADE2 library, now incorporated in the SHADE web server, is recommended as a routine procedure for deriving estimates of H-atom ADPs suitable for use in charge-density studies on molecular crystals, and its widespread use should reveal remaining deficiencies and perhaps...... results is substantial, suggesting that this is now the most readily and widely applicable of the three approximate procedures. Using this new library--SHADE2--it is shown that, in line with expectations, a segmented rigid-body description of the heavy atoms yields only a small improvement...

  2. Solving crystal structures from powder data. I. The role of the prior information in the two-stage method

    International Nuclear Information System (INIS)

    Altomare, A.; Carrozzini, B.; Giacovazzo, C.; Guagliardi, A.; Moliterni, A.G.G.; Rizzi, R.

    1996-01-01

    For pt.II see ibid., p.674-81, 1996. The principal limitation of the diffraction methods for crystal structure analysis from powder data is originated by the collapse of the three-dimensional reciprocal space into the one dimension of the powder diffraction pattern. The degradation of the information can make difficult even the solution of small crystal structures and can generate inefficiencies in the least-squares methods devoted to crystal structure refinement. In this paper, the current two-stage procedures, the first stage dedicated to powder-pattern decomposition and the second to direct phasing of powder data, are analysed. It is shown that in the first stage such procedures disregard a large amount of information that can become available during the process of crystal structure solution and analysis. The use of such information is essential for making direct-methods procedures more robust and for improving the accuracy of the least-squares techniques. The performances of EXTRA [Altomare, Burla, Cascarano, Giacovazzo, Guagliardi, Moliterni and Polidori (1995). J. Appl. Cryst. 28, 842-846], a program for full-pattern decomposition based on the Le Bail algorithm, and of SIRPOW.92 [Altomare, Burla, Cascarano, Giacovazzo, Guagliardi, Polidori and Camalli (1994). J. Appl. Cryst. 27, 435-436], a direct-methods program optimized for powder data, are discussed in order to offer to the reader a logical pathway for the analysis of the traditional techniques and for the proposition of a new approach. It is shown that pattern-decomposition programs based on the Le Bail algorithm are able to exploit the prior information in a more effective way than Pawley-method-based decomposition programs. (orig.)

  3. Poly[μ2-chlorido-nonamethyl-μ3-nitrato-tritin(IV]. Corrigendum

    Directory of Open Access Journals (Sweden)

    Madeleine Helliwell

    2008-07-01

    Full Text Available An error in the original formulation of the title compound in the paper by Sadiq-ur-Rehman, Sherzaman, Ali, Shahzadi & Helliwell [Acta Cryst. (2007, E63, m2329] is corrected.The title compound in the paper by Sadiq-ur-Rehman, Sherzaman, Ali, Shahzadi & Helliwell [Acta Cryst. (2007, E63, m2329] was an unexpected product which seemed to have nitrate coordinated to three Sn atoms. However, it was noticed that the charges do not balance and that it is most likely that the nitrate is in fact a carbonate. Regrettably, there is no material to carry out microanalysis, but a plausible mechanism has been suggested to explain the unexpected formation of the product. Trimethyltin chloride will react with methanol in the presence of a base (4-hydroxypiperidine to give trimethyltin methoxide, which will rapidly hydrolyze in air to give the hydroxide. Both the methoxide and the hydroxide will react with atmospheric CO2 to give the carbonate (Bloodworth et al., 1967; Blunden et al., 1984; Sato, 1967. Me3SnCl + MeOH + base → Me3SnOMe + base·HCl Me3SnOMe + H2O → Me3SnOH + MeOH Me3SnOH + CO2 → Me3SnOCO2HMe3SnOCO2H + Me3SnOMe → Me3SnOCO2SnMe3 + MeOH. The carbonate then forms a coordination copolymer with trimethyltin chloride. The name of the title compound is corrected to poly[μ3-carbonato-μ3-chlorido-nonamethyltritin(IV], [Sn3(CH39(CO3Cl] (Mr = 586.84.

  4. Assessment of radiation damage behaviour in a large collection of empirically optimized datasets highlights the importance of unmeasured complicating effects

    International Nuclear Information System (INIS)

    Krojer, Tobias; Delft, Frank von

    2011-01-01

    A retrospective analysis of radiation damage behaviour in a statistically significant number of real-life datasets is presented, in order to gauge the importance of the complications not yet measured or rigorously evaluated in current experiments, and the challenges that remain before radiation damage can be considered a problem solved in practice. The radiation damage behaviour in 43 datasets of 34 different proteins collected over a year was examined, in order to gauge the reliability of decay metrics in practical situations, and to assess how these datasets, optimized only empirically for decay, would have benefited from the precise and automatic prediction of decay now possible with the programs RADDOSE [Murray, Garman & Ravelli (2004 ▶). J. Appl. Cryst.37, 513–522] and BEST [Bourenkov & Popov (2010 ▶). Acta Cryst. D66, 409–419]. The results indicate that in routine practice the diffraction experiment is not yet characterized well enough to support such precise predictions, as these depend fundamentally on three interrelated variables which cannot yet be determined robustly and practically: the flux density distribution of the beam; the exact crystal volume; the sensitivity of the crystal to dose. The former two are not satisfactorily approximated from typical beamline information such as nominal beam size and transmission, or two-dimensional images of the beam and crystal; the discrepancies are particularly marked when using microfocus beams (<20 µm). Empirically monitoring decay with the dataset scaling B factor (Bourenkov & Popov, 2010 ▶) appears more robust but is complicated by anisotropic and/or low-resolution diffraction. These observations serve to delineate the challenges, scientific and logistic, that remain to be addressed if tools for managing radiation damage in practical data collection are to be conveniently robust enough to be useful in real time

  5. Apocrustacyanin C(1) crystals grown in space and on earth using vapour-diffusion geometry: protein structure refinements and electron-density map comparisons.

    Science.gov (United States)

    Habash, Jarjis; Boggon, Titus J; Raftery, James; Chayen, Naomi E; Zagalsky, Peter F; Helliwell, John R

    2003-07-01

    Models of apocrustacyanin C(1) were refined against X-ray data recorded on Bending Magnet 14 at the ESRF to resolutions of 1.85 and 2 A from a space-grown and an earth-grown crystal, respectively, both using vapour-diffusion crystal-growth geometry. The space crystals were grown in the APCF on the NASA Space Shuttle. The microgravity crystal growth showed a cyclic nature attributed to Marangoni convection, thus reducing the benefits of the microgravity environment, as reported previously [Chayen et al. (1996), Q. Rev. Biophys. 29, 227-278]. A subsequent mosaicity evaluation, also reported previously, showed only a partial improvement in the space-grown crystals over the earth-grown crystals [Snell et al. (1997), Acta Cryst. D53, 231-239], contrary to the case for lysozyme crystals grown in space with liquid-liquid diffusion, i.e. without any major motion during growth [Snell et al. (1995), Acta Cryst. D52, 1099-1102]. In this paper, apocrustacyanin C(1) electron-density maps from the two refined models are now compared. It is concluded that the electron-density maps of the protein and the bound waters are found to be better overall for the structures of apocrustacyanin C(1) studied from the space-grown crystal compared with those from the earth-grown crystal, even though both crystals were grown using vapour-diffusion crystal-growth geometry. The improved residues are on the surface of the protein, with two involved in or nearby crystal lattice-forming interactions, thus linking an improved crystal-growth mechanism to the molecular level. The structural comparison procedures developed should themselves be valuable for evaluating crystal-growth procedures in the future.

  6. Bulk Crystal Growth, and High-Resolution X-ray Diffraction Results of LiZnAs Semiconductor Material

    Science.gov (United States)

    Montag, Benjamin W.; Reichenberger, Michael A.; Sunder, Madhana; Ugorowski, Philip B.; Nelson, Kyle A.; Henson, Luke C.; McGregor, Douglas S.

    2017-08-01

    LiZnAs is being explored as a candidate for solid-state neutron detectors. The compact form, solid-state device would have greater efficiency than present day gas-filled 3He and 10BF3 detectors. Devices fabricated from LiZnAs having either natural Li (nominally 7.5% 6Li) or enriched 6Li (usually 95% 6Li) as constituent atoms may provide a material for compact high efficiency neutron detectors. The 6Li( n, t)4He reaction yields a total Q-value of 4.78 MeV, an energy larger than that of the 10B reaction, which can easily be identified above background radiations. LiZnAs material was synthesized by preparing equimolar portions of Li, Zn, and As sealed under vacuum (10-6 Torr) in quartz ampoules lined with boron nitride and subsequently reacted in a compounding furnace (Montag et al. in J Cryst Growth 412:103, 2015). The raw synthesized LiZnAs was purified by a static vacuum sublimation in quartz (Montag et al. in J Cryst Growth 438:99, 2016). Bulk crystalline LiZnAs ingots were grown from the purified material with a high-temperature Bridgman-style growth process described here. One of the largest LiZnAs ingots harvested was 9.6 mm in diameter and 4.2 mm in length. Samples were harvested from the ingot and were characterized for crystallinity using a Bruker AXS Inc. D8 AXS Inc. D2 CRYSO, energy dispersive x-ray diffractometer, and a Bruker AXS Inc. D8 DISCOVER, high-resolution x-ray diffractometer equipped with molybdenum radiation, Gobel mirror, four bounce germanium monochromator and a scintillation detector. The primary beam divergence was determined to be 0.004°, using a single crystal Si standard. The x-ray based characterization revealed that the samples nucleated in the (110) direction and a high-resolution open detector rocking curve recorded on the (220) LiZnAs yielded a full width at half maximum (FWHM) of 0.235°. Sectional pole figures using off-axis reflections of the (211) LiZnAs confirmed in-plane ordering, and also indicated the presence of multiple

  7. The active site of hen egg-white lysozyme: flexibility and chemical bonding

    Energy Technology Data Exchange (ETDEWEB)

    Held, Jeanette, E-mail: jeanette.netzel@uni-bayreuth.de; Smaalen, Sander van [University of Bayreuth, D-95440 Bayreuth (Germany)

    2014-04-01

    Chemical bonding at the active site of lysozyme is analyzed on the basis of a multipole model employing transferable multipole parameters from a database. Large B factors at low temperatures reflect frozen-in disorder, but therefore prevent a meaningful free refinement of multipole parameters. Chemical bonding at the active site of hen egg-white lysozyme (HEWL) is analyzed on the basis of Bader’s quantum theory of atoms in molecules [QTAIM; Bader (1994 ▶), Atoms in Molecules: A Quantum Theory. Oxford University Press] applied to electron-density maps derived from a multipole model. The observation is made that the atomic displacement parameters (ADPs) of HEWL at a temperature of 100 K are larger than ADPs in crystals of small biological molecules at 298 K. This feature shows that the ADPs in the cold crystals of HEWL reflect frozen-in disorder rather than thermal vibrations of the atoms. Directly generalizing the results of multipole studies on small-molecule crystals, the important consequence for electron-density analysis of protein crystals is that multipole parameters cannot be independently varied in a meaningful way in structure refinements. Instead, a multipole model for HEWL has been developed by refinement of atomic coordinates and ADPs against the X-ray diffraction data of Wang and coworkers [Wang et al. (2007), Acta Cryst. D63, 1254–1268], while multipole parameters were fixed to the values for transferable multipole parameters from the ELMAM2 database [Domagala et al. (2012), Acta Cryst. A68, 337–351] . Static and dynamic electron densities based on this multipole model are presented. Analysis of their topological properties according to the QTAIM shows that the covalent bonds possess similar properties to the covalent bonds of small molecules. Hydrogen bonds of intermediate strength are identified for the Glu35 and Asp52 residues, which are considered to be essential parts of the active site of HEWL. Furthermore, a series of weak C

  8. The transformation of amorphous calcium carbonate, ACC, to crystalline phases as function of time and temperature.

    Science.gov (United States)

    Gies, Hermann; Happel, Marian; Niedermayr, Andrea; Immenhauser, Adrian

    2017-04-01

    We present results from a structural study of the transformation of freeze dried amorphous calcium carbonate, ACC, in crystalline material using pair distribution function analysis, PDF analysis, of X-ray powder diffraction data, XPD data. PDF analysis allows for the analysis of local order of structural subunit in the range between molecular unit (1. and 2. coordination sphere) and long range periodicity as in crystalline materials. ACC was precipitated from aqueous solutions at 298 K and 278 K using different amounts of Mg cations as stabilizer. The samples were immediately separated from the solution and freeze dried. For the transformation study, the samples were heated and analysed using XPD until they were crystallized. The radial distribution obtained from the XPD data were compared to simulated radial distributions of the calcium carbonate polymorphs and their hydrated phases. An ACC precipitated from a solution with Ca:Mg:CO3 = 1:5:4 at 298 K (ration in mmol, pH = 8.2) and freeze dried right after isolation from the solution revealed a close resemblance with ikaite in its local order. Another ACC with Ca:Mg:CO3 = 1:10:1.4 (T = 298, pH = 8.7) showed distinctly different local order resembling monohydrocalcite. Both ACC, however, still had considerable amounts of water dominating the Ca-coordination sphere. During the transformation to calcite, the structural changes in the sample concerned the hydrate water coordinating Ca which was removed and replaced by the carbonate oxygens. The study shows that ACC obtained from different starting solutions show specific local order. Freeze drying leads to solid ACC powder which still contain considerable amounts of hydrate water. Structural subunits are distinct in ACC and different from the crystalline phase. The study supplements recent reports presented by Konrad et al., Purgstaller et al., and Tobler et al.. F. Konrad et al., Cryst. Growth Des. 16, 6310-6317(2016) B. Purgstaller et al., Geochimica et Cosmochimica

  9. The active site of hen egg-white lysozyme: flexibility and chemical bonding

    International Nuclear Information System (INIS)

    Held, Jeanette; Smaalen, Sander van

    2014-01-01

    Chemical bonding at the active site of lysozyme is analyzed on the basis of a multipole model employing transferable multipole parameters from a database. Large B factors at low temperatures reflect frozen-in disorder, but therefore prevent a meaningful free refinement of multipole parameters. Chemical bonding at the active site of hen egg-white lysozyme (HEWL) is analyzed on the basis of Bader’s quantum theory of atoms in molecules [QTAIM; Bader (1994 ▶), Atoms in Molecules: A Quantum Theory. Oxford University Press] applied to electron-density maps derived from a multipole model. The observation is made that the atomic displacement parameters (ADPs) of HEWL at a temperature of 100 K are larger than ADPs in crystals of small biological molecules at 298 K. This feature shows that the ADPs in the cold crystals of HEWL reflect frozen-in disorder rather than thermal vibrations of the atoms. Directly generalizing the results of multipole studies on small-molecule crystals, the important consequence for electron-density analysis of protein crystals is that multipole parameters cannot be independently varied in a meaningful way in structure refinements. Instead, a multipole model for HEWL has been developed by refinement of atomic coordinates and ADPs against the X-ray diffraction data of Wang and coworkers [Wang et al. (2007), Acta Cryst. D63, 1254–1268], while multipole parameters were fixed to the values for transferable multipole parameters from the ELMAM2 database [Domagala et al. (2012), Acta Cryst. A68, 337–351] . Static and dynamic electron densities based on this multipole model are presented. Analysis of their topological properties according to the QTAIM shows that the covalent bonds possess similar properties to the covalent bonds of small molecules. Hydrogen bonds of intermediate strength are identified for the Glu35 and Asp52 residues, which are considered to be essential parts of the active site of HEWL. Furthermore, a series of weak C

  10. Advances in the EDM-DEDM procedure.

    Science.gov (United States)

    Caliandro, Rocco; Carrozzini, Benedetta; Cascarano, Giovanni Luca; Giacovazzo, Carmelo; Mazzone, Anna Maria; Siliqi, Dritan

    2009-03-01

    The DEDM (difference electron-density modification) algorithm has been described in a recent paper [Caliandro et al. (2008), Acta Cryst. A64, 519-528]: it breaks down the collinearity between model structure phases and difference structure phase estimates. The new difference electron-density produced by DEDM, summed to the calculated Fourier maps, is expected to provide a representation of the full structure that is more accurate than that obtained by the observed Fourier synthesis. In the same paper, the DEDM algorithm was combined with the EDM (electron-density modification) approach to give the EDM-DEDM procedure which, when applied to practical molecular-replacement cases, was able to improve the model structures. In this paper, it is shown that EDM-DEDM suffers from some critical points that did not allow cyclical application of the procedure. These points are identified and modifications are made to allow iteration of the procedure. The applications indicate that EDM-DEDM may become a fundamental tool in protein crystallography.

  11. 4-(4-Bromophenyl-7,7-dimethyl-2-methylamino-3-nitro-7,8-dihydro-4H-chromen-5(6H-one including an unknown solvate

    Directory of Open Access Journals (Sweden)

    S. Antony Inglebert

    2014-05-01

    Full Text Available In the title compound, C18H19BrN2O4, the chromene unit is not quite planar (r.m.s. deviation = 0.199 Å, with the methyl C atoms lying 0.027 (4 and 1.929 (4 Å from the mean plane of the chromene unit. The six-membered carbocyclic ring of the chromene moiety adopts an envelope conformation, with the dimethyl-substituted C atom as the flap. The methylamine and nitro groups are slightly twisted from the chromene moiety, with C—N—C—O and O—N—C—C torsion angles of 2.7 (4 and −0.4 (4°, respectively. The dihedral angle between the mean plane of the chromene unit and the benzene ring is 85.61 (13°. An intramolecular N—H...O hydrogen bond generates an S(6 ring motif, which stabilizes the molecular conformation. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming hexagonal rings lying parallel to the ab plane. A region of disordered electron density, most probably disordered ethanol solvent molecules, occupying voids of ca 432 Å3 for an electron count of 158, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Their formula mass and unit-cell characteristics were not taken into account during refinement.

  12. Phase separation and magnetic ordering studied by high resolution neutron diffraction

    International Nuclear Information System (INIS)

    Caspi, E.N.; Melamud, M.; Pinto, H.; Shaked, H.; Chmaissem, O.; Jorgensen, J.D.; Short, S.

    1999-01-01

    Complete text of publication follows. In a previous work on the (U 1-x Nd x )Co 2 Ge 2 system, two magnetic transitions were observed in the temperature dependencies of the magnetic susceptibility and in the intensity of the magnetic reflections in neutron diffraction [1]. Because of insufficient resolution, it was not clear whether this is due to clustering or phase separation. In both cases the U-rich regions are expected to order magnetically at higher temperature than the U-poor ones, resulting in two magnetic transitions. In order to resolve this question a temperature dependent TOF neutron diffraction of the x = 0.25 compound has been performed on the SEPD at Argonne's IPNS [2]. The temperature dependent diffractograms were refined by the Rietveld method. It was found that the compound separates into two phases: x = 0.4 (55 wt%) and x = 0.1 (45 wt%). The temperature dependence of the magnetic moment was obtained for each phase, with the transition temperatures: T N (x=0.4) = 130 K, and T N (x=0.1) = 165 K. (author) [1] E. Caspi et al., Phys. Rev. B, 57 (198) 449.; [2] J.D. Jorgensen et al., J. Appl. Cryst. 22 (1989) 321

  13. Structural and spectral analyses of N,N'-(2,2'-dithiodi-o-phenylene)bis-(furan-2-carboxamide)

    Science.gov (United States)

    Yıldırım, Sema Öztürk; Büyükmumcu, Zeki; Pekdur, Özlem Savaş; Butcher, Ray J.; Doǧan, Şengül Dilem

    2018-02-01

    In this study we report structure determination of N,N'-(2,2'-dithiodi-o-phenylene)bis-(furan-2-carboxamide). 2,2'-Dithiobis(benzamide) derivatives have been reported to possess important biological properties such as antibacterial, antifungal activities and inhibition of blood platelet aggregation and redeterrmined at 100(2)K from the data published by Raftery, Lallbeeharry, Bhowon, Laulloo & Joulea [Acta Cryst. 2009, E65, o16]. 2,2'-Dithiobis(N-butyl-benzamide) has been reported to be useful as an antiseptic for cosmetics. The structural properties of the compound have been characterized by using 1H NMR and the structure were determined by single-crystal X-ray diffraction. Molecular structure crystallizes in triclinic form, space group with a = 9.6396(7) Å, b = 9.9115(7) Å, c = 12.0026(8) Å, α = 109.743(6)°, β = 103.653(6)°, γ = 104.633(6)° and V = 977.15(13) Å3. In the solid state of the molecular structure N-H…S, N-H…O and C-H…O, type interactions provide for stabilization. The geometries of the title compound have been optimized using density functional theory (DFT) method. The calculated values were found to be in agreement with the experimental data.

  14. A non-solvated form of [(Z-O-methyl-N-(2-methylphenylthiocarbamato-κS](triphenylphosphane-κPgold(I: crystal structure and Hirshfeld surface analysis

    Directory of Open Access Journals (Sweden)

    Chien Ing Yeo

    2016-10-01

    Full Text Available The title compound, [Au(C9H10NOS(C18H15P], features a near linear P—Au—S arrangement defined by phosphane P and thiolate S atoms with the minor distortion from the ideal [P—Au—S is 177.61 (2°] being traced in part to the close intramolecular approach of an O atom [Au...O = 3.040 (2 Å]. The packing features supramolecular layers lying parallel to (011 sustained by a combination of C—H...π and π–π [inter-centroid distance = 3.8033 (17 Å] interactions. The molecular structure and packing are compared with those determined for a previously reported hemi-methanol solvate [Kuan et al. (2008. CrystEngComm, 10, 548–564]. Relatively minor differences are noted in the conformations of the rings in the Au-containing molecules. A Hirshfeld surface analysis confirms the similarity in the packing with the most notable differences relating to the formation of C—H...S contacts between the constituents of the solvate.

  15. Crystal structure refinement of α-Si3N4 using synchrotron radiation powder diffraction data: unbiased refinement strategy

    International Nuclear Information System (INIS)

    Toraya, H.

    2000-01-01

    The crystal structure of α-silicon nitride (Si 3 N 4 ) was refined by the Rietveld method using synchrotron radiation powder diffraction data (wavelength = 1.2 A) collected at station BL-4B2 in the photon factory. A refinement procedure that adopted a new weight function, w = 1/Y o e (Y o is the observed profile intensity and e ≅ 2), for the least-squares fitting [Toraya (1998). J. Appl. Cryst. 31, 333-343] was studied. The most reasonable structural parameters were obtained with e = 1.7. Crystal data of α-Si 3 N 4 : trigonal, P31c, a = 7.75193 (3), c = 5.61949 (4) A, V = 292.447 (3) A 3 , Z = 4; R p = 5.08, R wp = 6.50, R B = 3.36, R F = 2.26%. The following five factors are considered equally important for deriving accurate structural parameters from powder diffraction data: (i) sufficiently large sin θ/λ range of >0.8 A -1 ; (ii) adequate counting statistics; (iii) correct profile model; (iv) proper weighting on observations to give a uniform distribution of the mean weighted squared residuals; (v) high-angular-resolution powder diffraction data. (orig.)

  16. PCDDB: new developments at the Protein Circular Dichroism Data Bank.

    Science.gov (United States)

    Whitmore, Lee; Miles, Andrew John; Mavridis, Lazaros; Janes, Robert W; Wallace, B A

    2017-01-04

    The Protein Circular Dichroism Data Bank (PCDDB) has been in operation for more than 5 years as a public repository for archiving circular dichroism spectroscopic data and associated bioinformatics and experimental metadata. Since its inception, many improvements and new developments have been made in data display, searching algorithms, data formats, data content, auxillary information, and validation techniques, as well as, of course, an increase in the number of holdings. It provides a site (http://pcddb.cryst.bbk.ac.uk) for authors to deposit experimental data as well as detailed information on methods and calculations associated with published work. It also includes links for each entry to bioinformatics databases. The data are freely available to accessors either as single files or as complete data bank downloads. The PCDDB has found broad usage by the structural biology, bioinformatics, analytical and pharmaceutical communities, and has formed the basis for new software and methods developments. © The Author(s) 2016. Published by Oxford University Press on behalf of Nucleic Acids Research.

  17. Sorption of uranyl ions on hydrous silicon dioxide

    International Nuclear Information System (INIS)

    Lieser, K.H.; Quandt-Klenk, S.; Thybusch, B.

    1992-01-01

    Sorption of uranyl ions on SiO 2 .χH 2 O (silica gel) is investigated in absence and in presence of carbonate as function of pH. The curves obtained are very similar to those observed for sorption of uranyl ion on TiO 2 .χH 2 O, indicating the dominating influence of the uranium species in solution. Between pH 2 and 5 the sorption ratio R s increases with hydrolysis of uranyl ions (formation of UO 2 OH + ), around pH 7 it is nearly independent of pH, and at higher pH it decreases again. The equilibrium constants are calculated for these ranges. In presence of carbonate R s decreases drastically above pH 6, due to the formation of carbonato complexes in solution. Sorption of uranyl ions on SiO 2 .χH 2 O, on TiO 2 .χH 2 O, and on cryst. SiO 2 and Al 2 O 3 is compared. The problems of 'surface complexation' modelling are discussed. (orig.)

  18. A comparative analysis of immunorestoration and recovery with conventional and immunotherapeutic protocols in canine generalized demodicosis: a newer insight of immunotherapeutic efficacy of T11TS.

    Science.gov (United States)

    Sarkar, P; Mukherjee, J; Ghosh, A; Bhattacharjee, M; Mahato, S; Chakraborty, A; Mondal, M; Banerjee, C; Chaudhuri, Swapna

    2004-01-01

    Demodex canis is a natural inhabiting mite of canine skin. Immunological disorder or genetic disorder induces the Demodex population to proliferate vigorously resulting in generalized demodicosis with consequent chronic immunosuppression. Signs of generalized demodicosis include alopecia, crysting, erythema, secondary pyoderma etc. Amitraz, an acaricide, is used conventionally for the treatment of generalized demodicosis. In many instances, the disease relapses due to the residual immunosuppression. The need of an immunorestorative therapy has been urged in generalized demodicosis. Two immunorestorative drugs, namely, Immuplus, a herbal drug, and T11TS, a sheep erythrocyte surface glycoprotein, has been used in two separate groups of dogs having generalized demodicosis and receiving Amitraz treatment. It was observed that though Amitraz treated group responded to the therapy showing increased E-rosettes and nonspecific cytotoxic efficacy of T-lymphocytes and decrease in phagocytic potential of macrophages, the groups treated with the immunotherapeutics like Immuplus and T11TS, responded better. However, the group treated with T11TS showed best recovery. These results emphasize the need for an immunorestorative therapy in generalized demodicosis and provide data in favor of T11TS as a better immunomodulator in comparison to Immuplus.

  19. Protein Circular Dichroism Data Bank (PCDDB): data bank and website design.

    Science.gov (United States)

    Whitmore, Lee; Janes, Robert W; Wallace, B A

    2006-06-01

    The Protein Circular Dichroism Data Bank (PCDDB) is a new deposition data bank for validated circular dichroism spectra of biomacromolecules. Its aim is to be a resource for the structural biology and bioinformatics communities, providing open access and archiving facilities for circular dichroism and synchrotron radiation circular dichroism spectra. It is named in parallel with the Protein Data Bank (PDB), a long-existing valuable reference data bank for protein crystal and NMR structures. In this article, we discuss the design of the data bank structure and the deposition website located at http://pcddb.cryst.bbk.ac.uk. Our aim is to produce a flexible and comprehensive archive, which enables user-friendly spectral deposition and searching. In the case of a protein whose crystal structure and sequence are known, the PCDDB entry will be linked to the appropriate PDB and sequence data bank files, respectively. It is anticipated that the PCDDB will provide a readily accessible biophysical catalogue of information on folded proteins that may be of value in structural genomics programs, for quality control and archiving in industrial and academic labs, as a resource for programs developing spectroscopic structural analysis methods, and in bioinformatics studies. Copyright 2006 Wiley-Liss, Inc.

  20. Circular dichroism spectral data and metadata in the Protein Circular Dichroism Data Bank (PCDDB): a tutorial guide to accession and deposition.

    Science.gov (United States)

    Janes, Robert W; Miles, A J; Woollett, B; Whitmore, L; Klose, D; Wallace, B A

    2012-09-01

    The Protein Circular Dichroism Data Bank (PCDDB) is a web-based resource containing circular dichroism (CD) and synchrotron radiation circular dichroism spectral and associated metadata located at http://pcddb.cryst.bbk.ac.uk. This resource provides a freely available, user-friendly means of accessing validated CD spectra and their associated experimental details and metadata, thereby enabling broad usage of this material and new developments across the structural biology, chemistry, and bioinformatics communities. The resource also enables researchers utilizing CD as an experimental technique to have a means of storing their data at a secure site from which it is easily retrievable, thereby making their results publicly accessible, a current requirement of many grant-funding agencies world-wide, as well as meeting the data-sharing requirements for journal publications. This tutorial provides extensive information on searching, accessing, and downloading procedures for those who wish to utilize the data available in the data bank, and detailed information on deposition procedures for creating and validating entries, including comprehensive explanations of their contents and formats, for those who wish to include their data in the data bank. Copyright © 2012 Wiley Periodicals, Inc.

  1. 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.

  2. Can I solve my structure by SAD phasing? Planning an experiment, scaling data and evaluating the useful anomalous correlation and anomalous signal.

    Science.gov (United States)

    Terwilliger, Thomas C; Bunkóczi, Gábor; Hung, Li Wei; Zwart, Peter H; Smith, Janet L; Akey, David L; Adams, Paul D

    2016-03-01

    A key challenge in the SAD phasing method is solving a structure when the anomalous signal-to-noise ratio is low. Here, algorithms and tools for evaluating and optimizing the useful anomalous correlation and the anomalous signal in a SAD experiment are described. A simple theoretical framework [Terwilliger et al. (2016), Acta Cryst. D72, 346-358] is used to develop methods for planning a SAD experiment, scaling SAD data sets and estimating the useful anomalous correlation and anomalous signal in a SAD data set. The phenix.plan_sad_experiment tool uses a database of solved and unsolved SAD data sets and the expected characteristics of a SAD data set to estimate the probability that the anomalous substructure will be found in the SAD experiment and the expected map quality that would be obtained if the substructure were found. The phenix.scale_and_merge tool scales unmerged SAD data from one or more crystals using local scaling and optimizes the anomalous signal by identifying the systematic differences among data sets, and the phenix.anomalous_signal tool estimates the useful anomalous correlation and anomalous signal after collecting SAD data and estimates the probability that the data set can be solved and the likely figure of merit of phasing.

  3. Raster-scanning serial protein crystallography using micro- and nano-focused synchrotron beams

    Energy Technology Data Exchange (ETDEWEB)

    Coquelle, Nicolas [Université Grenoble Alpes, IBS, 38044 Grenoble (France); CNRS, IBS, 38044 Grenoble (France); CEA, IBS, 38044 Grenoble (France); Brewster, Aaron S. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Kapp, Ulrike; Shilova, Anastasya; Weinhausen, Britta [European Synchrotron Radiation Facility, BP 220, 38043 Grenoble (France); Burghammer, Manfred, E-mail: burgham@esrf.fr [European Synchrotron Radiation Facility, BP 220, 38043 Grenoble (France); Ghent University, Ghent B-9000 (Belgium); Colletier, Jacques-Philippe, E-mail: burgham@esrf.fr [Université Grenoble Alpes, IBS, 38044 Grenoble (France); CNRS, IBS, 38044 Grenoble (France); CEA, IBS, 38044 Grenoble (France)

    2015-05-01

    A raster scanning serial protein crystallography approach is presented, that consumes as low ∼200–700 nl of sedimented crystals. New serial data pre-analysis software, NanoPeakCell, is introduced. High-resolution structural information was obtained from lysozyme microcrystals (20 µm in the largest dimension) using raster-scanning serial protein crystallography on micro- and nano-focused beamlines at the ESRF. Data were collected at room temperature (RT) from crystals sandwiched between two silicon nitride wafers, thereby preventing their drying, while limiting background scattering and sample consumption. In order to identify crystal hits, new multi-processing and GUI-driven Python-based pre-analysis software was developed, named NanoPeakCell, that was able to read data from a variety of crystallographic image formats. Further data processing was carried out using CrystFEL, and the resultant structures were refined to 1.7 Å resolution. The data demonstrate the feasibility of RT raster-scanning serial micro- and nano-protein crystallography at synchrotrons and validate it as an alternative approach for the collection of high-resolution structural data from micro-sized crystals. Advantages of the proposed approach are its thriftiness, its handling-free nature, the reduced amount of sample required, the adjustable hit rate, the high indexing rate and the minimization of background scattering.

  4. Cannabidiol revisited

    Directory of Open Access Journals (Sweden)

    Tobias Mayr

    2017-02-01

    Full Text Available The crystal structure of cannabidiol, C21H30O2, {systematic name: 2-[(1R,6R-3-methyl-6-(prop-1-en-2-ylcyclohex-2-enyl]-5-pentylbenzene-1,3-diol}, was determined earlier by Jones et al. [(1977. Acta Cryst. B33, 3211–3214] and Ottersen & Rosenqvist [(1977. Acta Chem. Scand. B31, 749–755]. In both investigations, the absolute configuration is given as R,R, referring to Mechoulam et al. [(1967.J. Am. Chem. Soc. 89, 4552–4554]. In the latter, the absolute configuration was identified by chemical means. Using the advantages of modern single-crystal X-ray diffractometers such as area detectors and high-intensity radiation sources, a high-quality structure determination including the absolute configuration was possible and is shown in this work. Furthermore, the rather uncommon Cu Kβ wavelength radiation was applied for the structure determination, which confirmed the absolute structure to be R,R.

  5. (η(6)-Benzene)(carbonato-κ(2) O,O')[di-cyclohex-yl(naphthalen-1-ylmeth-yl)phosphane-κP]ruthenium(II) chloro-form tris-olvate.

    Science.gov (United States)

    Gowrisankar, Saravanan; Neumann, Helfried; Spannenberg, Anke; Beller, Matthias

    2014-07-01

    The title compound, [Ru(CO3)(η(6)-C6H6){(C6H11)2P(CH2C10H7)}]·3CHCl3, was synthesized by carbonation of [RuCl2(η(6)-C6H6){(C6H11)2P(CH2C10H7)}] with NaHCO3 in methanol at room temperature. The Ru(II) atom is surrounded by a benzene ligand, a chelating carbonate group and a phosphane ligand in a piano-stool configuration. The crystal packing is consolidated by C-H⋯O and C-H⋯Cl hydrogen-bonding inter-actions between adjacent metal complexes and between the complexes and the solvent mol-ecules. The asymmetric unit contains one metal complex and three chloro-form solvent mol-ecules of which only one was modelled. The estimated diffraction contributions of the other two strongly disordered chloro-form solvent mol-ecules were substracted from the observed diffraction data using the SQUEEZE procedure in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148-155].

  6. (η6-Benzene)(carbonato-κ2 O,O′)[di­cyclohex­yl(naphthalen-1-ylmeth­yl)phosphane-κP]ruthenium(II) chloro­form tris­olvate

    Science.gov (United States)

    Gowrisankar, Saravanan; Neumann, Helfried; Spannenberg, Anke; Beller, Matthias

    2014-01-01

    The title compound, [Ru(CO3)(η6-C6H6){(C6H11)2P(CH2C10H7)}]·3CHCl3, was synthesized by carbonation of [RuCl2(η6-C6H6){(C6H11)2P(CH2C10H7)}] with NaHCO3 in methanol at room temperature. The RuII atom is surrounded by a benzene ligand, a chelating carbonate group and a phosphane ligand in a piano-stool configuration. The crystal packing is consolidated by C—H⋯O and C—H⋯Cl hydrogen-bonding inter­actions between adjacent metal complexes and between the complexes and the solvent mol­ecules. The asymmetric unit contains one metal complex and three chloro­form solvent mol­ecules of which only one was modelled. The estimated diffraction contributions of the other two strongly disordered chloro­form solvent mol­ecules were substracted from the observed diffraction data using the SQUEEZE procedure in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148–155]. PMID:25161531

  7. (η6-Benzene(carbonato-κ2O,O′[dicyclohexyl(naphthalen-1-ylmethylphosphane-κP]ruthenium(II chloroform trisolvate

    Directory of Open Access Journals (Sweden)

    Saravanan Gowrisankar

    2014-07-01

    Full Text Available The title compound, [Ru(CO3(η6-C6H6{(C6H112P(CH2C10H7}]·3CHCl3, was synthesized by carbonation of [RuCl2(η6-C6H6{(C6H112P(CH2C10H7}] with NaHCO3 in methanol at room temperature. The RuII atom is surrounded by a benzene ligand, a chelating carbonate group and a phosphane ligand in a piano-stool configuration. The crystal packing is consolidated by C—H...O and C—H...Cl hydrogen-bonding interactions between adjacent metal complexes and between the complexes and the solvent molecules. The asymmetric unit contains one metal complex and three chloroform solvent molecules of which only one was modelled. The estimated diffraction contributions of the other two strongly disordered chloroform solvent molecules were substracted from the observed diffraction data using the SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  8. (E-1-Phenylethanone semicarbazone

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2009-08-01

    Full Text Available In the title compound, C9H11N3O, the benzene ring is disordered over two positions with refined occupancies of 0.922 (5 and 0.078 (5. The program PLATON [Spek (2009. Acta Cryst. D65, 148–155] recommends the solution in the space group C2/m with a = 7.3050 (3, b = 6.6745 (2, c = 18.3853 (6 Å and β = 96.986 (2°. However, the large number of non-extinct reflections needed to be ignored if C2/m is chosen suggested that the space group is incorrect, even though the R values are lower than that for P21/c. The semicarbazone group is essentially planar, with a maximum deviation of 0.046 (1 Å for one of the N atoms. The mean plane of the semicarbazone group forms dihedral angles of 33.61 (8 and 39.1 (9° with the benzene ring of the major and minor components, respectively. In the crystal structure, molecules are linked by intermolecular N—H...O hydrogen bonds into extended chains along the c axis. The crystal structure is further stabilized by weak intermolucular C—H...π interactions.

  9. A P212121 polymorph of (+-clusianone

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    Teng-Jin Khoo

    2013-12-01

    Full Text Available The title compound, C33H42O4 [systematic name: (1S,5S,7R-3-benzoyl-4-hydroxy-8,8-dimethyl-1,5,7-tris(3-methylbut-2-enylbicyclo[3.3.1]nona-3-ene-2,9-dione], has a central bicyclo[3.3.1]nonane-2,4,9-trione surrounded by tetraprenylated and benzoyl groups. The compound was recrystallized several times in methanol using both a slow evaporation method and with a crystal-seeding technique. This subsequently produced diffraction-quality crystals which crystallize in the orthorhombic space group P212121, in contrast to a previous report of a structure determination in the Pna21 space group [McCandlish et al. (1976. Acta Cryst. B32, 1793–1801]. The title compound has a melting point of 365–366 K, and a specific rotation [α]20 value of +51.94°. A strong intramolecular O—H...O hydrogen bond is noted. In the crystal, molecules are assembled in the ab plane by weak C—H...O interactions.

  10. Solid-State Characterization and Relative Formation Enthalpies To Evaluate Stability of Cocrystals of an Antidiabetic Drug.

    Science.gov (United States)

    Duggirala, Naga Kiran; Frericks Schmidt, Heather L; Lei, Zhaohui; Zaworotko, Michael J; Krzyzaniak, Joseph F; Arora, Kapildev K

    2018-05-07

    The current study integrates formation enthalpy and traditional slurry experiments to quickly assess the physical stability of cocrystal drug substance candidates for their potential to support drug development. Cocrystals of an antidiabetic drug (GKA) with nicotinamide (NMA), vanillic acid (VLA), and ethyl vanillin (EVL) were prepared and characterized by powder X-ray diffractometry (PXRD), spectroscopic, and thermal techniques. The formation enthalpies of the cocrystals, and their physical mixtures (GKA + coformer) were measured by the differential scanning calorimetry (DSC) method reported by Zhang et al. [ Cryst. Growth Des. 2012 , 12 ( 8 ), 4090 - 4097 ]. The experimentally measured differences in the relative formation enthalpies obtained by integrating the heat flow of each cocrystal against the respective physical mixture were correlated to the physical stability of the cocrystals in the solid state. The relative formation enthalpies of all of the cocrystals studied suggest that the cocrystals are not physically stable at room temperature versus their physical mixtures. To further address relative stability, the cocrystals were slurried in 30% v/v aqueous ethanol, and it was observed that all of the cocrystals revert to GKA within 48 h at room temperature. The slurry experiments are consistent with the relative instability of the cocrystals with respect to their physical mixtures suggested by the DSC results.

  11. Crystal structure of tetrakis[μ2-2-(dimethylaminoethanolato-κ3N,O:O]di-μ3-hydroxido-dithiocyanato-κ2N-dichromium(IIIdilead(II dithiocyanate acetonitrile monosolvate

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    Julia A. Rusanova

    2016-04-01

    Full Text Available The tetranuclear complex cation of the title compound, [Cr2Pb2(NCS2(OH2(C4H10NO4](SCN2·CH3CN, lies on an inversion centre. The main structural feature of the cation is a distorted seco-norcubane Pb2Cr2O6 cage with a central four-membered Cr2O2 ring. The CrIII ion is coordinated in a distorted octahedron, which involves two N atoms of one bidentate ligand and one thiocyanate anion, two μ2-O atoms of 2-(dimethylaminoethanolate ligands and two μ3-O atoms of hydroxide ions. The coordination geometry of the PbII ion is a distorted disphenoid, which involves one N atom, two μ2-O atoms and one μ3-O atom. In addition, weak Pb...S interactions involving the coordinating and non-coordinating thiocyanate anions are observed. In the crystal, the complex cations are linked through the thiocyanate anions via the Pb...S interactions and O—H...N hydrogen bonds into chains along the c axis. The chains are further linked together via S...S contacts. The contribution of the disordered solvent acetonitrile molecule was removed with the SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] procedure in PLATON. The solvent is included in the reported molecular formula, weight and density.

  12. Nitrosonium complexation by the tetraphosphonate cavitand 5,11,17,23-tetramethyl-6,10:12,16:18,22:24,4-tetrakis(phenylphosphonato-κ2O,Oresorcin(4arene

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    Roberta Pinalli

    2017-12-01

    Full Text Available The crystal structure of a new supramolecular complex between the tetraphosphonate cavitand 5,11,17,23-tetramethyl-6,10:12,16:18,22:24,4-tetrakis(phenylphosphonato-κ2O,O′resorcin(4arene and the nitrosyl cation NO+, as the BF4− salt, is reported. The complex, of general formula [(C56H44P4O12(NO]BF4·CH2Cl2 or NO@Tiiii[H, CH3, C6H5] BF4·CH2Cl2, crystallizes in the space group P-1. The nitrosyl cation is disordered over two equivalent positions, with occupancies of 0.503 (2 and 0.497 (2, and interacts with two adjacent P=O groups at the upper rim of the cavitand through dipole–charge interactions. In the lattice, the cavitands are connected through a series of C—H...π interactions involving the methyl and methylenic H atoms and the aromatic rings of the macrocycle. The structure is further stabilized by the presence of C—H...F interactions between the hydrogen atoms of the cavitands and the F atoms of the tetrafluoridoborate anion. As a result of the disorder, the lattice dichloromethane molecules could not be modelled in terms of atomic sites, and were treated using the PLATON SQUEEZE procedure [Spek (2015. Acta Cryst. C71, 9–18]. The complexation process has also been studied in solution through NMR titrations.

  13. (1,6,7,12-Tetraazaperylene-κ2N,N′bis(4,4′,5,5′-tetramethyl-2,2′-bipyridyl-κ2N,N′ruthenium(II bis(hexafluoridophosphate acetonitrile trisolvate

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    Thomas Brietzke

    2014-06-01

    Full Text Available In the title compound, rac-[Ru(C14H16N22(C16H8N4](PF62·3C2H3N, discrete dimers of complex cations, [Ru(tmbpy2tape]2+, of opposite chirality are formed (tmbpy = tetramethylbipyridine; tape = tetraazaperylene, held together by π–π stacking interactions between the tetraazaperylene moieties with centroid–centroid distances in the range 3.563 (3–3.837 (3 Å. These interactions exhibit a parallel displaced π–π stacking mode. Additional weak C—H...π-ring and C—H...N and C—H...F interactions are found, leading to a three-dimensional architecture. The RuII atom is coordinated in a distorted octahedral geometry. The counter-charge is provided by two hexafluoridophosphate anions and the asymmetric unit is completed by three acetonitrile solvent molecules of crystallization. Four F atoms of one PF6− anion are disordered over three sets of sites with occupancies of 0.517 (3:0.244 (3:0.239 (3. Two acetonitrile solvent molecules are highly disordered and their estimated scattering contribution was subtracted from the observed diffraction data using the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  14. Protein energy landscapes determined by five-dimensional crystallography

    International Nuclear Information System (INIS)

    Schmidt, Marius; Srajer, Vukica; Henning, Robert; Ihee, Hyotcherl; Purwar, Namrta; Tenboer, Jason; Tripathi, Shailesh

    2013-01-01

    Barriers of activation within the photocycle of a photoactive protein were extracted from comprehensive time courses of time resolved crystallographic data collected at multiple temperature settings. Free-energy landscapes decisively determine the progress of enzymatically catalyzed reactions [Cornish-Bowden (2012 ▶), Fundamentals of Enzyme Kinetics, 4th ed.]. Time-resolved macromolecular crystallography unifies transient-state kinetics with structure determination [Moffat (2001 ▶), Chem. Rev.101, 1569–1581; Schmidt et al. (2005 ▶), Methods Mol. Biol.305, 115–154; Schmidt (2008 ▶), Ultrashort Laser Pulses in Medicine and Biology] because both can be determined from the same set of X-ray data. Here, it is demonstrated how barriers of activation can be determined solely from five-dimensional crystallography, where in addition to space and time, temperature is a variable as well [Schmidt et al. (2010 ▶), Acta Cryst. A66, 198–206]. Directly linking molecular structures with barriers of activation between them allows insight into the structural nature of the barrier to be gained. Comprehensive time series of crystallographic data at 14 different temperature settings were analyzed and the entropy and enthalpy contributions to the barriers of activation were determined. One hundred years after the discovery of X-ray scattering, these results advance X-ray structure determination to a new frontier: the determination of energy landscapes

  15. Structural study and thermodynamic characterization of inhibitor binding to lumazine synthase from Bacillus anthracis

    Energy Technology Data Exchange (ETDEWEB)

    Morgunova, Ekaterina [Karolinska Institutet NOVUM, Center of Structural Biochemistry, Hälsovägen 7-9, 141 57 Huddinge (Sweden); Illarionov, Boris; Saller, Sabine [Institut für Lebensmittelchemie, Universität Hamburg, Grindelallee 117, 20146 Hamburg (Germany); Popov, Aleksander [European Synchrotron Radiation Facility, BP 220, F-38043 Grenoble CEDEX 09 (France); Sambaiah, Thota [Department of Medicinal Chemistry and Molecular Pharmacology, Purdue University (United States); Bacher, Adelbert [Chemistry Department, Technical University of Munich, 85747 Garching (Germany); Cushman, Mark [Department of Medicinal Chemistry and Molecular Pharmacology, Purdue University (United States); Fischer, Markus [Institut für Lebensmittelchemie, Universität Hamburg, Grindelallee 117, 20146 Hamburg (Germany); Ladenstein, Rudolf, E-mail: rudolf.ladenstein@ki.se [Karolinska Institutet NOVUM, Center of Structural Biochemistry, Hälsovägen 7-9, 141 57 Huddinge (Sweden)

    2010-09-01

    Crystallographic studies of lumazine synthase, the penultimate enzyme of the riboflavin-biosynthetic pathway in B. anthracis, provide a structural framework for the design of antibiotic inhibitors, together with calorimetric and kinetic investigations of inhibitor binding. The crystal structure of lumazine synthase from Bacillus anthracis was solved by molecular replacement and refined to R{sub cryst} = 23.7% (R{sub free} = 28.4%) at a resolution of 3.5 Å. The structure reveals the icosahedral symmetry of the enzyme and specific features of the active site that are unique in comparison with previously determined orthologues. The application of isothermal titration calorimetry in combination with enzyme kinetics showed that three designed pyrimidine derivatives bind to lumazine synthase with micromolar dissociation constants and competitively inhibit the catalytic reaction. Structure-based modelling suggested the binding modes of the inhibitors in the active site and allowed an estimation of the possible contacts formed upon binding. The results provide a structural framework for the design of antibiotics active against B. anthracis.

  16. Density scaling of the transport properties of molecular and ionic liquids.

    Science.gov (United States)

    López, Enriqueta R; Pensado, Alfonso S; Comuñas, María J P; Pádua, Agílio A H; Fernández, Josefa; Harris, Kenneth R

    2011-04-14

    Casalini and Roland [Phys. Rev. E 69, 062501 (2004); J. Non-Cryst. Solids 353, 3936 (2007)] and other authors have found that both the dielectric relaxation times and the viscosity, η, of liquids can be expressed solely as functions of the group (TV (γ)), where T is the temperature, V is the molar volume, and γ a state-independent scaling exponent. Here we report scaling exponents γ, for the viscosities of 46 compounds, including 11 ionic liquids. A generalization of this thermodynamic scaling to other transport properties, namely, the self-diffusion coefficients for ionic and molecular liquids and the electrical conductivity for ionic liquids is examined. Scaling exponents, γ, for the electrical conductivities of six ionic liquids for which viscosity data are available, are found to be quite close to those obtained from viscosities. Using the scaling exponents obtained from viscosities it was possible to correlate molar conductivity over broad ranges of temperature and pressure. However, application of the same procedures to the self-diffusion coefficients, D, of six ionic and 13 molecular liquids leads to superpositioning of poorer quality, as the scaling yields different exponents from those obtained with viscosities and, in the case of the ionic liquids, slightly different values for the anion and the cation. This situation can be improved by using the ratio (D∕T), consistent with the Stokes-Einstein relation, yielding γ values closer to those of viscosity.

  17. 1,4,9,12-Tetramethoxy-14-octyl-5,8-dihydrodiindolo[3,2-b;2′,3′-h]carbazole with an unknown solvent

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    Norma Wrobel

    2017-03-01

    Full Text Available The title compound, 2C36H39N3O4·H2O, is a linear π-conjugated ladder oligomer with an alkyl chain on the central nitrogen atom. This diindolocarbazole, prepared via a twofold Cadogan reaction, adopts a sligthly convex shape, anti to the disordered octyl group. The unit cell contains nine molecules of the title compound and half a water molecule per main molecule. The water molecule forms hydrogen bridges, connecting the carbazole-NH and methoxy groups of different molecules. The crystal contains solvent molecules which are located in a channel parallel to the c axis. It was not possible to determine the position and nature of the solvent (a mixure of choroform, n-pentane and DMSO. The SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] option of PLATON was used to model the missing electron density. The given chemical formula and other crystal data do not take into account these solvent molecules.

  18. An unexpected oxidation: NaK5Cl2(S2O62 revisited

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    William T. A. Harrison

    2017-02-01

    Full Text Available The title compound, NaK5Cl2(S2O62 [systematic name: sodium pentapotassium dichloride bis(dithionate], arose as an unexpected product from an organic synthesis that used dithionite (S2O42− ions as a reducing agent to destroy excess permanganate ions. Compared to the previous study [Stanley (1953. Acta Cryst. 6, 187–196], the present tetragonal structure exhibits a root 2a × root 2a × c super-cell due to subtle changes in the orientations of the dithionate anions. The structure can be visualized as a three-dimensional framework of [001] columns of alternating trans-NaO4Cl2 and KO4Cl2 octahedra cross-linked by the dithionate ions with the interstices occupied by KO6Cl2 polyhedra to generate a densely packed three-dimensional framework. The asymmetric unit comprises two sodium ions (site symmetries 4 and -4, four potassium ions (site symmetries = -4, 4, 1 and 1, three chloride ions (site symmetries = 4, 4 and 2 and two half-dithionate ions (all atoms on general positions. Both dithionate ions are completed by crystallographic inversion symmetry. The crystal chosen for data collection was found to be rotationally twinned by 180° about the [100] axis in reciprocal space with a 0.6298 (13:0.3702 (13 domain ratio.

  19. Tetrakis(μ2-2,2-dimethylpropanoato-κ2O,O′bis[(pyridine-κNcopper(II]: a monoclinic polymorph

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    Lailatun Nazirah Ozair

    2010-05-01

    Full Text Available The structure of the dinuclear title complex, [Cu2(C5H9O24(C5H5N2], represents a monoclinic polymorph of the previously reported triclinic form [Blewett et al. (2006. Acta Cryst. E62, m420–m422]. Each carboxylate group is bidentate bridging and the distorted octahedral geometry about each CuII atom is completed by a pyridine N atom and the other Cu atom [Cu...Cu = 2.6139 (7 Å]. In the crystal, molecules are connected into supramolecular chains via π–π interactions formed by the pyridine rings [centroid–centroid distance = 3.552 (3 Å] and these are connected into a two-dimensional array in the ac plane by C—H...π contacts. One of the tert-butyl groups is disordered over two orientations in a 0.734 (6:0.266 (6 ratio.

  20. A second orthorhombic polymorph of (Z-3-(9-anthryl-1-(2-thienylprop-2-en-1-oneThis paper is dedicated to His Majesty King Bhumibol Adulyadej of Thailand (King Rama IX for his sustainable development of the country.

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    Suchada Chantrapromma

    2010-02-01

    Full Text Available The title heteroaryl chalcone, C21H14OS, is a second orthorhombic polymorph which crystallizes in the space group P212121. The structure was previously reported [Fun et al. (2009. Acta Cryst. E65, o2168-o2169] in the space group Pna21. The bond distances and angles are similar in both structures. In contrast, the overall crystal packing is different from that in the first orthorhombic Pna21 polymorph in which molecules were stacked into columns along the b axis and the thiophene units of two adjacent columns were stacked in a head to tail fashion. In the present polymorph, molecules are found to dimerize through a weak S...S interaction [3.6513 (7 Å] and these dimers are arranged into sheets parallel to the bc plane. There are no classical hydrogen bonds in the packing which features short C...O [3.2832 (2–3.6251 (9 Å], C...S [3.4879 (17–3.6251 (19 Å] and S...O [2.9948 (16 Å] contacts, together with C—H...π interactions. Similar contacts were found in the other polymorph.

  1. Nitrogen bonding in aluminum oxynitride films

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Paul W., E-mail: pwang@bradley.edu [Department of Physics, Bradley University, 1501 W. Bradley Ave., Peoria, IL 61625 (United States); Hsu, Jin-Cherng [Department of Physics, Fu Jen Catholic University, Hsinchuang, Taipei Hsien 24205, Taiwan (China); Lin, Yung-Hsin; Chen, Huang-Lu [Graduate Institute of Applied Science and Engineering, Fu Jen Catholic University, Hsinchuang, Taipei Hsien 24205, Taiwan (China)

    2010-04-15

    Assignment of oxidation states of N{sub 1s} in XPS spectra of aluminum oxynitride by curve fitting is difficult. The XPS curve fitting was previously discussed in the paper published in J. Non-Cryst. Solids, 224 (1998) 31, in which O{sub 1s} photoelectrons from GeO{sub 2} glass were used to illustrate how to fit the XPS spectra. Three different ways were pointed out to eliminate the ambiguity caused by curve fitting such as comparing the data to data from standard samples, investigating the continuous surface modifications caused by slowly sputtering the surface, and monitoring the continuous surface modifications due to gradual increases in surface species under heating, cooling, or irradiation. Our recent work in aluminum oxynitride films provides another example of how to fit the XPS spectra of N{sub 1s} by three different oxidation states of N{sup +}, N{sup 2+}, and N{sup 3+}, by comparison of the measured data to data from previously published results, and by the gradual changes of spectra as functions of the oxygen contents in the films. Three oxidation states in different nitrogen bonding in the aluminum oxynitride, AlO{sub 2}N, Al{sub 2}O{sub 5}N{sub 2}, and AlO{sub 3}N, were clearly deduced.

  2. 4′,5-Dihy­droxy-7-meth­oxy­flavanone dihydrate

    Science.gov (United States)

    Brito, Iván; Bórquez, Jorge; Simirgiotis, Mario; Cárdenas, Alejandro; López-Rodríguez, Matías

    2012-01-01

    The title compound, C16H14O5·2H2O [systematic name: 5-hy­droxy-2-(4-hy­droxy­phen­yl)-7-meth­oxy­chroman-4-one dihydrate], is a natural phytoalexin flavone isolated from the native chilean species Heliotropium taltalense and crystallizes with an organic mol­ecule and two water mol­ecules in the asymmetric unit. The 5-hy­droxy group forms a strong intra­molecular hydrogen bond with the carbonyl group, resulting in a six-membered ring. In the crystal, the components are linked by O—H⋯O hydrogen bonds, forming a three-dimensional network. The 4-hy­droxy­phenyl benzene ring is bonded equatorially to the pyrone ring, which adopts a slightly distorted sofa conformation. The title compound is the hydrated form of a previously reported structure [Shoja (1990 ▶). Acta Cryst. C46, 1969–1971]. There are only slight variations in the mol­ecular geometry between the two compounds. PMID:22259537

  3. Aqua(μ-cone-26,28-dibutoxy-25,27-bis{N-[5-(dimethylaminonaphthalene-1-sulfonyl]carbamoylmethoxy}-5,11,17,23-tetrakis(1,1-dimethylethylcalix[4]arene(2−disodium acetonitrile tetrasolvate

    Directory of Open Access Journals (Sweden)

    Pogisego Dinake

    2012-04-01

    Full Text Available The structure of the title complex, [Na2(C80H98N4O10S2(H2O]·4CH3CN, obtained after crystallization from acetonitrile, contains two formula units in the asymmetric unit (Z′ = 2 and an estimated four molecules of acetonitrile per calixarene moiety. It is unusual for two Na+ ions to occupy the lower rims of the cone calix[4]arene, as in this case, with one Na+ ion forming two O→ Na+ coordinate bonds with the two butoxy groups and four such bonds with the two N-dansyl carboxamide groups, forming six dative bonds between Na+ and O. On the other hand, the other Na+ ion forms only five O→Na+ coordinate bonds on the far end of the calix[4]arene lower rim, bringing the two dansyl groups in close proximity with each other. There also appears to be an O→Na+ coordination coming from a dangling water molecule. The structure contained both resolved and poorly resolved solvent molecules. The latter were treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  4. Etude structurale et vibrationnelle d'un nouveau composé complexe de cobalt: [Co(imidazole)4Cl]Cl.

    Science.gov (United States)

    Derbel, Amira; Mhiri, Tahar; Graia, Mohsen

    2015-10-01

    In the title complex, chlorido-tetra-kis-(1H-imidazole-κN (3))cobalt(II) chloride, [CoCl(C3H4N2)4]Cl, the Co(II) cation has a distorted square-pyramidal coordination environment. It is coordinated by four N atoms of four imidazole (Im) groups in the basal plane, and by a Cl atom in the apical position. It is isostructural with [Cu(Im)4Cl]Cl [Morzyk-Ociepa et al. (2012 ▸). J. Mol. Struct. 1028, 49-56] and [Cu(Im)4Br]Br [Hossaini Sadr et al. (2004 ▸). Acta Cryst. E60, m1324-m1326]. In the crystal, the [CoCl(C3H4N2)4](+) cations and Cl(-) anions are linked via N-H⋯Cl hydrogen bonds, forming layers parallel to (010). These layers are linked via C-H⋯Cl hydrogen bonds and C-H⋯π and π-π [inter-centroid distance = 3.794 (2) Å] inter-actions, forming a three-dimensional framework. The IR spectrum shows vibrational bands typical for imidazol groups. The monoclinic unit cell of the title compound emulates an ortho-rhom-bic cell as its β angle is close to 90°. The crystal is twinned, with the refined ratio of twin components being 0.569 (1):0.431 (1).

  5. 5,10,15,20-Tetrakis(4-acetyloxyphenylporphyrin including an unknown solvate

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    Micael D. Miranda

    2012-12-01

    Full Text Available Molecules of the title compound, C52H38N4O8, are located on an inversion center so that the asymmetric cell contains one half of the molecule. The macrocycle exhibits a ruffled conformation with a maximum deviation of 0.16 Å for the 24 macrocycle atoms: the dihedral angle between adjacent five-membered rings is 5.13 (19°. The benzene rings are rotated by 70.25 (19° with respect to their adjacent protonated five-membered rings, and by 65.56 (19° with respect to the unprotonated rings. The porphyrin conformation is supported by bifurcated N—H...(N,N hydrogen bonds. The structure contained poorly resolved solvent molecules in voids of volume 217 Å3 per unit cell. The latter were treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. As the solvent could not be identified exactly, it was not included in the calculation of the overall formula weight, density and absorption coefficient.

  6. Continuous wave and time resolved spectroscopy of InAsN/GaAsN based quantum dots

    International Nuclear Information System (INIS)

    Taliercio, T.; Valvin, P.; Intartaglia, R.; Guillet, T.; Lefebvre, P.; Bretagnon, T.; Gil, B.; Sallet, V.; Harmand, J.C.

    2005-01-01

    We present a study of the optical properties of quantum dots based on a new family of semiconductors: III-V dilute nitrides such as (In,Ga)(N,As). Continuous wave and time resolved photoluminescence (PL) experiments allowed us to evaluate the impact of N incorporation during the growth of InAs/GaAs quantum dots. Previous work [V. Sallet et al., to be submitted to J. Cryst. Growth (2005); O. Schumann et al., J. Appl. Phys. 96, 2832 (2004)] showed that increasing the flux of N atoms into the growth chamber modifies drastically the size of the dots which leads to a bimodal growth. Two populations of dots with different sizes appear. The quantum dot PL line broadens and a second PL line appears at higher energy. Time resolved PL allows us to identify the nature of this second PL line: second population of quantum dots. A second decay time is observed which we interpret as being the consequence of the perturbation of the electronic states of the quantum dots. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  7. Redetermination of 1-carboxycyclohexan-1-aminium chloride

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    Teresa González

    2009-02-01

    Full Text Available The crystal structure of the title compound, C7H14NO2+·Cl−, was reported previously [Chacko, Srinivasan & Zand (1975. J. Cryst. Mol. Struct. 5, 353–357] from Weissenberg photographic data with R = 0.113. It has now been redetermined, providing a significant increase in the precision of the derived geometric parameters, viz. mean σ(C—C = 0.003 Å in the present work compared with 0.021 Å for the previous work. The complete cation is generated by crystallographic mirrror symmetry, with three C atoms, two O atoms and the N atom lying on the reflecting plane; the chloride anion also has m site symmetry. The crystal structure is established by a two-dimensional network of O—H...Cl and N—H...Cl hydrogen bonds, generating C12(4 and C12(7 chains, and R24(8 and R24(14 rings.

  8. Structure of the Unbound Form of HIV-1 Subtype A Protease: Comparison with Unbound Forms of Proteases from other HIV Subtypes

    Energy Technology Data Exchange (ETDEWEB)

    Robbins, Arthur H.; Coman, Roxana M.; Bracho-Sanchez, Edith; Fernandez, Marty A.; Gilliland, C.Taylor; Li, Mi; Agbandje-McKenna, Mavis; Wlodawer, Alexander; Dunn, Ben M.; McKenna, Robert (NCI); (Florida)

    2010-03-12

    The crystal structure of the unbound form of HIV-1 subtype A protease (PR) has been determined to 1.7 {angstrom} resolution and refined as a homodimer in the hexagonal space group P6{sub 1} to an R{sub cryst} of 20.5%. The structure is similar in overall shape and fold to the previously determined subtype B, C and F PRs. The major differences lie in the conformation of the flap region. The flaps in the crystal structures of the unbound subtype B and C PRs, which were crystallized in tetragonal space groups, are either semi-open or wide open. In the present structure of subtype A PR the flaps are found in the closed position, a conformation that would be more anticipated in the structure of HIV protease complexed with an inhibitor. The amino-acid differences between the subtypes and their respective crystal space groups are discussed in terms of the differences in the flap conformations.

  9. Powder diffraction from a continuous microjet of submicrometer protein crystals.

    Science.gov (United States)

    Shapiro, D A; Chapman, H N; Deponte, D; Doak, R B; Fromme, P; Hembree, G; Hunter, M; Marchesini, S; Schmidt, K; Spence, J; Starodub, D; Weierstall, U

    2008-11-01

    Atomic-resolution structures from small proteins have recently been determined from high-quality powder diffraction patterns using a combination of stereochemical restraints and Rietveld refinement [Von Dreele (2007), J. Appl. Cryst. 40, 133-143; Margiolaki et al. (2007), J. Am. Chem. Soc. 129, 11865-11871]. While powder diffraction data have been obtained from batch samples of small crystal-suspensions, which are exposed to X-rays for long periods of time and undergo significant radiation damage, the proof-of-concept that protein powder diffraction data from nanocrystals of a membrane protein can be obtained using a continuous microjet is shown. This flow-focusing aerojet has been developed to deliver a solution of hydrated protein nanocrystals to an X-ray beam for diffraction analysis. This method requires neither the crushing of larger polycrystalline samples nor any techniques to avoid radiation damage such as cryocooling. Apparatus to record protein powder diffraction in this manner has been commissioned, and in this paper the first powder diffraction patterns from a membrane protein, photosystem I, with crystallite sizes of less than 500 nm are presented. These preliminary patterns show the lowest-order reflections, which agree quantitatively with theoretical calculations of the powder profile. The results also serve to test our aerojet injector system, with future application to femtosecond diffraction in free-electron X-ray laser schemes, and for serial crystallography using a single-file beam of aligned hydrated molecules.

  10. Theoretical study of the properties of X-ray diffraction moiré fringes. I

    International Nuclear Information System (INIS)

    Yoshimura, Jun-ichi

    2015-01-01

    A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory, where the effect of the Pendellösung intensity oscillation on the moiré pattern is explained in detail. A detailed and comprehensive theoretical description of X-ray diffraction moiré fringes for a bicrystal specimen is given on the basis of a calculation by plane-wave dynamical diffraction theory. Firstly, prior to discussing the main subject of the paper, a previous article [Yoshimura (1997 ▸). Acta Cryst. A53, 810–812] on the two-dimensionality of diffraction moiré patterns is restated on a thorough calculation of the moiré interference phase. Then, the properties of moiré fringes derived from the above theory are explained for the case of a plane-wave diffraction image, where the significant effect of Pendellösung intensity oscillation on the moiré pattern when the crystal is strained is described in detail with theoretically simulated moiré images. Although such plane-wave moiré images are not widely observed in a nearly pure form, knowledge of their properties is essential for the understanding of diffraction moiré fringes in general

  11. The experimental search for new predicted binary-alloy structures

    Science.gov (United States)

    Erb, K. C.; Richey, Lauren; Lang, Candace; Campbell, Branton; Hart, Gus

    2010-10-01

    Predicting new ordered phases in metallic alloys is a productive line of inquiry because configurational ordering in an alloy can dramatically alter their useful material properties. One is able to infer the existence of an ordered phase in an alloy using first-principles calculated formation enthalpies.ootnotetextG. L. W. Hart, ``Where are Nature's missing structures?,'' Nature Materials 6 941-945 2007 Using this approach, we have been able to identify stable (i.e. lowest energy) orderings in a variety of binary metallic alloys. Many of these phases have been observed experimentally in the past, though others have not. In pursuit of several of the missing structures, we have characterized potential orderings in PtCd, PtPd and PtMo alloys using synchrotron x-ray powder diffraction and symmetry-analysis tools.ootnotetextB. J. Campbell, H. T. Stokes, D. E. Tanner, and D. M. Hatch, ``ISODISPLACE: a web-based tool for exploring structural distortions,'' J. Appl. Cryst. 39, 607-614 (2006)

  12. 4-Aminobenzoic acid 4-methylpyridine/4-methylpyridinium 4-aminobenzoate 0.58/0.42: a redetermination from the original data

    Directory of Open Access Journals (Sweden)

    Jan Fábry

    2017-10-01

    Full Text Available The title structure, 4-aminobenzoic acid 4-methylpyridine/4-methylpyridinium 4-aminobenzoate 0.58/0.42, 0.58(C6H7N·C7H7NO2·0.42(C6H8N+·C7H6NO2−, has been redetermined from the data published by Kumar et al. (2015. Acta Cryst. E71, o125-o126. The improvement of the present redetermination consists in the introduction of disorder of the methyl group over two positions as well as in the correction of the positional parameters of the hydrogen atoms that are involved in the O—H...N or N—H...O hydrogen bonds. After the correction, the hydroxyl hydrogen atom turned out to be disordered over two positions about the centre of the O...N bond, which is relatively long [2.642 (2 Å], while the H atoms of the primary amine group account more realistically for the hydrogen-bond pattern after the removal of the positional constraints. All the O—H...N or N—H...O hydrogen bonds which are present in the title structure are of moderate strength.

  13. Molecular and crystal structure of gossypol tetramethyl ether with an unknown solvate

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    Muhabbat Honkeldieva

    2015-02-01

    Full Text Available The title compound, C34H38O8 (systematic name: 5,5′-diisopropyl-2,2′,3,3′-tetramethoxy-7,7′-dimethyl-2H,2′H-8,8′-bi[naphtho[1,8-bc]furan]-4,4′-diol, has been obtained from a gossypol solution in a mixture of dimethyl sulfate and methanol. The molecule is situated on a twofold rotation axis, so the asymmetric unit contains one half-molecule. In the molecule, the hydroxy groups are involved in intramolecular O—H...O hydrogen bonds, and the two naphthyl fragments are inclined each to other by 83.8 (1°. In the crystal, weak C—H...O and C—H...π interactions consolidate the packing, which exhibits channels with an approximate diameter of 6 Å extending along the c-axis direction. These channels are filled with highly disordered solvent molecules, so their estimated scattering contribution was subtracted from the observed diffraction data using the SQUEEZE option in PLATON [Spek, A. L. (2015. Acta Cryst. C71, 9–18].

  14. Crystal structure of 2-methylamino-4-(6-methyl-4-oxo-4H-chromen-3-yl-3-nitropyrano[3,2-c]chromen-5(4H-one with an unknown solvate

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    Rajamani Raja

    2015-09-01

    Full Text Available In the title compound, C23H16N2O7, the mean planes of the two chromene units (r.m.s. deviations = 0.031 and 0.064 Å are almost normal to one another with a dihedral angle of 85.59 (6°. The central six-membered pyran ring has a distorted envelope conformation, with the methine C atom at the flap. There is an intramolecular N—H...O hydrogen bond, which generates an S(6 ring motif. In the crystal, molecules are linked by pairs of N—H...O hydrogen bonds, forming inversion dimers with an R22(12 ring motif. The dimers are linked by pairs of C—H...O hydrogen bonds, enclosing R22(6 ring motifs, forming zigzag chains along [001]. The chains are linked by a second pair of C—H...O hydrogen bonds, forming slabs parallel to (110. Within the slabs there are C—H...π interactions present. A region of disordered electron density was treated with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as plausible solvent molecule(s. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s.

  15. Crystal structure of triaqua(2,6-dimethylpyrazine-κN4bis(thiocyanato-κNmanganese(II 2,5-dimethylpyrazine disolvate

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    Stefan Suckert

    2015-12-01

    Full Text Available In the crystal structure of the title complex, [Mn(NCS2(C6H8N2(H2O3]·2C6H8N2, the MnII cation is coordinated by two terminally N-bonded thiocyanate anions, three water molecules and one 2,6-dimethylpyrazine ligand within a slightly distorted N3O3 octahedral geometry; the entire complex molecule is generated by the application of a twofold rotation axis. The asymmetric unit also contains an uncoordinating 2,5-dimethylpyrazine ligand in a general position. Obviously, the coordination to the 2,6-dimethylpyrazine ligand is preferred because coordination to the 2,5-dimethylpyrazine is hindered due to the bulky methyl group proximate to the N atom. The discrete complexes are linked by water-O—H...N(2,6-dimethylpyzazine/2,5-dimethylpyzazine hydrogen bonding, forming a three-dimensional network. In the crystal, molecules are arranged in a way that cavities are formed in which unspecified, disordered solvent molecules reside. These were modelled employing the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18]. The composition of the unit cell does not take into account the presence of the unspecified solvent.

  16. Chlorido(pyridine-κN(5,10,15,20-tetraphenylporphyrinato-κ4Ncobalt(III chloroform hemisolvate

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    Yassin Belghith

    2012-08-01

    Full Text Available In the title complex, [CoCl(C44H28N4(C5H5N]·0.5CHCl3 or [CoIII(TPPCl(py]·0.5CHCl3 (where TPP is the dianion of tetraphenylporphyrin and py is pyridine, the average equatorial cobalt–pyrrole N atom bond length (Co—Np is 1.958 (7 Å and the axial Co—Cl and Co—Npy distances are 2.2339 (6 and 1.9898 (17 Å, respectively. The tetraphenylporphyrinate dianion exhibits an important nonplanar conformation with major ruffling and saddling distortions. In the crystal, molecules are linked via weak C—H...π interactions. In the difference Fourier map, a region of highly disordered electron density was estimated using the SQUEEZE routine [PLATON; Spek (2009, Acta Cryst. D65, 148–155] to be equivalent to one half-molecule of CHCl3 per molecule of the complex.

  17. Tetrakis(μ3-2-{[1,1-bis(hydroxymethyl-2-oxidoethyl]iminomethyl}-6-nitrophenolatotetracopper(II

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    Eduard N. Chygorin

    2014-02-01

    Full Text Available The title cluster, [Cu4(C11H12N2O64], was obtained from the Cu0–FeCl2·4H2O–H4L–Et3N–DMF reaction system (in air, where H4L is 2-hydroxymethyl-2{[(2-hydroxy-3-nitrophenylmethylidene]amino}propane-1,3-diol and DMF is dimethylformamide. The asymmetric unit consists of one Cu2+ ion and one dianionic ligand; a -4 symmetry element generates the cluster, which contains a {Cu4O4} cubane-like core. The metal ion has an elongated square-based pyramidal CuNO4 coordination geometry with the N atom in a basal site. An intramolecular O—H...O hydrogen bond is observed. The solvent molecules were found to be highly disordered and their contribution to the scattering was removed with the SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155], which indicated a solvent cavity of volume 3131 Å3 containing approximately 749 electrons. These solvent molecules are not considered in the given chemical formula.

  18. Crystal structure of an unknown tetrahydrofuran solvate of tetrakis(μ3-cyanato-κ3N:N:Ntetrakis[(triphenylphosphane-κPsilver(I

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    Peter Frenzel

    2015-10-01

    Full Text Available In the title compound, [{[(C6H53P]Ag}4{NCO}4], a distorted Ag4N4-heterocubane core is set up by four AgI ions being coordinated by the N atoms of the cyanato anions in a μ3-bridging mode. In addition, a triphenylphosphine ligand is datively bonded to each of the AgI ions. Intramolecular Ag...Ag distances as short as 3.133 (9 Å suggest the presence of argentophilic (d10...d10 interactions. Five moderate-to-weak C—H...O hydrogen-bonding interactions are observed in the crystal structure, spanning a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as being part of disordered tetrahydrofuran solvent molecules. The given chemical formula and other crystal data do not take into account these solvent molecules.

  19. (RS-Efonidipine acetone hemisolvate

    Directory of Open Access Journals (Sweden)

    Yu-Heng Liu

    2016-09-01

    Full Text Available The asymmetric unit of the title compound, C34H38N3O7P·0.5C3H6O {systematic name: (RS-2-[phenyl(phenylmethylamino]ethyl 5-(5,5-dimethyl-2-oxo-1,3-dioxa-2λ5-phosphacyclohex-2-yl-2,6-dimethyl-4-(3-nitrophenyl-1,4-dihydropyridine-3-carboxylate acetone hemisolvate}, contains one R-efonidipine molecule, one S-efonidipine molecule and half of a solvate acetone molecule. In both efonidipine molecules, the six-membered rings of the dioxaphosphinanyl moieties display a chair conformation and the dihydropyridine rings display a flattened boat conformation. In the crystal, N—H...O, C—H...O hydrogen bonds and weak C—H...π interactions link the molecules into a three-dimensional supramolecular structure. A solvent-accessible void of 199 Å3 is found in the structure; the contribution of the heavily disordered solvate molecule was suppressed by use of the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18].

  20. (4′-Phenyl-2,2′:6′,2′′-terpyridine-κ3N,N′,N′′bis(thiocyanato-κNzinc(II unknown solvate

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    An-ran Wang

    2016-11-01

    Full Text Available The title compound, [Zn(NCS2(C21H15N3], crystallizes with three independent complex molecules in the asymmetric unit. In each complex molecule, the ZnII atom is coordinated by three N atoms of a 4′-phenyl-2,2′:6′,2′′-terpyridine ligand, and by the N atoms of two NCS− anions. The ZnII atoms are therefore five-coordinate, ZnN5, with distorted square-pyramidal geometries. In the crystal, the three independent molecules are linked by a series of offset π–π interactions [intercentroid distances vary between 3.680 (5 and 3.791 (5 Å], forming columns along the a-axis direction. The columns are linked via C—H...S interactions, forming a fence-like arrangement parallel to the ab plane. A small region of disordered electron density was corrected for using the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18], but the formula mass and unit-cell characteristics were not taken into account during the refinement.

  1. Bis(2-amino-1,3-benzothiazole-κN3dichloridozinc(II ethanol hemisolvate

    Directory of Open Access Journals (Sweden)

    Young-Inn Kim

    2012-02-01

    Full Text Available In the title compound, [ZnCl2(C7H6N2S2]·0.5CH3CH2OH, the ZnII atom is coordinated by two N atoms of two 2-aminobenzothiazole ligands and two Cl atoms within a distorted tetrahedral geometry. The dihedral angle between the N/Zn/N and Cl/Zn/Cl planes is 86.22 (7°. The benzothiazole molecules are almost perpendicular to each other, forming a dihedral angle of 80.20 (8°. The molecular structure is stabilized by intramolecular N—H...Cl hydrogen bonds. In the crystal, intermolecular N—H...Cl hydrogen bonds link the molecules into a three-dimensional network. The SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155] was used to model a disordered ethanol solvent molecule; the calculated unit-cell data allow for the presence of half of this molecule in the asymmetric unit.

  2. Crystal structure of 4′-allyl-4,5,6,7,2′,7′-hexachlorofluorescein allyl ester unknown solvate

    Directory of Open Access Journals (Sweden)

    Lili Wang

    2018-01-01

    Full Text Available In the title compound, 4′-allyl-4,5,6,7,2′,7′-hexachlorofluorescein allyl ester {systematic name: prop-2-en-1-yl 2,3,4,5-tetrachloro-6-[2,7-dichloro-6-hydroxy-3-oxo-4-(prop-2-en-1-yl-3H-xanthen-9-yl]benzoate}, C26H14Cl6O5, accompanied by unknown solvate molecules, the dihedral angle between the xanthene ring system (r.m.s. deviation = 0.046 Å and the pentasubstituted benzene ring is 71.67 (9°. Both allyl groups are disordered over two sets of sites in statistical ratios. The scattering contributions of the disordered solvent molecules (both Ph2O and CHCl3, as identified by NMR were removed with the PLATON SQUEEZE algorithm [Spek (2015. Acta Cryst. C71, 9–18]. In the crystal, tetrameric supramolecular aggregates linked by O—H...O hydrogen bonds occur; these further interact with neighboring aggregates through C—Cl...π interactions arising from the benzene rings, forming infinite two-dimensional sheets. Each C6Cl4 ring shifts in the direction perpendicular to the two-dimensional sheet, exhibiting a helical chain in which every C6Cl4 ring is utilized as both a donor and an acceptor of Cl...π contacts. Thus, these two-dimensional sheets pack in a helical fashion, constructing a three-dimensional network.

  3. (Acetonitrile{2-[bis(pyridin-2-ylmethyl-κ2Namino-κN]-N-(2,6-dimethylphenylacetamide-κO}(perchlorato-κOzinc (acetonitrile{2-[bis(pyridin-2-ylmethyl-κ2Namino-κN]-N-(2,6-dimethylphenylacetamide-κO}zinc tris(perchlorate

    Directory of Open Access Journals (Sweden)

    Ove Alexander Høgmoen Åstrand

    2013-02-01

    Full Text Available In the title salt, [Zn(C22H24N4O(CH3CN][Zn(ClO4(C22H24N4O(CH3CN](ClO43, two differently coordinated zinc cations occur. In the first complex, the metal ion is coordinated by the N,N′,N′′,O-tetradentate acetamide ligand and an acetonitrile N atom, generating an approximate trigonal–bipyramidal coordination geometry, with the O atom in an equatorial site and the acetonitrile N atom in an axial site. In the second complex ion, a perchlorate ion is also bonded to the zinc ion, generating a distorted trans-ZnO2N4 octahedron. Of the uncoordinating perchlorate ions, one lies on a crystallographic twofold axis and one lies close to a twofold axis and has a site occupancy of 0.5. N—H...O and N—H...(O,O hydrogen bonds are observed in the crystal. Disordered solvent molecules occupy about 11% of the unit-cell volume; their contribution to the scattering was removed with the SQUEEZE routine of the PLATON program [Spek (2009. Acta Cryst. D65, 148–155.].

  4. Crystal structure of an unknown solvate of bis(tetra-n-butylammonium [N,N′-(4-trifluoromethyl-1,2-phenylenebis(oxamato-κ4O,N,N′,O′]nickelate(II

    Directory of Open Access Journals (Sweden)

    François Eya'ane Meva

    2015-06-01

    Full Text Available In the title compound, [N(C4H94]2[Ni(C11H3F3N2O6] or [N(n-Bu4]2[Ni(topbo] [n-Bu = n-butyl and topbo = 4-trifluoromethyl-1,2-phenylenebis(oxamate], the Ni2+ cation is coordinated by two deprotonated amido N atoms and two carboxylate O atoms, setting up a slightly distorted square-planar coordination environment. The [Ni(topbo]2− anion lies on a twofold rotation axis. Due to an incompatibility with the point-group symmetry of the complete molecule, orientational disorder of the CF3 group is observed. The tetrahedral ammonium cations and the anion are linked by weak intermolecular C—H...O and C—H...F hydrogen-bonding interactions into a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as plausible solvent molecule(s. The given chemical formula and other crystal data do not take into account the unknown solvent molecule.

  5. V1.42In1.83Mo15Se19

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    Michel Potel

    2010-10-01

    Full Text Available The structure of the title compound, vanadium indium pentadecamolybdenum nonadecaselenide, V1.42In1.83Mo15Se19, is isotypic with In2.9Mo15Se19 [Grüttner et al. (1979. Acta Cryst. B35, 285–292]. It is characterized by two cluster units Mo6Sei8Sea6 and Mo9Sei11Sea6 (where i represents inner and a apical atoms that are present in a 1:1 ratio. The cluster units are centered at Wyckoff positions 2b and 2c and have point-group symmetry overline{3} and overline{6}, respectively. The clusters are interconnected through additional Mo—Se bonds. In the title compound, the V3+ cations replace the trivalent indium atoms present in In2.9Mo15Se19, and a deficiency is observed on the monovalent indium site. One Mo, one Se and the V atom are situated on mirror planes, and two other Se atoms and the In atom are situated on threefold rotation axes.

  6. Thermodynamic properties of the Pd77.5Cu6Si16.5 undercooled liquid

    International Nuclear Information System (INIS)

    Fiore, Gianluca; Battezzati, Livio

    2009-01-01

    Proper understanding of glass formation implies the knowledge of the thermodynamics of the undercooled melts. Specifically, high values of the excess specific heat of the liquid are expected for good glass-formers. Extending the work of Gillessen and Herlach [F. Gillessen, D.M. Herlach, J. Non-Cryst. Solids 117-118 (1990) 555-558], we re-propose a calculation of the temperature dependence of entropy difference between amorphous-liquid and crystal states. An amorphous Pd 77.5 Cu 6 Si 16.5 alloy has been produced by injection casting in a cylindrical copper mould. DSC measurements in the liquid, amorphous and crystalline states were performed with samples sliced from the cylinder to determine the heat of fusion, of crystallization and the difference in specific heat capacity between amorphous-liquid and crystal phases. These thermodynamic quantities are used to calculate the thermodynamic functions of the liquid-glass with reference to the equilibrium crystal mixture. The data are compared to those of other bulk glass-formers in terms of fragility plots.

  7. Structure of thallium and lead calculated from Shaw local pseudopotential and molecular dynamics

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    Gasser J. G.

    2011-05-01

    Full Text Available Recently, we (Es Sbihi Phil. Mag 2010 have successfully calculated, by molecular dynamics, the static structure factor of liquid bismuth at different temperatures. Our results were in very good agreement with the Waseda experimental data. Our assumption was to consider the true density of states which presents a gap as measured by Indlekofer (J. Non-Cryst. Solids 1989 and calculated by Hafner-Jank (Phys. Rev. B 1990 for liquid bismuth. The number of electrons at the Fermi energy has been calculated with three conduction electrons for bismuth (number of p electrons. With this assumption, the structures were determined with an effective ion-ion potential constructed from the Shaw local Optimised Model Potential (OMP and the Ichimaru-Utsumi dielectric function. In the present paper, we generalize our assumptions to liquid thallium and lead which also present such a gap. Their calculated structures are also very close to the experimental ones. This confirms that the number of conduction electrons on the Fermi sphere is consistent with the number of p electrons as has been even shown for our electronic transport properties of liquid lead (A. Ben Abdellah, Phys. Rev. B 2003.

  8. Role of Steric Hindrance in the Crystal Packing of Z′ = 4 Superstructure of Trimethyltin Hydroxide

    KAUST Repository

    Dey, S.

    2018-01-22

    The roomerature crystal structure of trimethyltin hydroxide, (CH)SnOH, has been described by Anderson et al. [Cryst. Growth Des. 2011, 11, 820-826] as a 2a × 2b × 8c, 32-fold superstructure. We report a a × b × 8c, eight-fold superstructure with orthorhombic P2cn symmetry and Z′ = 4. Structured diffuse scattering observed at the positions of presumed superlattice reflections along a∗ and b∗ might have appeared as Bragg reflections in the experiment by Anderson et al. Alternatively, Anderson et al. and the present work might have studied different polymorphs of (CH)SnOH. Crystalline (CH)SnOH constitutes polymeric chains arranged parallel to c. In the eight-fold superstructure at 220 K, the polymeric chains possess a distorted zigzag arrangement of linked linear O-Sn-O units with bent angle at oxygen of ∼139.2°. This structure is essentially different from the 8-helical arrangement in the published 32-fold superstructure model. The origin of the distorted zigzag structure is explained by steric hindrance between hydrogen atoms of adjacent hydroxy groups and (CH)Sn groups. Frustration in the packing of the chains is determined by steric hindrance between methyl groups of neighboring chains, which prevents the formation of interchain C-H···O hydrogen bonds.

  9. Crystal structure of bis(azido-κNbis[2,5-bis(pyridin-2-yl-1,3,4-thiadiazole-κ2N2,N3]cobalt(II

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    Abdelhakim Laachir

    2015-05-01

    Full Text Available In the mononuclear title complex, [Co(N32(C12H8N4S2], the cobalt(II atom is located on an inversion centre and displays an axially weakly compressed octahedral coordination geometry. The equatorial positions are occupied by the N atoms of two 2,5-bis(pyridin-2-yl-1,3,4-thiadiazole ligands, whereas the axial positions are occupied by N atoms of the azide anions. The thiadiazole and pyridine rings linked to the metal are almost coplanar, with a maximum deviation from the mean plane of 0.0273 (16 Å. The cohesion of the crystal is ensured by weak C—H...N hydrogen bonds and by π–π interactions between pyridine rings [intercentroid distance = 3.6356 (11 Å], forming a layered arrangement parallel to (001. The structure of the title compound is isotypic with that of the analogous nickel(II complex [Laachir et al. (2013. Acta Cryst. E69, m351–m352].

  10. Poly[di-μ2-acetato-κ4O:O′-μ3-thiourea-κ3S:S:S-lead(II]: a redetermination

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    Hafid Zouihri

    2016-12-01

    Full Text Available The structure of the title polymeric lead(II thiourea complex, [Pb(CH3O2{SC(NH22}]n, has been redetermined at significantly higher precision using diffractometer data at 100 K. The previous determination used data obtained from multiple-film integrated Weissenberg photographs [Nardelli et al. (1960. Acta Cryst. 13, 898–904]. The main difference between the two models is in the precision of the bond lengths, angles and cell parameters. In the crystal, the eight-coordinate PbII atom is chelated by two carboxylate groups and bridged by three S atoms from thiourea ligands. The coordination sphere is completed by an O atom from a third carboxylate group, the second O atom of which binds to a neighbouring PbII atom, forming a polymeric chain that runs the a axis. Two of these chains are related by centres of symmetry. Intermolecular hydrogen bonds connect neighbouring chains to one another, generating a three-dimensional network.

  11. WinPSSP : a revamp of the computer program PSSP and its performance solving the crystal structures of small organic compounds and solids of biological and pharmaceutical interest

    Energy Technology Data Exchange (ETDEWEB)

    Pagola, Silvina; Polymeros, Alekos; Kourkoumelis, Nikolaos

    2017-02-01

    The direct-space methods softwarePowder Structure Solution Program(PSSP) [Pagola & Stephens (2010).J. Appl. Cryst.43, 370–376] has been migrated to the Windows OS and the code has been optimized for fast runs.WinPSSPis a user-friendly graphical user interface that allows the input of preliminary crystal structure information, integrated intensities of the reflections and FWHM, the definition of structural parameters and a simulated annealing schedule, and the visualization of the calculated and experimental diffraction data overlaid for each individual solution. The solutions are reported as filename.cif files, which can be used to analyze packing motifs and chemical bonding, and to input the atomic coordinates into the Rietveld analysis softwareGSAS. WinPSSPperformance in straightforward crystal structure determinations has been evaluated using 18 molecular solids with 6–20 degrees of freedom. The free-distribution program as well as multimedia tutorials can be accessed at http://users.uoi.gr/nkourkou/winpssp/.

  12. Molecular architecture of the nucleoprotein C-terminal domain from the Ebola and Marburg viruses.

    Science.gov (United States)

    Baker, Laura E; Ellena, Jeffrey F; Handing, Katarzyna B; Derewenda, Urszula; Utepbergenov, Darkhan; Engel, Daniel A; Derewenda, Zygmunt S

    2016-01-01

    The Filoviridae family of negative-sense, single-stranded RNA (ssRNA) viruses is comprised of two species of Marburgvirus (MARV and RAVV) and five species of Ebolavirus, i.e. Zaire (EBOV), Reston (RESTV), Sudan (SUDV), Taï Forest (TAFV) and Bundibugyo (BDBV). In each of these viruses the ssRNA encodes seven distinct proteins. One of them, the nucleoprotein (NP), is the most abundant viral protein in the infected cell and within the viral nucleocapsid. It is tightly associated with the viral RNA in the nucleocapsid, and during the lifecycle of the virus is essential for transcription, RNA replication, genome packaging and nucleocapsid assembly prior to membrane encapsulation. The structure of the unique C-terminal globular domain of the NP from EBOV has recently been determined and shown to be structurally unrelated to any other known protein [Dziubańska et al. (2014), Acta Cryst. D70, 2420-2429]. In this paper, a study of the C-terminal domains from the NP from the remaining four species of Ebolavirus, as well as from the MARV strain of Marburgvirus, is reported. As expected, the crystal structures of the BDBV and TAFV proteins show high structural similarity to that from EBOV, while the MARV protein behaves like a molten globule with a core residual structure that is significantly different from that of the EBOV protein.

  13. Dynamic quantum crystallography: lattice-dynamical models refined against diffraction data. II. Applications to L-alanine, naphthalene and xylitol.

    Science.gov (United States)

    Hoser, Anna A; Madsen, Anders Ø

    2017-03-01

    In the first paper of this series [Hoser & Madsen (2016). Acta Cryst. A72, 206-214], a new approach was introduced which enables the refinement of frequencies of normal modes obtained from ab initio periodic computations against single-crystal diffraction data. In this contribution, the performance of this approach is tested by refinement against data in the temperature range from 23 to 205 K on the molecular crystals of L-alanine, naphthalene and xylitol. The models, which are lattice-dynamical models derived at the Γ point of the Brillouin zone, are able to describe the atomic vibrations of L-alanine and naphthalene to a level where the residual densities are similar to those obtained from the independent atom model. For the more flexible molecule xylitol, larger deviations are found. Hydrogen ADPs (anisotropic displacement parameters) derived from the models are in similar or better agreement with neutron diffraction results than ADPs obtained by other procedures. The heat capacity calculated after normal mode refinement for naphthalene is in reasonable agreement with the heat capacity obtained from calorimetric measurements (to less than 1 cal mol -1  K -1 below 300 K), with deviations at higher temperatures indicating anharmonicity. Standard uncertainties and correlation of the refined parameters have been derived based on a Monte Carlo procedure. The uncertainties are quite small and probably underestimated.

  14. Difference in the structures of alanine tri- and tetra-peptides with antiparallel β-sheet assessed by X-ray diffraction, solid-state NMR and chemical shift calculations by GIPAW.

    Science.gov (United States)

    Asakura, Tetsuo; Yazawa, Koji; Horiguchi, Kumiko; Suzuki, Furitsu; Nishiyama, Yusuke; Nishimura, Katsuyuki; Kaji, Hironori

    2014-01-01

    Alanine oligomers provide a key structure for silk fibers from spider and wild silkworms.We report on structural analysis of L-alanyl-L-alanyl-L-alanyl-L-alanine (Ala)4 with anti-parallel (AP) β-structures using X-ray and solid-state NMR. All of the Ala residues in the (Ala)4 are in equivalent positions, whereas for alanine trimer (Ala)3 there are two alternative locations in a unit cell as reported previously (Fawcett and Camerman, Acta Cryst., 1975, 31, 658-665). (Ala)4 with AP β-structure is more stable than AP-(Ala)3 due to formation of the stronger hydrogen bonds. The intermolecular structure of (Ala)4 is also different from polyalanine fiber structure, indicating that the interchain arrangement of AP β-structure changes with increasing alanine sequencelength. Furthermore the precise (1)H positions, which are usually inaccesible by X-ray diffraction method, are determined by high resolution (1)H solid state NMR combined with the chemical shift calculations by the gauge-including projector augmented wave method. Copyright © 2013 Wiley Periodicals, Inc.

  15. (4,4′-Dimethoxy-2,2′-bipyridine-κ2N,N′bis[2-(pyridin-2-ylphenyl-κC1]iridium(III hexafluoridophosphate unknown solvate

    Directory of Open Access Journals (Sweden)

    Yano Natsumi

    2016-03-01

    Full Text Available The asymmetric unit of the title complex, [Ir(C11H8N2(C12H12N2O2]PF6, comprises a [Ir(ppy2(diMeO-bpy]+ cation (Hppy = 2-phenylpyridine and diMeO-bpy = 4,4′-dimethoxy-2,2′-bipyridine and a PF6− anion. The IrIII atom is coordinated by two anionic ppy− ligands, each coordinating in a C^N cyclometalated mode, and one neutral diMeO-bpy ligand, leading to a distorted octahedral geometry defined by a cis-C2N4 donor set. Intermolecular C—F...H contacts lead to a three-dimensional architecture that define columns parallel to a. Unknown disordered solvent molecules reside in these columns with the electron density being treated with SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18]. The unit-cell data do not reflect the presence of the unresolved solvent.

  16. Poly[μ-aqua-diaqua(μ2-pyrazine-2,3-dicarboxylatodilithium(I

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    Kutalmis Guven

    2009-12-01

    Full Text Available The asymmetric unit of the title compound, [Li2(C6H2N2O4(H2O3]n, consists of two independent Li+ cations, one pyrazine-2,3-dicarboxylate dianion and three water molecules. One of the Li+ cations has a distorted tetrahedral geometry, coordinated by one of the carboxylate O atoms of the pyrazine-2,3-dicarboxylate ligand and three O atoms from three water molecules, whereas the other Li+ cation has a distorted trigonal-bipyramidal geometry, coordinated by a carboxylate O atom of a symmetry-related pyrazine-2,3-dicarboxylate ligand, two water molecules and a chelating pyrazine-2,3-dicarboxylate ligand (by utilizing both N and O atoms of an adjacent molecule. The synthesis of a hydrated polymeric dinuclear lithium complex formed with two pyrazine-2,3-dicarboxylic acid ligands has been reported previously [Tombul et al. (2008a. Acta Cryst. E64, m491–m492]. By comparision to the complex reported here, the dinuclear complex formed with two pyrazine-2,3-dicarboxylic acid ligands differs in the coordination geometry of both Li atoms. The crystal structure further features O—H...O and O—H...N hydrogen-bonding interactions involving the water molecules and carboxylate O atoms.

  17. p-type doping efficiency in CdTe: Influence of second phase formation

    Science.gov (United States)

    McCoy, Jedidiah J.; Swain, Santosh K.; Sieber, John R.; Diercks, David R.; Gorman, Brian P.; Lynn, Kelvin G.

    2018-04-01

    Cadmium telluride (CdTe) high purity, bulk, crystal ingots doped with phosphorus were grown by the vertical Bridgman melt growth technique to understand and improve dopant solubility and activation. Large net carrier densities have been reproducibly obtained from as-grown ingots, indicating successful incorporation of dopants into the lattice. However, net carrier density values are orders of magnitude lower than the solubility of P in CdTe as reported in literature, 1018/cm3 to 1019/cm3 [J. H. Greenberg, J. Cryst. Growth 161, 1-11 (1996) and R. B. Hall and H. H. Woodbury, J. Appl. Phys. 39(12), 5361-5365 (1968)], despite comparable starting charge dopant densities. Growth conditions, such as melt stoichiometry and post growth cooling, are shown to have significant impacts on dopant solubility. This study demonstrates that a significant portion of the dopant becomes incorporated into second phase defects as compounds of cadmium and phosphorous, such as cadmium phosphide, which inhibits dopant incorporation into the lattice and limits maximum attainable net carrier density in bulk crystals. Here, we present an extensive study on the characteristics of these second phase defects in relation to their composition and formation kinetics while providing a pathway to minimize their formation and enhance solubility.

  18. Evaluation of macromolecular electron-density map quality using the correlation of local r.m.s. density

    International Nuclear Information System (INIS)

    Terwilliger, Thomas C.; Berendzen, Joel

    1999-01-01

    The correlation of local r.m.s. density is shown to be a good measure of the presence of distinct solvent and macromolecule regions in macromolecular electron-density maps. It has recently been shown that the standard deviation of local r.m.s. electron density is a good indicator of the presence of distinct regions of solvent and protein in macromolecular electron-density maps [Terwilliger & Berendzen (1999 ▶). Acta Cryst. D55, 501–505]. Here, it is demonstrated that a complementary measure, the correlation of local r.m.s. density in adjacent regions on the unit cell, is also a good measure of the presence of distinct solvent and protein regions. The correlation of local r.m.s. density is essentially a measure of how contiguous the solvent (and protein) regions are in the electron-density map. This statistic can be calculated in real space or in reciprocal space and has potential uses in evaluation of heavy-atom solutions in the MIR and MAD methods as well as for evaluation of trial phase sets in ab initio phasing procedures

  19. A new crystal modification of diammonium hydrogen phosphate, (NH42(HPO4

    Directory of Open Access Journals (Sweden)

    Bernhard Spingler

    2010-04-01

    Full Text Available The addition of hexafluoridophosphate salts (ammonium, silver, thallium or potassium is usually used to precipitate complex cations from aqueous solutions. It has long been known that PF6− is sensitive towards hydrolysis under acidic conditions [Gebala & Jones (1969. J. Inorg. Nucl. Chem. 31, 771–776; Plakhotnyk et al. (2005. J. Fluorine Chem. 126, 27–31]. During the course of our investigation into coinage metal complexes of diphosphine ligands, we used ammonium hexafluoridophosphate in order to crystallize [Ag(diphosphine2]PF6 complexes. From these solutions we always obtained needle-like crystals which turned out to be the title compound, 2NH4+·HPO42−. It was received as the hydrolysis product of NH4PF6. The crystals are a new modification of diammonium hydrogen phosphate. In contrast to the previously published polymorph [Khan et al. (1972. Acta Cryst. B28, 2065–2069], Z′ of the title compound is 2. In the new modification of the title compound, there are eight molecules of (NH42(HPO4 in the unit cell. The structure consists of PO3OH and NH4 tetrahedra, held together by O—H...O and N—H...O hydrogen bonds.

  20. High-resolution mapping of two-dimensional lattice distortions in ion-implanted crystals from X-ray diffractometry data

    International Nuclear Information System (INIS)

    Nikulin, A.Y.; Gureyev, T.E.; Stevenson, A.W.; Wilkins, S.W.; Hashizume, H.; Cookson, D.

    1996-01-01

    The triple-crystal synchrotron X-ray diffractometry data described in Nikulin, Stevenson, Hashizume, Wilkins, Foran, Cookson and Garrett (J. Appl. Cryst. 28, 57-60 (1995)) has been analyzed to map out two-dimensional (2D) lattice distortions in silicon (111) crystals implanted with B + ions of 100 keV energy through a periodic SiO 2 strip pattern. The lateral periodic structure produced a series of satellite reflections associated with the 111 Bragg peak. The 2D reconstruction incorporates the use of the Petrashen-Chukhovskii method, which retrieves the phases of the Bragg waves for these satellite reflections, together with that for the fundamental. The finite Fourier series is then synthesized with the relative phases determined. Localized distortions perpendicular to the surface arising from deposited B + ions in near-surface layers of the crystal are clearly displayed with spatial resolutions of 0.016 and 0.265 μm in the depth and lateral directions respectively. For a sample with the oxide layer removed from the surface, two equally plausible strain maps have been obtained by assigning relative phases to eleven satellites using a sequential trial method and a minimum-energy method. Failed map reconstructions for the oxide-covered sample are discussed in terms of the non-unique solutions of the Petrashen-Chukhovskii phase-recovery algorithm and the ambiguous phases determined for the satellites. 16 refs., 8 figs

  1. Large and high-quality single-crystal growth of cuprate superconductor Bi-2223 using the traveling-solvent floating-zone (TSFZ) method

    Science.gov (United States)

    Adachi, Shintaro; Usui, Tomohiro; Kosugi, Kenta; Sasaki, Nae; Sato, Kentaro; Fujita, Masaki; Yamada, Kazuyoshi; Fujii, Takenori; Watanabe, Takao

    In high superconducting transition temperature (high-Tc) cuprates, it is empirically known that Tc increases on increasing the number of CuO2 planes in a unit cell n from 1 to 3. Bi-family cuprates are ideal for investigating the microscopic mechanism involved. However, it is difficult to grow tri-layered Bi-2223, probably owing to its narrow crystallization field. Here, we report improved crystal growth of this compound using the TSFZ method under conditions slightly different from those in an earlier report [J. Cryst. Growth 223, 175 (2001)]. A Bi-rich feed-rod composition of Bi2.2Sr1.9Ca2Cu3Oy and a slightly oxygen-reduced atmosphere (mixed gas flow of O2 (10%) and Ar (90%)) were adopted for the crystal growth. In addition, to increase the supersaturation of the melts, we applied a large temperature gradient along the solid-liquid interface by shielding a high-angle light beam using Al foil around the quartz tube. In this way, we succeeded in preparing large (2 × 2 × 0 . 05 mm3) and high-quality (almost 100% pure) Bi-2223 single crystals. Hirosaki University Grant for Exploratory Research by Young Scientists and Newly-appointed Scientists.

  2. Rapid automated superposition of shapes and macromolecular models using spherical harmonics.

    Science.gov (United States)

    Konarev, Petr V; Petoukhov, Maxim V; Svergun, Dmitri I

    2016-06-01

    A rapid algorithm to superimpose macromolecular models in Fourier space is proposed and implemented ( SUPALM ). The method uses a normalized integrated cross-term of the scattering amplitudes as a proximity measure between two three-dimensional objects. The reciprocal-space algorithm allows for direct matching of heterogeneous objects including high- and low-resolution models represented by atomic coordinates, beads or dummy residue chains as well as electron microscopy density maps and inhomogeneous multi-phase models ( e.g. of protein-nucleic acid complexes). Using spherical harmonics for the computation of the amplitudes, the method is up to an order of magnitude faster than the real-space algorithm implemented in SUPCOMB by Kozin & Svergun [ J. Appl. Cryst. (2001 ▸), 34 , 33-41]. The utility of the new method is demonstrated in a number of test cases and compared with the results of SUPCOMB . The spherical harmonics algorithm is best suited for low-resolution shape models, e.g . those provided by solution scattering experiments, but also facilitates a rapid cross-validation against structural models obtained by other methods.

  3. On the application of the expected log-likelihood gain to decision making in molecular replacement.

    Science.gov (United States)

    Oeffner, Robert D; Afonine, Pavel V; Millán, Claudia; Sammito, Massimo; Usón, Isabel; Read, Randy J; McCoy, Airlie J

    2018-04-01

    Molecular-replacement phasing of macromolecular crystal structures is often fast, but if a molecular-replacement solution is not immediately obtained the crystallographer must judge whether to pursue molecular replacement or to attempt experimental phasing as the quickest path to structure solution. The introduction of the expected log-likelihood gain [eLLG; McCoy et al. (2017), Proc. Natl Acad. Sci. USA, 114, 3637-3641] has given the crystallographer a powerful new tool to aid in making this decision. The eLLG is the log-likelihood gain on intensity [LLGI; Read & McCoy (2016), Acta Cryst. D72, 375-387] expected from a correctly placed model. It is calculated as a sum over the reflections of a function dependent on the fraction of the scattering for which the model accounts, the estimated model coordinate error and the measurement errors in the data. It is shown how the eLLG may be used to answer the question `can I solve my structure by molecular replacement?'. However, this is only the most obvious of the applications of the eLLG. It is also discussed how the eLLG may be used to determine the search order and minimal data requirements for obtaining a molecular-replacement solution using a given model, and for decision making in fragment-based molecular replacement, single-atom molecular replacement and likelihood-guided model pruning.

  4. 4-(3-Chlorophenyl-1-(3-chloropropylpiperazin-1-ium chloride redetermined at 100 K

    Directory of Open Access Journals (Sweden)

    Muzzaffar Ahmad Bhat

    2016-02-01

    Full Text Available The crystal structure of the title salt, C13H19Cl2N2+·Cl−, has been reported previously [Homrighausen & Krause Bauer (2002. Acta Cryst. E58, o1395–o1396] based on room-temperature data, where it was found to contain a disordered chloropropyl group. We now present the structure at 100 K in which the chloropropyl group is ordered. The piperazine ring adopts a chair conformation with the exocyclic N—C bonds in equatorial orientations. The dihedral angle between the piperazine ring (all atoms and the benzene ring is 28.47 (5°. The chloropropyl group has an extended conformation [N—C—C—C = −177.25 (8 ° and C—C—C—Cl = 174.23 (7°]. In the crystal, charge-assisted N—H...Cl hydrogen bonds link the cation and anion into ion pairs. Numerous weak C—H...Cl interactions link the ion pairs into a three-dimensional network. Short Cl...Cl contacts [3.2419 (4 Å] are also observed.

  5. Crystal structure of a new monoclinic polymorph of N-(4-methylphenyl-3-nitropyridin-2-amine

    Directory of Open Access Journals (Sweden)

    Aina Mardia Akhmad Aznan

    2014-08-01

    Full Text Available The title compound, C12H11N3O2, is a second monoclinic polymorph (P21, with Z′ = 4 of the previously reported monoclinic (P21/c, with Z′ = 2 form [Akhmad Aznan et al. (2010. Acta Cryst. E66, o2400]. Four independent molecules comprise the asymmetric unit, which have the common features of a syn disposition of the pyridine N atom and the toluene ring, and an intramolecular amine–nitro N—H...O hydrogen bond. The differences between molecules relate to the dihedral angles between the rings which range from 2.92 (19 to 26.24 (19°. The geometry-optimized structure [B3LYP level of theory and 6–311 g+(d,p basis set] has the same features except that the entire molecule is planar. In the crystal, the three-dimensional architecture is consolidated by a combination of C—H...O, C—H...π, nitro-N—O...π and π–π interactions [inter-centroid distances = 3.649 (2–3.916 (2 Å].

  6. Crystal structure of a new monoclinic polymorph of N-(4-methyl-phen-yl)-3-nitro-pyridin-2-amine.

    Science.gov (United States)

    Aznan, Aina Mardia Akhmad; Abdullah, Zanariah; Lee, Vannajan Sanghiran; Tiekink, Edward R T

    2014-08-01

    The title compound, C12H11N3O2, is a second monoclinic polymorph (P21, with Z' = 4) of the previously reported monoclinic (P21/c, with Z' = 2) form [Akhmad Aznan et al. (2010 ▶). Acta Cryst. E66, o2400]. Four independent mol-ecules comprise the asymmetric unit, which have the common features of a syn disposition of the pyridine N atom and the toluene ring, and an intra-molecular amine-nitro N-H⋯O hydrogen bond. The differences between mol-ecules relate to the dihedral angles between the rings which range from 2.92 (19) to 26.24 (19)°. The geometry-optimized structure [B3LYP level of theory and 6-311 g+(d,p) basis set] has the same features except that the entire mol-ecule is planar. In the crystal, the three-dimensional architecture is consolidated by a combination of C-H⋯O, C-H⋯π, nitro-N-O⋯π and π-π inter-actions [inter-centroid distances = 3.649 (2)-3.916 (2) Å].

  7. Brillouin-zone database on the Bilbao Crystallographic Server.

    Science.gov (United States)

    Aroyo, Mois I; Orobengoa, Danel; de la Flor, Gemma; Tasci, Emre S; Perez-Mato, J Manuel; Wondratschek, Hans

    2014-03-01

    The Brillouin-zone database of the Bilbao Crystallographic Server (http://www.cryst.ehu.es) offers k-vector tables and figures which form the background of a classification of the irreducible representations of all 230 space groups. The symmetry properties of the wavevectors are described by the so-called reciprocal-space groups and this classification scheme is compared with the classification of Cracknell et al. [Kronecker Product Tables, Vol. 1, General Introduction and Tables of Irreducible Representations of Space Groups (1979). New York: IFI/Plenum]. The compilation provides a solution to the problems of uniqueness and completeness of space-group representations by specifying the independent parameter ranges of general and special k vectors. Guides to the k-vector tables and figures explain the content and arrangement of the data. Recent improvements and modifications of the Brillouin-zone database, including new tables and figures for the trigonal, hexagonal and monoclinic space groups, are discussed in detail and illustrated by several examples.

  8. On the correlation between hydrogen bonding and melting points in the inositols

    Directory of Open Access Journals (Sweden)

    Sándor L. Bekö

    2014-01-01

    Full Text Available Inositol, 1,2,3,4,5,6-hexahydroxycyclohexane, exists in nine stereoisomers with different crystal structures and melting points. In a previous paper on the relationship between the melting points of the inositols and the hydrogen-bonding patterns in their crystal structures [Simperler et al. (2006. CrystEngComm 8, 589], it was noted that although all inositol crystal structures known at that time contained 12 hydrogen bonds per molecule, their melting points span a large range of about 170 °C. Our preliminary investigations suggested that the highest melting point must be corrected for the effect of molecular symmetry, and that the three lowest melting points may need to be revised. This prompted a full investigation, with additional experiments on six of the nine inositols. Thirteen new phases were discovered; for all of these their crystal structures were examined. The crystal structures of eight ordered phases could be determined, of which seven were obtained from laboratory X-ray powder diffraction data. Five additional phases turned out to be rotator phases and only their unit cells could be determined. Two previously unknown melting points were measured, as well as most enthalpies of melting. Several previously reported melting points were shown to be solid-to-solid phase transitions or decomposition points. Our experiments have revealed a complex picture of phases, rotator phases and phase transitions, in which a simple correlation between melting points and hydrogen-bonding patterns is not feasible.

  9. Development of a new micro-furnace for "in situ" high-temperature single crystal X-ray diffraction measurements

    Science.gov (United States)

    Alvaro, Matteo; Angel, Ross J.; Marciano, Claudio; Zaffiro, Gabriele; Scandolo, Lorenzo; Mazzucchelli, Mattia L.; Milani, Sula; Rustioni, Greta; Domeneghetti, Chiara M.; Nestola, Fabrizio

    2015-04-01

    -position method (King and Finger 1979), and thus maximize precision in unit-cell parameter measurements. The software has been modified to restrict the χ circle movements to between -90° and +90° to reduce chimney effects in the furnace and thus improve stability. Moreover, the temperature stability during the measurements is further improved by optimizing the order of measurements to minimize χ circle movements, and then imposing a waiting time after large angular movements on χ to allow the temperature inside the furnace to re-equilibrate before each measurement. Temperature calibration has been performed iteratively by combining measurements with a standard small diameter thermocouple mounted in the same conditions as the sample together with the lattice parameter determination of materials with known thermal expansion behavior (i.e. silicon, quartz etc…). This procedure has the main advantage that the temperature calibration can obtained with a large number of measurements over a large temperature interval (room-T to 1200°C) and allows the waiting time for the χ movements to be calibrated as a function of temperature. References Angel RJ, Finger LW (2011) JAppCryst, 44:247-251. King HE, Finger LW (1979) JAppCryst,12:374-378

  10. FlexED8: the first member of a fast and flexible sample-changer family for macromolecular crystallography.

    Science.gov (United States)

    Papp, Gergely; Felisaz, Franck; Sorez, Clement; Lopez-Marrero, Marcos; Janocha, Robert; Manjasetty, Babu; Gobbo, Alexandre; Belrhali, Hassan; Bowler, Matthew W; Cipriani, Florent

    2017-10-01

    Automated sample changers are now standard equipment for modern macromolecular crystallography synchrotron beamlines. Nevertheless, most are only compatible with a single type of sample holder and puck. Recent work aimed at reducing sample-handling efforts and crystal-alignment times at beamlines has resulted in a new generation of compact and precise sample holders for cryocrystallography: miniSPINE and NewPin [see the companion paper by Papp et al. (2017, Acta Cryst., D73, 829-840)]. With full data collection now possible within seconds at most advanced beamlines, and future fourth-generation synchrotron sources promising to extract data in a few tens of milliseconds, the time taken to mount and centre a sample is rate-limiting. In this context, a versatile and fast sample changer, FlexED8, has been developed that is compatible with the highly successful SPINE sample holder and with the miniSPINE and NewPin sample holders. Based on a six-axis industrial robot, FlexED8 is equipped with a tool changer and includes a novel open sample-storage dewar with a built-in ice-filtering system. With seven versatile puck slots, it can hold up to 112 SPINE sample holders in uni-pucks, or 252 miniSPINE or NewPin sample holders, with 36 samples per puck. Additionally, a double gripper, compatible with the SPINE sample holders and uni-pucks, allows a reduction in the sample-exchange time from 40 s, the typical time with a standard single gripper, to less than 5 s. Computer vision-based sample-transfer monitoring, sophisticated error handling and automatic error-recovery procedures ensure high reliability. The FlexED8 sample changer has been successfully tested under real conditions on a beamline.

  11. Crystal structure of the disintegrin heterodimer from saw-scaled viper (Echis carinatus) at 1.9 A resolution.

    Science.gov (United States)

    Bilgrami, Sameeta; Yadav, Savita; Kaur, Punit; Sharma, Sujata; Perbandt, Markus; Betzel, Christian; Singh, Tej P

    2005-08-23

    Disintegrins constitute a family of potent polypeptide inhibitors of integrins. Integrins are transmembrane heterodimeric molecules involved in cell-cell and cell-extracellular matrix interactions. They are involved in many diseases such as cancer and thrombosis. Thus, disintegrins have a great potential as anticancer and antithrombotic agents. A novel heterodimeric disintegrin was isolated from the venom of saw-scaled viper (Echis carinatus) and was crystallized. The crystals diffracted to 1.9 A resolution and belonged to space group P4(3)2(1)2. The data indicated the presence of a pseudosymmetry. The structure was solved by applying origin shifts to the disintegrin homodimer schistatin solved in space group I4(1)22 with similar cell dimensions. The structure refined to the final R(cryst)/R(free) factors of 0.213/0.253. The notable differences are observed between the loops, (Gln39-Asp48) containing the important Arg42-Gly43-Asp44, of the present heterodimer and schistatin. These differences are presumably due to the presence of two glycines at positions 43 and 46 that allow the molecule to adopt variable conformations. A comparative analysis of the surface-charge distributions of various disintegrins showed that the charge distribution on monomeric disintegrins occurred uniformly over the whole surface of the molecule, while in the dimeric disintegrins, the charge is distributed only on one face. Such a feature may be important in the binding of two integrins to a single dimeric disintegrin. The phylogenetic analysis developed on the basis of amino acid sequence and three-dimensional structures indicates that the protein diversification and evolution presumably took place from the medium disintegrins and both the dimeric and short disintegrins evolved from them.

  12. Towards true 3D textural analysis; using your crystal mush wisely.

    Science.gov (United States)

    Jerram, D. A.; Morgan, D. J.; Pankhurst, M. J.

    2014-12-01

    The crystal cargo that is found in volcanic and plutonic rocks contains a wealth of information about magmatic mush processes, crystallisation history, crystal entrainment and recycling. Phenocryst populations predominantly record episodes of growth/nucleation and bulk geochemical changes within an evolving crystal-melt body. Ante- and xeno-crysts provide useful clues to the nature of mush interaction with wall rock and with principal magma(s). Furthermore, crystal evolutions (core to rim) record pathways through pressure, temperature and compositional space. These can often illustrate complex recycling within systems, describing the plumbing architecture. Understanding this architecture underpins our knowledge of how igneous systems can interact with the crust, grow, freeze, re-mobilise and prime for eruption. Initially, 2D studies produced corrected 3D crystal size distributions to help provide information about nucleation and residence times. It immediately became clear that crystal shape is an important factor in determining the confidence placed upon 3D reconstructions of 2D data. Additionally studies utilised serial sections of medium- to coarse-grain-size populations which allowed 3D reconstruction using modelling software to be improved, since size and shape etc. can be directly constrained. Finally the advent of textural studies using X-ray tomography has revolutionised the way in which we can inspect the crystal cargo in mushy systems, allowing us to image in great detail crystal packing arrangements, 3D CSDs, shapes and orientations etc. The latest most innovative studies use X-ray micro-computed tomography to rapidly characterise chemical populations within the crystal cargo, adding a further dimension to this approach, and implies the ability to untangle magmatic chemical components to better understand their individual and combined evolution. In this contribution key examples of the different types of textural analysis techniques in 2D and 3D

  13. Ionic network analysis of tectosilicates: the example of coesite at variable pressure.

    Science.gov (United States)

    Reifenberg, Melina; Thomas, Noel W

    2018-04-01

    The method of ionic network analysis [Thomas (2017). Acta Cryst. B73, 74-86] is extended to tectosilicates through the example of coesite, the high-pressure polymorph of SiO 2 . The structural refinements of Černok et al. [Z. Kristallogr. (2014), 229, 761-773] are taken as the starting point for applying the method. Its purpose is to predict the unit-cell parameters and atomic coordinates at (p-T-X) values in-between those of diffraction experiments. The essential development step for tectosilicates is to define a pseudocubic parameterization of the O 4 cages of the SiO 4 tetrahedra. The six parameters a PC , b PC , c PC , α PC , β PC and γ PC allow a full quantification of the tetrahedral structure, i.e. distortion and enclosed volume. Structural predictions for coesite require that two separate quasi-planar networks are defined, one for the silicon ions and the other for the O 4 cage midpoints. A set of parametric curves is used to describe the evolution with pressure of these networks and the pseudocubic parameters. These are derived by fitting to the crystallographic data. Application of the method to monoclinic feldspars and to quartz and cristobalite is discussed. Further, a novel two-parameter quantification of the degree of tetrahedral distortion is described. At pressures in excess of ca 20.45 GPa it is not possible to find a self-consistent solution to the parametric curves for coesite, pointing to the likelihood of a phase transition.

  14. A universal treatment of X-ray and neutron diffraction in crystals. II. Extinction

    International Nuclear Information System (INIS)

    Hu Huachen

    1997-01-01

    For pt.I see ibid., p.484-92, 1997. Based on the formalism for calculating the integrated reflection power ratio of a plane mosaic crystal by using three dimensionless parameters exact and universal expressions for the secondary-extinction factors in X-ray and neutron crystallography are developed that can be applied to reflections of all possible values of extinction factor, reflection symmetry and the absorption-to-scattering cross-section ratio of the crystal. The representation by three parameters gives a clear and definite physical meaning to the concept of extinction. The theory has been extended to treat the extinction of a spherical crystal, and the striking difference in the evaluated secondary-extinction factor between the equivalent single-plate and the exact method in the spherical-crystal treatment under θ B = 0 is explained. As a demonstration of the feasibility of using these expressions, the diffraction data for LiF and MgO crystal plates measured by Lawrence [Acta Cryst. (1972), A28, 400-404; (1973), A29, 208-210] are reanalyzed by this method. All the reflections including the strongest ones (Y o down to 0.026) are reanalyzed simultaneously with single-valued particle size and mosaic spread as fitting parameters and allowing for primary extinction if necessary. The results (R factor = 0.014 and 0.053 for LiF and MgO, respectively) are unprecedentedly good. Furthermore, in disagreement with Lawrence, the extinction of LiF is found to be of secondary type and in the case of MgO both primary and secondary extinction should be considered. The analysis also shows that the formula Y ∝ Y p Y s is valid only for very weak extinctions and that the Hamilton-Darwin equations are valid in a range much broader than previously anticipated. (orig.)

  15. Plasma characteristics in non-sinusoidally excited CCP discharges

    Science.gov (United States)

    Lafleur, Trevor; Booth, Jean-Paul

    2012-10-01

    Using particle-in-cell (PIC) simulations we perform a characterization of the plasma response to positive pulse-type voltage excitations (with a repetition frequency of 13.56 MHz) in a geometrically symmetric CCP reactor (with a gap length of 2 cm) operated with argon (for pressures between 20-500 mTorr). Use of these non-sinusoidal waveforms generates an electrical asymmetry effect in the system, which necessitates the formation of a DC bias. This DC bias, together with the shape of the voltage waveforms used, produces a number of new phenomena that are not present in typical sinusoidal discharges: (1) the plasma density and ion flux can be increased as the pulse width is reduced, (2) a significant asymmetry in the ion fluxes to the powered and grounded electrodes develops as the pressure increases, (3) the average ion energy striking the grounded electrode remains low and approximately constant as the pulse width decreases, and (4) the sheath at the grounded electrode never fully collapses; electrons are no longer lost in sharp pulses, but escape essentially throughout the rf cycle. Effects (1) and (3) above offer the possibility for a new form of control in these types of discharges, where the ion flux can be increased while the ion energy on the grounded electrode can be kept small and essentially constant. This effect has recently been exploited to control the crystallinity of silicon thin films [1], where the low ion bombarding energy was found to improve the quality of films grown. [4pt] [1] Johnson E V, Pouliquen S, Delattre P A, and Booth J P, J. Non-Cryst. Solids 2012, in press.

  16. Octakis(dimethyl sulfoxide-κOcerium(III μ6-oxido-dodeca-μ2-oxido-hexaoxidohexamolybdate(VI dimethyl sulfoxide tetrasolvate

    Directory of Open Access Journals (Sweden)

    Arbia Ben Khélifa

    2012-07-01

    Full Text Available The title complex, [Ce(C2H6OS8]2[Mo6O19]3·4C2H6OS, was obtained as a byproduct of the reaction of [(C4H94N]2[Mo6O19] with Ce(NO33·6H2O and phthalic acid in dimethylsulfoxide solution. The asymmetric unit consists of a complex [Ce(C2H6OS8]3+ cation, one and a half of the Lindqvist-type [Mo6O19]2− polyanions and two dimethylsulfoxide solvent molecules; the half polyanion lies on an inversion center. The Ce3+ ion is coordinated by eight dimethylsulfoxide ligands through the O atoms in the form of a distorted square antiprism. The Ce—O bond lengths range from 2.429 (6 to 2.550 (5 Å. The cohesion of the structure is ensured by S...O [3.115 (6, 3.242 (10 and 3.12 (3 Å], O...O [3.037 (10 Å] and C—H...O interactions between cations and anions. The S and C atoms of a dmso ligand are disordered over three sites in a 0.45:0.30:0.25 ratio. The dimethylsulfoxide solvent molecules are highly disordered and could not be modelled successfully; their contribution was therefore removed from the refinement using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Potential solvent-accessible voids of 500.0 Å3 occur in the crystal structure.

  17. Crystal structures of three 4-substituted-2,2′-bipyridines synthesized by Sonogashira and Suzuki–Miyaura cross-coupling reactions

    Directory of Open Access Journals (Sweden)

    Thuy Luong Thi Thu

    2017-04-01

    Full Text Available Facile synthetic routes for three 4-substituted 2,2′-bipyridine derivatives, 4-[2-(4-methylphenylethynyl]-2,2′-bipyridine, C19H14N2, (I, 4-[2-(pyridin-3-ylethynyl]-2,2′-bipyridine, C17H11N3, (II, and 4-(indol-4-yl-2,2′-bipyridine, C18H13N3, (III, via Sonogashira and Suzuki–Miyaura cross-coupling reactions, respectively, are described. As indicated by X-ray analysis, the 2,2′-bipyridine core, the ethylene linkage and the substituents of (I and (II are almost planar [dihedral angles between the two ring systems: 8.98 (5 and 9.90 (6° for the two molecules of (I in the asymmetric unit and 2.66 (14° for (II], allowing π-conjugation. On the contrary, in (III, the indole substituent ring is rotated significantly out of the bipyridine plane [dihedral angle = 55.82 (3°], due to steric hindrance. The crystal packings of (I and (II are dominated by π–π interactions, resulting in layers of molecules parallel to (30-2 in (I and columns of molecules along the a axis in (II. The packing of (III exhibits zigzag chains of molecules along the c axis interacting through N—H...N hydrogen bonds and π–π interactions. The contributions of unknown disordered solvent molecules to the diffraction intensities in (II were removed with the SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] algorithm of PLATON. The given chemical formula and other crystal data do not take into account these solvent molecules.

  18. Structure of Hordeum vulgare NADPH-dependent thioredoxin reductase 2. Unwinding the reaction mechanism

    Energy Technology Data Exchange (ETDEWEB)

    Kirkensgaard, Kristine G. [Carlsberg Laboratory (Denmark); Enzyme and Protein Chemistry, Department of Systems BioIogy, Technical University of Denmark (Denmark); Hägglund, Per; Finnie, Christine; Svensson, Birte [Enzyme and Protein Chemistry, Department of Systems BioIogy, Technical University of Denmark (Denmark); Henriksen, Anette, E-mail: anette@crc.dk [Carlsberg Laboratory (Denmark)

    2009-09-01

    The first crystal structure of a cereal NTR, a protein involved in seed development and germination, has been determined. The structure is in a conformation that excludes NADPH binding and indicates that a domain reorientation facilitated by Trx binding precedes NADPH binding in the reaction mechanism. Thioredoxins (Trxs) are protein disulfide reductases that regulate the intracellular redox environment and are important for seed germination in plants. Trxs are in turn regulated by NADPH-dependent thioredoxin reductases (NTRs), which provide reducing equivalents to Trx using NADPH to recycle Trxs to the active form. Here, the first crystal structure of a cereal NTR, HvNTR2 from Hordeum vulgare (barley), is presented, which is also the first structure of a monocot plant NTR. The structure was determined at 2.6 Å resolution and refined to an R{sub cryst} of 19.0% and an R{sub free} of 23.8%. The dimeric protein is structurally similar to the structures of AtNTR-B from Arabidopsis thaliana and other known low-molecular-weight NTRs. However, the relative position of the two NTR cofactor-binding domains, the FAD and the NADPH domains, is not the same. The NADPH domain is rotated by 25° and bent by a 38% closure relative to the FAD domain in comparison with AtNTR-B. The structure may represent an intermediate between the two conformations described previously: the flavin-oxidizing (FO) and the flavin-reducing (FR) conformations. Here, analysis of interdomain contacts as well as phylogenetic studies lead to the proposal of a new reaction scheme in which NTR–Trx interactions mediate the FO to FR transformation.

  19. Distinguishing tautomerism in the crystal structure of (Z)-N-(5-ethyl-2,3-di-hydro-1,3,4-thiadiazol-2-ylidene) -4-methylbenzenesulfonamide using DFT-D calculations and {sup 13}C solid-state NMR

    Energy Technology Data Exchange (ETDEWEB)

    Li, Xiaozhou; Bond, Andrew D.; Johansson, Kristoffer E.; Van de Streek, Jacco, E-mail: jacco.vandestreek@sund.ku.dk [Department of Pharmacy, University of Copenhagen, Universitetsparken 2, Copenhagen DK-2100 (Denmark)

    2014-08-01

    The crystal structure of (Z)-N-(5-ethyl-2,3-di-hydro-1,3,4-thiadiazol-2-ylidene) -4-methylbenzenesulfonamide contains an imine tautomer, rather than the previously reported amine tautomer. The tautomers can be distinguished using dispersion-corrected density functional theory calculations and by comparison of calculated and measured {sup 13}C solid-state NMR spectra. The crystal structure of the title compound, C{sub 11}H{sub 13}N{sub 3}O{sub 2}S{sub 2}, has been determined previously on the basis of refinement against laboratory powder X-ray diffraction (PXRD) data, supported by comparison of measured and calculated {sup 13}C solid-state NMR spectra [Hangan et al. (2010 ▶). Acta Cryst. B66, 615–621]. The mol@@ecule is tautomeric, and was reported as an amine tautomer [systematic name: N-(5-ethyl-1,3,4-thia@@diazol-2-yl)-p-toluene@@sulfonamide], rather than the correct imine tautomer. The protonation site on the mol@@ecule’s 1,3,4-thia@@diazole ring is indicated by the inter@@molecular contacts in the crystal structure: N—H⋯O hydrogen bonds are established at the correct site, while the alternative protonation site does not establish any notable inter molecular inter@@actions. The two tautomers provide essentially identical Rietveld fits to laboratory PXRD data, and therefore they cannot be directly distinguished in this way. However, the correct tautomer can be distinguished from the incorrect one by previously reported qu@@anti@@tative criteria based on the extent of structural distortion on optimization of the crystal structure using dispersion-corrected density functional theory (DFT-D) calculations. Calculation of the {sup 13}C SS-NMR spectrum based on the correct imine tautomer also provides considerably better agreement with the measured {sup 13}C SS-NMR spectrum.

  20. Improving experimental phases for strong reflections prior to density modification

    International Nuclear Information System (INIS)

    Uervirojnangkoorn, Monarin; Hilgenfeld, Rolf; Terwilliger, Thomas C.; Read, Randy J.

    2013-01-01

    A genetic algorithm has been developed to optimize the phases of the strongest reflections in SIR/SAD data. This is shown to facilitate density modification and model building in several test cases. Experimental phasing of diffraction data from macromolecular crystals involves deriving phase probability distributions. These distributions are often bimodal, making their weighted average, the centroid phase, improbable, so that electron-density maps computed using centroid phases are often non-interpretable. Density modification brings in information about the characteristics of electron density in protein crystals. In successful cases, this allows a choice between the modes in the phase probability distributions, and the maps can cross the borderline between non-interpretable and interpretable. Based on the suggestions by Vekhter [Vekhter (2005 ▶), Acta Cryst. D61, 899–902], the impact of identifying optimized phases for a small number of strong reflections prior to the density-modification process was investigated while using the centroid phase as a starting point for the remaining reflections. A genetic algorithm was developed that optimizes the quality of such phases using the skewness of the density map as a target function. Phases optimized in this way are then used in density modification. In most of the tests, the resulting maps were of higher quality than maps generated from the original centroid phases. In one of the test cases, the new method sufficiently improved a marginal set of experimental SAD phases to enable successful map interpretation. A computer program, SISA, has been developed to apply this method for phase improvement in macromolecular crystallography

  1. Crystal structure of di-μ-chlorido-bis[chloridobis(1,2-dimethyl-5-nitro-1H-imidazole-κN3copper(II] acetonitrile disolvate

    Directory of Open Access Journals (Sweden)

    Patrick J. Quinlivan

    2016-11-01

    Full Text Available 1,2-Dimethyl-5-nitroimidazole (dimetridazole, dimet is a compound that belongs to a class of nitroimidazole drugs that are effective at inhibiting the activity of certain parasites and bacteria. However, there are few reports that describe structures of compounds that feature metals complexed by dimet. Therefore, we report here that dimet reacts with CuCl2·H2O to yield a chloride-bridged copper(II dimer, [Cu2Cl4(C5H7N3O24] or [Cu(μ-ClCl(dimet2]2. In this molecule, the CuII ions are coordinated in an approximately trigonal–bipyramidal manner, and the molecule lies across an inversion center. The dihedral angle between the imidazole rings in the asymmetric unit is 4.28 (7°. Compared to metronidazole, dimetridazole lacks the hydroxyethyl group, and thus cannot form intermolecular O...H hydrogen-bonding interactions. Instead, [Cu(μ-ClCl(dimet2]2 exhibits weak intermolecular interactions between the hydrogen atoms of C—H groups and (i oxygen in the nitro groups, and (ii the terminal and bridging chloride ligands. The unit cell contains four disordered acetonitrile molecules. These were modeled as providing a diffuse contribution to the overall scattering by SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18], which identified two voids, each with a volume of 163 Å3 and a count of 46 electrons, indicative of a total of four acetonitrile molecules. These acetonitrile molecules are included in the chemical formula to give the expected calculated density and F(000.

  2. Automation of High-Throughput Crystal Screening and Data Collection at SSRL

    International Nuclear Information System (INIS)

    Miller, Mitchell D.; Brinen, Linda S.; Deacon, Ashley M.; Bedem, Henry van den; Wolf, Guenter; Xu Qingping; Zhang Zepu; Cohen, Aina; Ellis, Paul; McPhillips, Scott E.; McPhillips, Timothy M.; Phizackerley, R. Paul; Soltis, S. Michael

    2004-01-01

    A robotic system for auto-mounting crystals from liquid nitrogen is now operational on SSRL beamlines (Cohen et al., J. Appl. Cryst. (2002). 35, 720-726). The system uses a small industrial 4-axis robot with a custom built actuator. Once mounted, automated alignment of the sample loop to the X-ray beam readies the crystal for data collection. After data collection, samples are returned to the cassette. The beamline Dewar accommodates three compact sample cassettes (holding up to 96 samples each). During the past 4 months, the system on beamline 11-1 has been used to screen over 1000 crystals. The system has reduced both screening time and manpower. Integration of the hardware components is accomplished in the Distributed Control System architecture developed at SSRL (McPhillips et al., J. Synchrotron Rad. (2002) 9, 401-406). A crystal-screening interface has been implemented in Blu-Ice. Sample details can be uploaded from an Excel spreadsheet. The JCSG generates these spreadsheets automatically from their tracking database using standard database tools (http://www.jcsg.org). New diffraction image analysis tools are being employed to aid in extracting results. Automation also permits tele-presence. For example, samples have been changed during the night without leaving home and scientists have screened crystals 1600 miles from the beamline. The system developed on beamline 11-1 has been replicated onto 1-5, 9-1, 9-2, and 11-3 and is used by both general users and the JCSG

  3. Structure of Hordeum vulgare NADPH-dependent thioredoxin reductase 2. Unwinding the reaction mechanism

    International Nuclear Information System (INIS)

    Kirkensgaard, Kristine G.; Hägglund, Per; Finnie, Christine; Svensson, Birte; Henriksen, Anette

    2009-01-01

    The first crystal structure of a cereal NTR, a protein involved in seed development and germination, has been determined. The structure is in a conformation that excludes NADPH binding and indicates that a domain reorientation facilitated by Trx binding precedes NADPH binding in the reaction mechanism. Thioredoxins (Trxs) are protein disulfide reductases that regulate the intracellular redox environment and are important for seed germination in plants. Trxs are in turn regulated by NADPH-dependent thioredoxin reductases (NTRs), which provide reducing equivalents to Trx using NADPH to recycle Trxs to the active form. Here, the first crystal structure of a cereal NTR, HvNTR2 from Hordeum vulgare (barley), is presented, which is also the first structure of a monocot plant NTR. The structure was determined at 2.6 Å resolution and refined to an R cryst of 19.0% and an R free of 23.8%. The dimeric protein is structurally similar to the structures of AtNTR-B from Arabidopsis thaliana and other known low-molecular-weight NTRs. However, the relative position of the two NTR cofactor-binding domains, the FAD and the NADPH domains, is not the same. The NADPH domain is rotated by 25° and bent by a 38% closure relative to the FAD domain in comparison with AtNTR-B. The structure may represent an intermediate between the two conformations described previously: the flavin-oxidizing (FO) and the flavin-reducing (FR) conformations. Here, analysis of interdomain contacts as well as phylogenetic studies lead to the proposal of a new reaction scheme in which NTR–Trx interactions mediate the FO to FR transformation

  4. Modified Statistical Dynamical Diffraction Theory: A Novel Metrological Analysis Method for Partially Relaxed and Defective Carbon-doped Silicon and Silicon Germanium Heterostructures

    Science.gov (United States)

    Shreeman, Paul K.

    The statistical dynamical diffraction theory, which has been initially developed by late Kato remained in obscurity for many years due to intense and difficult mathematical treatment that proved to be quite challenging to implement and apply. With assistance of many authors in past (including Bushuev, Pavlov, Pungeov, and among the others), it became possible to implement this unique x-ray diffraction theory that combines the kinematical (ideally imperfect) and dynamical (the characteristically perfect diffraction) into a single system of equations controlled by two factors determined by long range order and correlation function within the structure. The first stage is completed by the publication (Shreeman and Matyi, J. Appl. Cryst., 43, 550 (2010)) demonstrating the functionality of this theory with new modifications hence called modified statistical dynamical diffraction theory (mSDDT). The foundation of the theory is also incorporated into this dissertation, and the next stage of testing the model against several ion-implanted SiGe materials has been published: (Shreeman and Matyi, physica status solidi (a)208(11), 2533-2538, 2011). The dissertation with all the previous results summarized, dives into comprehensive analysis of HRXRD analyses complete with several different types of reflections (symmetrical, asymmetrical and skewed geometry). The dynamical results (with almost no defects) are compared with well-known commercial software. The defective materials, to which commercially available modeling software falls short, is then characterized and discussed in depth. The results will exemplify the power of the novel approach in the modified statistical dynamical diffraction theory: Ability to detect and measure defective structures qualitatively and quantitatively. The analysis will be compared alongside with TEM data analysis for verification and confirmation. The application of this theory will accelerate the ability to quickly characterize the relaxed

  5. Redetermined structure of gossypol (P3 polymorph

    Directory of Open Access Journals (Sweden)

    Muhabbat Honkeldieva

    2015-07-01

    Full Text Available An improved crystal structure of the title compound, C30H30O8 (systematic name: 1,1′,6,6′,7,7′-hexahydroxy-5,5′-diisopropyl-3,3′-dimethyl[2,2′-binaphthalene]-8,8′-dicarbaldehyde, was determined based on modern CCD data. Compared to the previous structure [Talipov et al. (1985. Khim. Prirod. Soedin. (Chem. Nat. Prod., 6, 20–24], geometrical precision has been improved (typical C—C bond-distance s.u. = 0.002 Å in the present structure compared to 0.005 Å in the previous structure and the locations of several H atoms have been corrected. The gossypol molecules are in the aldehyde tautomeric form and the dihedral angle between the naphthyl fragments is 80.42 (4°. Four intramolecular O—H...O hydrogen bonds are formed. In the crystal, inversion dimers with graph-set motif R22(20 are formed by pairs of O—H...O hydrogen bonds; another pair of O—H...O hydrogen bonds with the same graph-set motif links the dimers into [001] chains. The packing of such chains in the crystal leads to the formation of channels (diameter = 5–8 Å propagating in the [101] direction. The channels presumably contain highly disordered solvent molecules; their contribution to the scattering was removed with the SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] routine in PLATON and the stated molecular mass, density etc., do not take them into account.

  6. 3-(1H-Indol-3-yl-2-(2-nitrobenzenesulfonamidopropanoic acid including an unknown solvate

    Directory of Open Access Journals (Sweden)

    Islam Ullah Khan

    2012-07-01

    Full Text Available In the title compound, C17H15N3O6S, which crystallized with highly disordered methanol and/or water solvent molecules, the dihedral angle between the the indole and benzene ring systems is 5.3 (2°, which allows for the formation of intramolecular π–π stacking interactions [centroid–centroid separations = 3.641 (3 and 3.694 (3 Å] and an approximate overall U-shape for the molecule. In the crystal, dimers linked by pairs of Ns—H...Oc (s = sulfonamide and c = carboxylate hydrogen bonds generate R22(10 loops, whereas Ni—H...π (i = indole interactions lead to chains propagating in [100] or [010]. Together, these lead to a three-dimensional network in which the solvent voids are present as intersecting (two-dimensional systems of [100] and [010] channels. The title compound was found to contain a heavily disordered solvent molecule, which could be methanol or water or a mixture of the two. Due to its uncertain nature and the unresolvable disorder, the data were processed with the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155], which revealed 877.8 Å3 of solvent-accessible volume per unit cell and 126 electron-units of scattering density or 109.7 Å3 (16 electron units per organic molecule.. This was not included in the calculations of overall formula weight, density and absorption coefficient.

  7. Space of symmetry matrices with elements 0, ±1 and complete geometric description; its properties and application.

    Science.gov (United States)

    Stróż, Kazimierz

    2011-09-01

    A fixed set, that is the set of all lattice metrics corresponding to the arithmetic holohedry of a primitive lattice, is a natural tool for keeping track of the symmetry changes that may occur in a deformable lattice [Ericksen (1979). Arch. Rat. Mech. Anal. 72, 1-13; Michel (1995). Symmetry and Structural Properties of Condensed Matter, edited by T. Lulek, W. Florek & S. Walcerz. Singapore: Academic Press; Pitteri & Zanzotto (1996). Acta Cryst. A52, 830-838; and references quoted therein]. For practical applications it is desirable to limit the infinite number of arithmetic holohedries, and simplify their classification and construction of the fixed sets. A space of 480 matrices with cyclic consecutive powers, determinant 1, elements from {0, ±1} and geometric description were analyzed and offered as the framework for dealing with the symmetry of reduced lattices. This matrix space covers all arithmetic holohedries of primitive lattice descriptions related to the three shortest lattice translations in direct or reciprocal spaces, and corresponds to the unique list of 39 fixed points with integer coordinates in six-dimensional space of lattice metrics. Matrices are presented by the introduced dual symbol, which sheds some light on the lattice and its symmetry-related properties, without further digging into matrices. By the orthogonal lattice distortion the lattice group-subgroup relations are easily predicted. It was proven and exemplified that new symbols enable classification of lattice groups on an absolute basis, without metric considerations. In contrast to long established but sophisticated methods for assessing the metric symmetry of a lattice, simple filtering of the symmetry operations from the predefined set is proposed. It is concluded that the space of symmetry matrices with elements from {0, ±1} is the natural environment of lattice symmetries related to the reduced cells and that complete geometric characterization of matrices in the arithmetic

  8. Crystal structure of an unknown solvate of (piperazine-κN{5,10,15,20-tetrakis[4-(benzoyloxyphenyl]porphyrinato-κ4N}zinc

    Directory of Open Access Journals (Sweden)

    Soumaya Nasri

    2016-07-01

    Full Text Available The title compound, [Zn(C72H44N4O8(C4H10N2] or [Zn(TPBP(pipz] (where TPBP and pipz are 5,10,15,20-tetrakis[4-(benzoyloxyphenyl]porphyrinato and piperazine ligands respectively, features a distorted square-pyramidal coordination geometry about the central ZnII atom. This central atom is chelated by the four N atoms of the porphyrinate anion and further coordinated by a nitrogen atom of the piperazine axial ligand, which adopts a chair confirmation. The average Zn—N(pyrrole bond length is 2.078 (7 Å and the Zn— N(pipz bond length is 2.1274 (19 Å. The zinc cation is displaced by 0.4365 (4 Å from the N4C20 mean plane of the porphyrinate anion toward the piperazine axial ligand. This porphyrinate macrocycle exhibits major saddle and moderate ruffling deformations. In the crystal, the supramolecular structure is made by parallel pairs of layers along (100, with an interlayer distance of 4.100 Å while the distance between two pairs of layers is 4.047 Å. A region of electron density was treated with the SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] procedure in PLATON following unsuccessful attempts to model it as being part of disordered n-hexane solvent and water molecules. The given chemical formula and other crystal data do not take into account these solvent molecules.

  9. Crystal and molecular structure of 2-thiouridine

    Energy Technology Data Exchange (ETDEWEB)

    Hawkinson, S W

    1977-01-01

    The ''minor'' nucleoside 2-thiouridine, C/sub 9/H/sub 12/O/sub 5/N/sub 2/S, crystallizes in a monoclinic cell, space group P2/sub 1/ with a = 5.049 (2), b = 7.526 (2), c = 14.050 (3) A, ..beta.. = 90.17 (2)/sup 0/, and d = 1.619 g cm/sup -3/ (for Z = 2) at 22 +- 2/sup 0/C. The structure was derived from 1334 unique intensities measured with an Oak Ridge computer-controlled diffractometer to a limit of sin theta/lambda = 0.65 A/sup -1/ with Nb-filtered Mo K..cap alpha.. radiation. Atomic parameters were obtained by a combination of Patterson and Fourier techniques and refined by full-matrix least squares to a final R(F) value of 0.023 for all data. The bond lengths and angles in the molecule agree well with those of other thiopyrimidines (C(2) - S = 1.677 A). The conformation of the sugar ring relative to the base is anti with a torsion angle chi(O(1')--C(1') ..-->.. N(1)--C(6)) of 17/sup 0/. The sugar exists in the 3'-endo conformation. The O(5')--C(5') bond is gauche to C(4) - O(1') and trans to C(4')--C(3') (torsion angles of 74 and -169/sup 0/ respectively). The molecules are linked together in the crystal by hydrogen bonds in an intricate network which is identical to that inferred by Kojic-Prodic, Liminga, Sljukic and Ruzic-Toros (Acta Cryst. (1974), B30, 1550-1555) for the crystal structure of 5,6-dihydro-2-thiouridine. 2 figures; 6 tables.

  10. Anharmonic thermal vibrations of be metal found in the MEM nuclear density map

    International Nuclear Information System (INIS)

    Takata, Masaki; Sakata, Makoto; Larsen, F.K.; Kumazawa, Shintaro; Iversen, B.B.

    1993-01-01

    A direct observation of the thermal vibrations of Be metal was performed by the Maximum Entropy Method (MEM) using neutron single crystal data. In the previous study, the existence of the small but significant cubic anharmonicity of Be has been found by the conventional least squares refinement of the observed structure factors [Larsen, Lehmann and Merisalo (1980) Acta Cryst. A36, 159-163]. In the present study, the same data were used for the MEM analysis which are comprised of 48 reflections up to sinθ/λ = 1.41A -1 in order to obtain the high resolution nuclear density of Be without using any thermal vibrational model. It was directly visible in the MEM map that not only the cubic terms but also quartic anharmonicities exist in the thermal vibrations of Be nuclei. In order to evaluate thermal parameters of Be including anharmonic terms quantitatively, the least squares refinement of the effective one-particle potential (OPP) parameters up to quartic term was carried out by using the MEM nuclear densities around atomic sites as the data set to be fitted. It was found that the present treatment has a great advantage to decide the most appropriate model of OPP by visually comparing the model with MEM density map. As a result of the least squares refinement, the anharmonic thermal parameters are obtained as α 33 = -0.340(5)[eV/A 3 ], α 40 = 0, β 20 = 9.89(1)[eV/A 4 ] and γ 00 = 0. No other anharmonic term was significant. (author)

  11. Crystal structure of the anti-(carcinoembryonic antigen) single-chain Fv antibody MFE-23 and a model for antigen binding based on intermolecular contacts.

    Science.gov (United States)

    Boehm, M K; Corper, A L; Wan, T; Sohi, M K; Sutton, B J; Thornton, J D; Keep, P A; Chester, K A; Begent, R H; Perkins, S J

    2000-03-01

    MFE-23 is the first single-chain Fv antibody molecule to be used in patients and is used to target colorectal cancer through its high affinity for carcinoembryonic antigen (CEA), a cell-surface member of the immunoglobulin superfamily. MFE-23 contains an N-terminal variable heavy-chain domain joined by a (Gly(4)Ser)(3) linker to a variable light-chain (V(L)) domain (kappa chain) with an 11-residue C-terminal Myc-tag. Its crystal structure was determined at 2.4 A resolution by molecular replacement with an R(cryst) of 19.0%. Five of the six antigen-binding loops, L1, L2, L3, H1 and H2, conformed to known canonical structures. The sixth loop, H3, displayed a unique structure, with a beta-hairpin loop and a bifurcated apex characterized by a buried Thr residue. In the crystal lattice, two MFE-23 molecules were associated back-to-back in a manner not seen before. The antigen-binding site displayed a large acidic region located mainly within the H2 loop and a large hydrophobic region within the H3 loop. Even though this structure is unliganded within the crystal, there is an unusually large region of contact between the H1, H2 and H3 loops and the beta-sheet of the V(L) domain of an adjacent molecule (strands DEBA) as a result of intermolecular packing. These interactions exhibited remarkably high surface and electrostatic complementarity. Of seven MFE-23 residues predicted to make contact with antigen, five participated in these lattice contacts, and this model for antigen binding is consistent with previously reported site-specific mutagenesis of MFE-23 and its effect on CEA binding.

  12. Molecular ordering of ethanol at the calcite surface.

    Science.gov (United States)

    Pasarín, I S; Yang, M; Bovet, N; Glyvradal, M; Nielsen, M M; Bohr, J; Feidenhans'l, R; Stipp, S L S

    2012-02-07

    To produce biominerals, such as shells, bones, and teeth, living beings create organic compounds that control the growth of the solid phase. Investigating the atomic scale behavior of individual functional groups at the mineral-fluid interface provides fundamental information that is useful for constructing accurate predictive models for natural systems. Previous investigations of the activity of coccolith-associated polysaccharides (CAP) on calcite, using atomic force microscopy (AFM) [Henriksen, K., Young, J. R., Bown, P. R., and Stipp, S. L. S. Palentology 2004, 43 (Part 3), 725-743] and molecular dynamics (MD) modeling [Yang, M., Stipp, S. L. S., and Harding, J. H. Cryst. Growth Des. 2008, 8 (11), 4066-4074], have suggested that OH functional groups control polysaccharide attachment. The purpose of this work was to characterize, using X-ray reflectivity (XR) combined with molecular dynamics (MD) simulations, the structuring on calcite of a layer of the simplest carbon chain molecule that contains an OH group, ethanol (CH(3)-CH(2)-OH). We found evidence that EtOH forms a highly ordered structure at the calcite surface, where the first layer molecules bond with calcite. The ethanol molecules stand up perpendicularly at the interface or nearly so. As a consequence, the fatty, CH(3) ends form a new surface, about 6 Å from the termination of the bulk calcite, and beyond that, there is a thin gap where ethanol density is low. Following is a more disordered layer that is two to three ethanol molecules thick, about 14 Å, where density more resembles that of bulk liquid ethanol. The good agreement between theory and experiment gives confidence that a theoretical approach can offer information about behavior in more complex systems.

  13. Texture, residual stress and structural analysis of thin films using a combined X-ray analysis

    International Nuclear Information System (INIS)

    Lutterotti, L.; Chateigner, D.; Ferrari, S.; Ricote, J.

    2004-01-01

    Advanced thin films for today's industrial and research needs require highly specialized methodologies for a successful quantitative characterization. In particular, in the case of multilayer and/or unknown phases a global approach is necessary to obtain some or all the required information. A full approach has been developed integrating novel texture and residual stress methodologies with the Rietveld method (Acta Cryst. 22 (1967) 151) (for crystal structure analysis) and it has been coupled with the reflectivity analysis. The complete analysis can be done at once and offers several benefits: the thicknesses obtained from reflectivity can be used to correct the diffraction spectra, the phase analysis help to identify the layers and to determine the electron density profile for reflectivity; quantitative texture is needed for quantitative phase and residual stress analyses; crystal structure determination benefits of the previous. To achieve this result, it was necessary to develop some new methods, especially for texture and residual stresses. So it was possible to integrate them in the Rietveld, full profile fitting of the patterns. The measurement of these spectra required a special reflectometer/diffractometer that combines a thin parallel beam (for reflectivity) and a texture/stress goniometer with a curved large position sensitive detector. This new diffraction/reflectivity X-ray machine has been used to test the combined approach. Several spectra and the reflectivity patterns have been collected at different tilting angles and processed at once by the special software incorporating the aforementioned methodologies. Some analysis examples will be given to show the possibilities offered by the method

  14. Neutron Imaging of Lithium Concentration for Validation of Li-Ion Battery State of Charge Estimation

    Science.gov (United States)

    2010-12-01

    2008: Understanding liq- uid water distribution and removal phenomena in an op- erating pemfc via neutron radiography. Journal of The...2008: Measurement of liq- uid water accumulation in a pemfc with dead-ended an- ode. Journal of The Electrochemical Society, 155 (11), B1168–B1178

  15. Linking Leisure Interests to the RIASEC World of Work Map

    Science.gov (United States)

    Armstrong, Patrick Ian; Rounds, James

    2008-01-01

    The present study presents an interpretive framework for linking leisure interests, measured by the Leisure Interest Questionnaire (LIQ), to J. L. Holland's (1997) circumplex model of the world of work. Published data representing correlations between the LIQ and Holland's RIASEC interest types were obtained from Hansen and Scullard (2002).…

  16. Polymer synthesis in ionic liquids : towards a green industry

    NARCIS (Netherlands)

    Guerrero-Sanchez, C.A.; Schubert, U.S.

    2004-01-01

    The screening of six ionic liqs. used as reaction media in free radical polymn. of Me methacrylate and styrene was performed. AIBN was used as initiator for the polymn. of Me methacrylate and benzoyl peroxide in the case of styrene. Soly. of the used ionic liqs. in these monomers and water was also

  17. Skin permeability and pharmacokinetics of diclofenac epolamine administered by dermal patch in Yorkshire-Landrace pigs

    Directory of Open Access Journals (Sweden)

    Tse S

    2012-10-01

    Full Text Available Susanna Tse,1 Kendall D Powell,2 Stephen MacLennan,3 Allan R Moorman,4 Craig Paterson,5 Rosonald R Bell11Pfizer Inc, Groton, CT, USA; 2Tandem Labs, Durham, NC, USA; 3BioCryst Pharmaceuticals Inc, Durham, NC, USA; 4Alta Vetta Pharmaceutical Consulting LLC, Durham, NC, USA; 5Salix Pharmaceuticals Inc, Raleigh, NC, USAPurpose: This study compared the pharmacokinetic profile, and systemic and local absorption of diclofenac, following dermal patch application and oral administration in Yorkshire- Landrace pigs.Patients and methods: Twelve anesthetized, female, Yorkshire-Landrace pigs were randomized to receive either the dermal patch (FLECTOR® patch, 10 × 14 cm; Alpharma Pharmaceuticals, a subsidiary of Pfizer Inc, New York, NY or 50 mg oral diclofenac (Voltaren®; Novartis, East Hanover, NJ. Tissue (skin area of 2 × 2 cm and underlying muscles approximately 2–3 cm in depth and blood (10 mL samples were collected at timed intervals up to 11.5 hours after initial patch application or oral administration. The concentrations of diclofenac in plasma, skin, and muscle samples were analyzed using validated ultra performance liquid chromatography tandem mass spectrometric methods.Results: Peak systemic exposure of diclofenac was very low by dermal application compared with oral administration (maximum concentration [Cmax] values of 3.5 vs 9640 ng/mL, respectively. Absorption of diclofenac into underlying muscles beneath the dermal patch was sustained, and followed apparently zero-order kinetics, with the skin serving as a depot with elevated concentrations of diclofenac. Concentrations of diclofenac in muscles beneath the patch application site were similar to corresponding tissues after oral administration (Cmax values of 879 and 1160 ng/mL, respectively. In contrast to the wide tissue distribution of diclofenac after oral administration, dermal patch application resulted in high concentrations of diclofenac only on the treated skin and immediate

  18. Bis(1,3-dimethyl-1H-imidazolium hexafluorosilicate methanol 0.33-solvate

    Directory of Open Access Journals (Sweden)

    Maxim V. Borzov

    2013-08-01

    Full Text Available The title compound, 6C5H9N2+·3SiF62−·CH3OH, (I, was prepared by recrystallization of the crude salt from methanol along with solvent-free 2C5H9N2+·SiF62− (II. Crystals of these solvatomorphs can be separated manually. The solvate (I crystallizes in a rare hexagonal space group P6/mcc. Its asymmetric unit comprises one half of an imidazolium cation bisected by the crystallographic m-plane, one-sixth and one-twelfth of two crystallographically independent SiF62– dianions (Si atoms are located on the 3.2 and 6/m inversion centres, and one-twelfth of a methanol molecule (C atoms are situated on the 622 inversion centres, other atoms are disordered between general positions. In (I, all F atoms of 3.2-located SiF62– dianions participate in the formation of symmetry-equivalent contacts to the H atoms of imidazolium fragments, thus forming rod-type ensembles positioned on the -6 axes. These `pillar' rods are, in turn, F...H interlinked through SiF62– dianions disordered around the 6/m centres. The twelvefold disordered methanol molecules are appended to this array by O—H...F hydrogen bonds to the 6/m located SiF62– dianions. In terms of graph-set notation, the first and second level networks in (I are N1 = C22(7[3R44(14]D22(4 and N2 = D22(5 (C—H...O hydrogen bonds are not considered. After locating all symmetrically independent atoms in the cation and anions, there remained a strong (> 3 e Å−3 residual electron density peak located at the 622 inversion centre. Treatment of this pre-refined model with the SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155] revealed two voids per unit cell, indicative of the presence of the solvent methanol molecule disordered about the 622 inversion centre.

  19. Molecular replacement then and now

    International Nuclear Information System (INIS)

    Scapin, Giovanna

    2013-01-01

    A brief overview, with examples, of the evolution of molecular-replacement methods and models over the past few years is presented. The ‘phase problem’ in crystallography results from the inability to directly measure the phases of individual diffracted X-ray waves. While intensities are directly measured during data collection, phases must be obtained by other means. Several phasing methods are available (MIR, SAR, MAD, SAD and MR) and they all rely on the premise that phase information can be obtained if the positions of marker atoms in the unknown crystal structure are known. This paper is dedicated to the most popular phasing method, molecular replacement (MR), and represents a personal overview of the development, use and requirements of the methodology. The first description of noncrystallographic symmetry as a tool for structure determination was explained by Rossmann and Blow [Rossmann & Blow (1962 ▶), Acta Cryst.15, 24–31]. The term ‘molecular replacement’ was introduced as the name of a book in which the early papers were collected and briefly reviewed [Rossmann (1972 ▶), The Molecular Replacement Method. New York: Gordon & Breach]. Several programs have evolved from the original concept to allow faster and more sophisticated searches, including six-dimensional searches and brute-force approaches. While careful selection of the resolution range for the search and the quality of the data will greatly influence the outcome, the correct choice of the search model is probably still the main criterion to guarantee success in solving a structure using MR. Two of the main parameters used to define the ‘best’ search model are sequence identity (25% or more) and structural similarity. Another parameter that may often be undervalued is the quality of the probe: there is clearly a relationship between the quality and the correctness of the chosen probe and its usefulness as a search model. Efforts should be made by all structural biologists to

  20. Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation.

    Science.gov (United States)

    Martin-Garcia, Jose M; Conrad, Chelsie E; Nelson, Garrett; Stander, Natasha; Zatsepin, Nadia A; Zook, James; Zhu, Lan; Geiger, James; Chun, Eugene; Kissick, David; Hilgart, Mark C; Ogata, Craig; Ishchenko, Andrii; Nagaratnam, Nirupa; Roy-Chowdhury, Shatabdi; Coe, Jesse; Subramanian, Ganesh; Schaffer, Alexander; James, Daniel; Ketwala, Gihan; Venugopalan, Nagarajan; Xu, Shenglan; Corcoran, Stephen; Ferguson, Dale; Weierstall, Uwe; Spence, John C H; Cherezov, Vadim; Fromme, Petra; Fischetti, Robert F; Liu, Wei

    2017-07-01

    Crystal structure determination of biological macromolecules using the novel technique of serial femtosecond crystallography (SFX) is severely limited by the scarcity of X-ray free-electron laser (XFEL) sources. However, recent and future upgrades render microfocus beamlines at synchrotron-radiation sources suitable for room-temperature serial crystallography data collection also. Owing to the longer exposure times that are needed at synchrotrons, serial data collection is termed serial millisecond crystallography (SMX). As a result, the number of SMX experiments is growing rapidly, with a dozen experiments reported so far. Here, the first high-viscosity injector-based SMX experiments carried out at a US synchrotron source, the Advanced Photon Source (APS), are reported. Microcrystals (5-20 µm) of a wide variety of proteins, including lysozyme, thaumatin, phycocyanin, the human A 2A adenosine receptor (A 2A AR), the soluble fragment of the membrane lipoprotein Flpp3 and proteinase K, were screened. Crystals suspended in lipidic cubic phase (LCP) or a high-molecular-weight poly(ethylene oxide) (PEO; molecular weight 8 000 000) were delivered to the beam using a high-viscosity injector. In-house data-reduction (hit-finding) software developed at APS as well as the SFX data-reduction and analysis software suites Cheetah and CrystFEL enabled efficient on-site SMX data monitoring, reduction and processing. Complete data sets were collected for A 2A AR, phycocyanin, Flpp3, proteinase K and lysozyme, and the structures of A 2A AR, phycocyanin, proteinase K and lysozyme were determined at 3.2, 3.1, 2.65 and 2.05 Å resolution, respectively. The data demonstrate the feasibility of serial millisecond crystallography from 5-20 µm crystals using a high-viscosity injector at APS. The resolution of the crystal structures obtained in this study was dictated by the current flux density and crystal size, but upcoming developments in beamline optics and the planned APS

  1. Studies on the effects of application of different foliar fertilizer materials, crop residue and inter cropping on Banana plants

    Energy Technology Data Exchange (ETDEWEB)

    Hassan, Yusuf Munim [Faculty of Agriculture, University of Khartoum, Khartoum (Sudan)

    1997-12-31

    Five separate experiments were conducted at university of Khartoum demonstration farm during 1993 to 1995 under both orchard and nursery conditions to evaluate the effect of foliar application of different fertilizers, use of crop residue and intercropping on banana (dwarf cavendish). In the first experiment, the effects of foliar application of different concentrations of potassium solution (38%) were studied. The results indicated that application of all concentrations resulted in greater increases in overall growth parameters, higher leaf-N, P, K, Ca, Mg, Mn, Fe, Zn and Cu contents, higher values of yield and yield components , finger length of both plant crop and the first ratoon crop and reduction of time from planting to flowering and from flowering to harvesting of both plant crop and the first crop compared to the control. In the second experiment, the effects of three different foliar fertilizers, namely, compound cryst, fetrilon comb-2 and x-garden were investigated. The results revealed that all fertilizers gave greater values of all growth parameters, higher leaf-N, P, K, Ca, Mg, Mn, Fe, Zn and Cu contents, higher values of yield and yield components , finger length of both plant crop and the first ratoon crop and reduction of time from planting to flowering and from flowering to harvesting of both plant crop and the first crop compared to the control. In the third experiment, the effect of four different fertilizer materials containing different combinations of NPK on growth parameters and nutrient elements contents of leaves of banana suckers grown under nursery conditions was evaluated. The results revealed that all fertilizer materials gave greater increases of growth parameters over the control as well as higher leaf-N, P, K, Ca, Mg, Mn, Fe, Zn and Cu contents. In the fourth experiment, the effect of different concentrations of N{sub 19}, P{sub 19}, K{sub 19} fertilizers on growth characteristics and nutrient elements contents of leaves of banana

  2. Towards a compact and precise sample holder for macromolecular crystallography.

    Science.gov (United States)

    Papp, Gergely; Rossi, Christopher; Janocha, Robert; Sorez, Clement; Lopez-Marrero, Marcos; Astruc, Anthony; McCarthy, Andrew; Belrhali, Hassan; Bowler, Matthew W; Cipriani, Florent

    2017-10-01

    SPINE was tested at different institutes using evaluation kits, and pilot beamlines are being equipped with compatible robotics for large-scale evaluation. A companion paper describes a new sample changer FlexED8 (Papp et al., 2017, Acta Cryst., D73, 841-851).

  3. Crystallography beyond periodic Crystal perfection

    International Nuclear Information System (INIS)

    Estevez-Rams, E.

    2008-01-01

    Full text: The discovery of the quasi-crystals [D. Schechtman et. Al., Phys.] Rev. Lett. [53, 1951-1953 (1984)] made very narrow definition of the crystalline state based on the periodicity of a local arrangement of atoms. Since the definition of this State has been a matter of much controversy [G.R. Desiraju, Nature 423, 485 (2003); S. van Smaalen, IUCR Aperiodic Commission Reports. August 7, 2002; International Union of Crystallography. Report of the Executive Committee for 1991; ACTA Cryst. A48, 922-946 (1992)]. We will make a presentation of the current time of the crystallography in this regard from the conceptual point of view. We show the use of the formalism of algorithmic complexity or Kolmogorov [M. Li and P. Vitanyi, An Introduction to Kolmogorov Complexity and Its Applications (Springer Verlag, Heidelberg, 1993), W.H. Zurek, Phys.] Rev. 40, 4731 (1989); Nature 341, 119-124 (1989)] provides a different perspective on the nature of the Crystallographic order. Infinite crystals can be considered solid with zero algorithmic complexities by atom. Show statistical analysis of inorganic compounds [J.L.C. Daams et al., Atlas of Crystal Structure Types for Intermetallic Phases (ASM International, Ohio, 1991), Fachinformationszentrum/NIST Inorganic Crystal Structure Database, Karlsruhe (2003) icsd.fkf.mpg.de] demonstrating that the minimization of complexity is a trend in the crystalline arrangement. We will then compare the degree of disorder of some typical solids according to their algorithmic complexity. Finally, space diffraction will be studied from this same perspective and will be discussed that zero algorithmic complexities by point in space of diffraction does not necessarily imply the same thing for the Atomic arrangement. The discrete portion of the diffraction pattern is a fingerprint of the underlying order but not the actual existence of long-range order. Experimental results will be showcased [E. Estévez-Rams et al., Physical Review B, 63 (2001

  4. Crystal structures of N2,N3,N5,N6-tetrakis(pyridin-2-ylmethylpyrazine-2,3,5,6-tetracarboxamide and N2,N3,N5,N6-tetrakis(pyridin-4-ylmethylpyrazine-2,3,5,6-tetracarboxamide

    Directory of Open Access Journals (Sweden)

    Dilovan S. Cati

    2017-02-01

    Full Text Available The title compounds, C32H28N10O4· unknown solvent, (I, and C32H28N10O4, (II, are pyrazine-2,3,5,6-tetracarboxamide derivatives. In (I, the substituents are (pyridin-2-ylmethylcarboxamide, while in (II, the substituents are (pyridin-4-ylmethylcarboxamide. Both compounds crystallize in the monoclinic space group P21/n, with Z′ = 1 for (I, and Z′ = 0.5 for (II. The whole molecule of (II is generated by inversion symmetry, the pyrazine ring being situated about a center of inversion. In (I, the four pyridine rings are inclined to the pyrazine ring by 83.9 (2, 82.16 (18, 82.73 (19 and 17.65 (19°. This last dihedral angle involves a pyridine ring that is linked to the adjacent carboxamide O atom by an intramolecular C—H...O hydrogen bond. In compound (II, the unique pyridine rings are inclined to the pyrazine ring by 33.3 (3 and 81.71 (10°. There are two symmetrical intramolecular C—H...O hydrogen bonds present in (II. In the crystal of (I, molecules are linked by N—H...O and N—H...N hydrogen bonds, forming layers parallel to (10-1. The layers are linked by C—H...O and C—H...N hydrogen bonds, forming a three-dimensional framework. In the crystal of (II, molecules are linked by N—H...N hydrogen bonds, forming chains propagating along the [010] direction. The chains are linked by a weaker N—H...N hydrogen bond, forming layers parallel to the (101 plane, which are in turn linked by C—H...O hydrogen bonds, forming a three-dimensional structure. In the crystal of compound (I, a region of disordered electron density was treated with the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18]. Their contribution was not taken into account during refinement. In compound (II, one of the pyridine rings is positionally disordered, and the refined occupancy ratio for the disordered Car—Car—Npy atoms is 0.58 (3:0.42 (3.

  5. Crystal structures of a copper(II and the isotypic nickel(II and palladium(II complexes of the ligand (E-1-[(2,4,6-tribromophenyldiazenyl]naphthalen-2-ol

    Directory of Open Access Journals (Sweden)

    Souheyla Chetioui

    2016-08-01

    Full Text Available In the copper(II complex, bis{(E-1-[(2,4,6-tribromophenyldiazenyl]naphthalen-2-olato}copper(II, [Cu(C16H8Br3N2O2], (I, the metal cation is coordinated by two N atoms and two O atoms from two bidentate (E-1-[(2,4,6-tribromophenyldiazenyl]naphthalen-2-olate ligands, forming a slightly distorted square-planar environment. In one of the ligands, the tribromobenzene ring is inclined to the naphthalene ring system by 37.4 (5°, creating a weak intramolecular Cu...Br interaction [3.134 (2 Å], while in the other ligand, the tribromobenzene ring is inclined to the naphthalene ring system by 72.1 (6°. In the isotypic nickel(II and palladium(II complexes, namely bis{(E-1-[(2,4,6-tribromophenyldiazenyl]naphthalen-2-olato}nickel(II, [Ni(C16H8Br3N2O2], (II, and bis{(E-1-[(2,4,6-tribromophenyldiazenyl]naphthalen-2-olato}palladium(II, [Pd(C16H8Br3N2O2], (III, respectively, the metal atoms are located on centres of inversion, hence the metal coordination spheres have perfect square-planar geometries. The tribromobenzene rings are inclined to the naphthalene ring systems by 80.79 (18° in (II and by 80.8 (3° in (III. In the crystal of (I, molecules are linked by C—H...Br hydrogen bonds, forming chains along [010]. The chains are linked by C—H...π interactions, forming sheets parallel to (011. In the crystals of (II and (III, molecules are linked by C—H...π interactions, forming slabs parallel to (10-1. For the copper(II complex (I, a region of disordered electron density was corrected for using the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18]. The formula mass and unit-cell characteristics of the disordered solvent molecules were not taken into account during refinement.

  6. Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation

    Directory of Open Access Journals (Sweden)

    Jose M. Martin-Garcia

    2017-07-01

    Full Text Available Crystal structure determination of biological macromolecules using the novel technique of serial femtosecond crystallography (SFX is severely limited by the scarcity of X-ray free-electron laser (XFEL sources. However, recent and future upgrades render microfocus beamlines at synchrotron-radiation sources suitable for room-temperature serial crystallography data collection also. Owing to the longer exposure times that are needed at synchrotrons, serial data collection is termed serial millisecond crystallography (SMX. As a result, the number of SMX experiments is growing rapidly, with a dozen experiments reported so far. Here, the first high-viscosity injector-based SMX experiments carried out at a US synchrotron source, the Advanced Photon Source (APS, are reported. Microcrystals (5–20 µm of a wide variety of proteins, including lysozyme, thaumatin, phycocyanin, the human A2A adenosine receptor (A2AAR, the soluble fragment of the membrane lipoprotein Flpp3 and proteinase K, were screened. Crystals suspended in lipidic cubic phase (LCP or a high-molecular-weight poly(ethylene oxide (PEO; molecular weight 8 000 000 were delivered to the beam using a high-viscosity injector. In-house data-reduction (hit-finding software developed at APS as well as the SFX data-reduction and analysis software suites Cheetah and CrystFEL enabled efficient on-site SMX data monitoring, reduction and processing. Complete data sets were collected for A2AAR, phycocyanin, Flpp3, proteinase K and lysozyme, and the structures of A2AAR, phycocyanin, proteinase K and lysozyme were determined at 3.2, 3.1, 2.65 and 2.05 Å resolution, respectively. The data demonstrate the feasibility of serial millisecond crystallography from 5–20 µm crystals using a high-viscosity injector at APS. The resolution of the crystal structures obtained in this study was dictated by the current flux density and crystal size, but upcoming developments in beamline optics and the

  7. Studies on the effects of application of different foliar fertilizer materials, crop residue and inter cropping on Banana plants

    International Nuclear Information System (INIS)

    Hassan, Yusuf Munim

    1996-01-01

    Five separate experiments were conducted at university of Khartoum demonstration farm during 1993 to 1995 under both orchard and nursery conditions to evaluate the effect of foliar application of different fertilizers, use of crop residue and intercropping on banana (dwarf cavendish). In the first experiment, the effects of foliar application of different concentrations of potassium solution (38%) were studied. The results indicated that application of all concentrations resulted in greater increases in overall growth parameters, higher leaf-N, P, K, Ca, Mg, Mn, Fe, Zn and Cu contents, higher values of yield and yield components , finger length of both plant crop and the first ratoon crop and reduction of time from planting to flowering and from flowering to harvesting of both plant crop and the first crop compared to the control. In the second experiment, the effects of three different foliar fertilizers, namely, compound cryst, fetrilon comb-2 and x-garden were investigated. The results revealed that all fertilizers gave greater values of all growth parameters, higher leaf-N, P, K, Ca, Mg, Mn, Fe, Zn and Cu contents, higher values of yield and yield components , finger length of both plant crop and the first ratoon crop and reduction of time from planting to flowering and from flowering to harvesting of both plant crop and the first crop compared to the control. In the third experiment, the effect of four different fertilizer materials containing different combinations of NPK on growth parameters and nutrient elements contents of leaves of banana suckers grown under nursery conditions was evaluated. The results revealed that all fertilizer materials gave greater increases of growth parameters over the control as well as higher leaf-N, P, K, Ca, Mg, Mn, Fe, Zn and Cu contents. In the fourth experiment, the effect of different concentrations of N 19 , P 19 , K 19 fertilizers on growth characteristics and nutrient elements contents of leaves of banana suckers was

  8. Nanoscale observations of the effect of citrate on calcium oxalate precipitation on calcite surfaces.

    Science.gov (United States)

    Burgos-Cara, Alejandro; Ruiz-Agudo, Encarnacion; Putnis, Christine V.

    2016-04-01

    . Inhibition of calcium oxalate monohydrate growth by citrate and the effect of the background electrolyte. J Cryst Growth 2007;306:135-45.

  9. Amorphous and liquid samples structure and density measurements at high pressure - high temperature using diffraction and imaging techniques

    Science.gov (United States)

    Guignot, N.; King, A.; Clark, A. N.; Perrillat, J. P.; Boulard, E.; Morard, G.; Deslandes, J. P.; Itié, J. P.; Ritter, X.; Sanchez-Valle, C.

    2016-12-01

    -dispersive setup and synchrotron radiation (2004), J. Appl. Cryst. (2004). 37, 947-956 J. Philippe, Y. Le Godec, F. Bergame et M. Morand, Patent INPI 11 62335 (2013)

  10. Formation of novel spiro, spiroansa and dispiroansa derivatives of ...

    Indian Academy of Sciences (India)

    Administrator

    cyclotetraphosphazene from the reactions of polyfunctional amines ... ionic liq- uids,. 5 liquid crystalline materials,. 6 tumour growth inhibitor,. 7 ... Analytical thin layer chromatog- ..... very reactive and give multiple substituted products.

  11. Comparison study of the partial-breast irradiation techniques: Dosimetric analysis of three-dimensional conformal radiation therapy, electron beam therapy, and helical tomotherapy depending on various tumor locations

    International Nuclear Information System (INIS)

    Kim, Min-Joo; Park, So-Hyun; Son, Seok-Hyun; Cheon, Keum-Seong; Choi, Byung-Ock; Suh, Tae-Suk

    2013-01-01

    The partial-breast irradiation (PBI) technique, an alternative to whole-breast irradiation, is a beam delivery method that uses a limited range of treatment volume. The present study was designed to determine the optimal PBI treatment modalities for 8 different tumor locations. Treatment planning was performed on computed tomography (CT) data sets of 6 patients who had received lumpectomy treatments. Tumor locations were classified into 8 subsections according to breast quadrant and depth. Three-dimensional conformal radiation therapy (3D-CRT), electron beam therapy (ET), and helical tomotherapy (H-TOMO) were utilized to evaluate the dosimetric effect for each tumor location. Conformation number (CN), radical dose homogeneity index (rDHI), and dose delivered to healthy tissue were estimated. The Kruskal-Wallis, Mann-Whitney U, and Bonferroni tests were used for statistical analysis. The ET approach showed good sparing effects and acceptable target coverage for the lower inner quadrant—superficial (LIQ-S) and lower inner quadrant—deep (LIQ-D) locations. The H-TOMO method was the least effective technique as no evaluation index achieved superiority for all tumor locations except CN. The ET method is advisable for treating LIQ-S and LIQ-D tumors, as opposed to 3D-CRT or H-TOMO, because of acceptable target coverage and much lower dose applied to surrounding tissue

  12. A non-classical view of the modulation of mineral precipitation by organic additives

    Science.gov (United States)

    Ruiz-Agudo, Encarnacion; Ruiz-Agudo, Cristina; Burgos-Cara, Alejandro; Putnis, Christine; Rodriguez-Navarro, Carlos; Putnis, Andrew

    2016-04-01

    inhibit the nucleation of solid phases. These effects are linked to the influence of these molecules on polymorph selection. As well, these additives can affect non-classical growth by oriented assembly of nanoparticles. REFERENCES Rodriguez-Navarro, C., Kudłacz, K., Cizer, Ö., Ruiz-Agudo, E., 2015. Formation of amorphous calcium carbonate and its transformation into mesostructured calcite. CrystEngComm 17 (1), 58-72. Ruiz Agudo, C; Ruiz Agudo, E; Putnis, C.V.; Putnis, A., 2015. Mechanistic principles of barite formation: from nanoparticles to micron-sized crystals. Crystal Growth & Design 15, 3724-3733. Verch, A., Gebauer, D., Antonietti, M., Cölfen, H., 2011. How to control the scaling of CaCO3: a "fingerprinting technique" to classify additives. Physical chemistry chemical physics: PCCP 13 (37), 16811-16820.

  13. Crystal structures of NiSO4·9H2O and NiSO4·8H2O: magnetic properties, stability with respect to morenosite (NiSO4·7H2O), the solid-solution series (Mg x Ni1-x )SO4·9H2O

    Science.gov (United States)

    Fortes, A. D.; Knight, K. S.; Gibbs, A. S.; Wood, I. G.

    2018-02-01

    Since being discovered initially in mixed-cation systems, a method of forming end-member NiSO4·9H2O and NiSO4·8H2O has been found. We have obtained powder diffraction data from protonated analogues (with X-rays) and deuterated analogues (using neutrons) of these compounds over a range of temperatures, allowing us to determine their crystal structures—including all H-atoms—and to characterise the transitions on warming from 220 to 278 K; glass → 9-hydrate → 8-hydrate + ice → 7-hydrate + ice → partial melt (7-hydrate + liquid). NiSO4·8D2O is triclinic, space-group P\\bar {1} , Z = 2, with unit cell parameters at 150 K, a = 6.12463(8) Å, b = 6.8401(1) Å, c = 12.5339(2) Å, α = 92.846(1)°, β = 97.822(1)°, γ = 96.627(1)° and V = 515.58(1) Å3. The structure consists of two symmetry-inequivalent Ni(D2O)6 octahedra on sites of \\bar {1} symmetry. These are directly joined by a water-water H-bond to form chains of octahedra parallel with the c-axis at x = 0. Two interstitial water molecules serve both to bridge the Ni(D2O)6 octahedral chains in the b-c plane and also to connect with the SO4 2- tetrahedral oxyanion. These tetrahedra are linked by the two interstitial water molecules in a reticular motif to form sheets perpendicular to c. NiSO4·9D2O is monoclinic, space-group P21/c, Z = 4, with unit-cell parameters at 150 K, a = 6.69739(6) Å, b = 11.8628(1) Å, c = 14.5667(1) Å, β = 94.9739(8)° and V = 1152.96(1) Å3. The structure is isotypic with the Mg analogue described elsewhere (Fortes et al., Acta Cryst B 73:47‒64, 2017b). It shares the motif of H-bonded octahedral chains with NiSO4·8D2O, although in the enneahydrate these run parallel with the b-axis at x = 0. Three interstitial water molecules bridge the Ni(D2O)6 octahedra to the SO4 2- tetrahedral oxyanion. The tetrahedra sit at x ≈ 0.5 and are linked by two of the three interstitial water molecules in a pentagonal motif to form ribbons parallel with b. A solid-solution series

  14. PREFACE: Special issue: Proceedings of the Joint 19th AIRAPT and 41st EHPRG International Conference on High Pressure Science and Technology (Bordeaux, 7--11 July 2003)

    Science.gov (United States)

    Demazeau, Gérard

    2004-04-01

    , and was also by any measure a scientific success, with innumerable questions and discussions among this diverse group, and the scholarly contributions in this volume. We thank the participants, and Dr Richard Palmer, the Publisher of Journal of Physics: Condensed Matter and his staff for working to make this volume appear very quickly, thereby increasing the value of the papers to the community. We would also thank the Office of the vice-president for research at Université de Montréal, the Department of Physics and Astronomy at Arizona State University, the Department of Physics and Astronomy at Ohio University and the Canada Research Chair Program for financial assistance that made the meeting more enjoyable. We were both pleased to be part of this delightful occasion, and wish to take this last opportunity to wish Mike a happy birthday, and urge him to even greater achievements in coming years. Bibliography [1] Weaire D and Thorpe M F 1971 Electronic Properties of an Amorphous Solid: I. A Simple Tight Binding Theory Phys. Rev. B 4 2508--20 [2] Thorpe M F 1983 Continuous Deformations in Random Networks J. Non-Cryst. Solids 57 355-70 [3] Jacobs D J, Rader A J, Kuhn L A and Thorpe M F 2001 Protein Flexibilty Predictions using Graph Theory Proteins 44 150-65

  15. Barite formation in the presence of a commercial copolymer

    Science.gov (United States)

    Ruiz-Agudo, Cristina; Putnis, Christine; Ruiz-Agudo, Encarnacion; Putnis, Andrew

    2015-04-01

    early stages of barite precipitation in the presence and absence of this copolymer. With this purpose, barite was precipitated by mixing of BaCl2 and Na2SO4 solutions (with copolymer previously added to the sulphate solution). The process was quenched with ethanol at different times and the particles obtained were observed ex-situ using TEM. According to our observations, the organic molecule seems to be incorporated into barite nanoparticles, hindering or delaying their recrystallization into micron-sized crystals and stabilizing barite mesocrystals. Benton,W.J.; Collins, I.R.; Grimsey, I.M.; Parkinson, G.M.; Rodger, S.A. Faraday Discussions 1993, 95, 281-297. L. Qi; H. Cölfen; M. Antonietti. Angew. Chem. Int. Ed. 2000, 39 (3), 604-607. Wang, T.; Coelfen, H. Langmuir 2006, 22, 8975-8985. Mavredaki, E.; Neville, A.; Sorbie, K. S. Cryst. Growth Des. 2011, 11, 4751-4758. Acknowledgement: C.R-A. acknowledges a Marie Curie Fellowship: EU ITN MINSC (Mineral Scale Formation, PITN-GA-2011-290040).

  16. Opal instability: a relationship between water and microstructure?

    Science.gov (United States)

    Chauviré, Boris; Thomas, Paul; Rondeau, Benjamin; Fritsch, Emmanuel

    2017-04-01

    instability. The identification of the main factors controlling the destabilization will lead to the development of a non-destructive method for the categorization of gem-stability, increasing confidence in this gemstone for dealers, cutters and the consumer. References Aguilar B., Fritsch E., Ostroumov M., Barreau A. (2004) Why do opal die? An investigation of destabilization by whitening. 32nd Inter. Geol. Congress, Florence, Italy, 20-28 Aôut. Poster. Aguilar Reyes B.O, Ostrooumov M., Fritsch E. (2005) Estudio mineralogico de la desestabilizacion de opalos mexicanos. Revista Mexicana de Ciencas Geologicas 22(3), 391-400. Paris M, Fritsch E, Aguilar Reyes BO (2007) 1H, 29Si and 27Al NMR study of the destabilization process of a paracrystalline opal from Mexico. J. Non Cryst. Solids 353, 1650-1656. Pearson G (1985) Role of Water in Cracking of Opal. The Aust. Gemol. 15, 435-445. Rondeau B., Fritsch E., Mazzero F., Gauthier J.-P. (2011) The craze for stability. InColor 18, 42-45.

  17. Stress-Induced Proton Disorder in Hydrous Ringwoodite

    Science.gov (United States)

    Koch-Müller, M.; Rhede, D.; Mrosko, M.; Speziale, S.; Schade, U.

    2008-12-01

    observed up to 30 GPa without any discontinuity and their pressure behaviour (dν/dP) can well be described by linear fits. Molecular vibrations are very sensitive to non-hydrostatic conditions and we interpret the disappearance of the OH-bands as a stress-induced proton disordering in hydrous ringwoodite due to the use of hard pressure transmiting media like CsI or argon without thermal annealing. Thus, our study cannot confirm the phase transition observed by Camorro Perez et al. (2006) in ringwoodite. But as they used Neon as pressure transmitting medium, which is known to become non-hydrostatic at pressure above 16 GPa (Bell and Mao, 1981) we argue that their observation of a sudden disappearance of the OH band may also be related to non-hydrostatic conditions. References Bell P.M. and Mao H.-K. (1981) Carnegie Inst. Wash Yrbk 80: 404-406. Camorro Perez E.M., Daniel I., Chervin J.-C., Dumas P., Bass J.D. and Inoue T. (2006) Phys. Chem. Minerals, 33, 502 - 510. Kudoh Y., Kuribayashi T., Mizohata H., Ohtani E., (2000) Phys. Chem. Mineral. 27, 474-479. Wittlinger J., Fischer R., Wener S., ScheiderJ., Schulz J. (1997) Acta Cryst B53, 745 - 749.

  18. Poor Prognosis of Lower Inner Quadrant in Lymph Node-negative Breast Cancer Patients Who Received No Chemotherapy: A Study Based on Nationwide Korean Breast Cancer Registry Database.

    Science.gov (United States)

    Hwang, Ki-Tae; Kim, Jongjin; Kim, Eun-Kyu; Jung, Sung Hoo; Sohn, Guiyun; Kim, Seung Il; Jeong, Joon; Lee, Hyouk Jin; Park, Jin Hyun; Oh, Sohee

    2017-07-01

    We aimed to investigate the prognostic influence of primary tumor site on the survival of patients with breast cancer. Data of 63,388 patients with primary breast cancer from the Korean Breast Cancer Registry were analyzed. Primary tumor sites were classified into 5 groups: upper outer quadrant, lower outer quadrant, upper inner quadrant, lower inner quadrant (LIQ), and central portion. We analyzed overall survival (OS) and breast cancer-specific survival (BCSS) according to primary tumor site. Central portion and LIQ showed lower survival rates regarding both OS and BCSS compared with the other 3 quadrants (all P < .05) and hazard ratios were 1.267 (95% CI, 1.180-1.360, P < .001) and 1.215 (95% CI, 1.097-1.345, P < .001), respectively. Although central portion showed more unfavorable clinicopathologic features, LIQ showed more favorable features than the other 3 quadrants. Primary tumor site was a significant factor in univariate and multivariate analyses for OS and BCSS (all P < .001). For lymph node-negative patients, LIQ showed a worse OS than the other primary tumor sites in the subgroup with no chemotherapy (P < .001), but that effect disappeared in the subgroup with chemotherapy (P = .058). LIQ showed a worse prognosis despite having more favorable clinicopathologic features than other tumor locations and it was more prominent for lymph node-negative patients who received no chemotherapy. The hypothesis of possible hidden internal mammary node metastasis could be suggested to play a key role in LIQ lesions. Copyright © 2017 Elsevier Inc. All rights reserved.

  19. Vanadium oxide based cpd. useful as a cathode active material - is used in lithium or alkali metal batteries to prolong life cycles

    DEFF Research Database (Denmark)

    1997-01-01

    A mixt. of metallic iron particles and vanadium pentoxide contg. V in its pentavalent state in a liq. is reacted to convert at least some of the pentavalent V to its tetravalent state and form a gel. The liq. phase is then sepd. from the oxide based gel to obtain a solid material(I) comprising Fe......, V and oxygen where at least some of the V is in the tetravalent state. USE-(I) is a cathode active material in electric current producing storage cells. ADVANTAGE-Use of (I) in Li or alkali metal batteries gives prolonged life cycles.Storage cells using (I) have improved capacity during charge...

  20. Fulltext PDF

    Indian Academy of Sciences (India)

    meet at an angle while lattice positions are mirrored across a twin grain boundary (see Figure 6). Suggestions for Further Work. Recrystallization: We used the aqueous glycerol-dishwashing liq- uid formulation referred to above to visualize recrystallization. If the raft is broken up by stirring using an earbud, one observes.

  1. Observation of the Unusual Aggregation Kinetics of Colloidal ...

    Indian Academy of Sciences (India)

    of Holthoff et al.,26 the coagulation rate constants can be obtained ... Rui Tian et al. Hofmeister ... work are nano-scale materials made up of one Al-O ..... and Ninham B 2006 J. Mol. Liq. ... Zhang Y, Furyk S, Bergbreiter D and Cremer P 2005.

  2. Switchable narrow band reflectors produced in a single curing step

    NARCIS (Netherlands)

    2006-01-01

    A method to produce a multiphase polymer-based film by polymg. monomer in the presence of a non-reactive liq. crystal and a dichroic photoinitiator whereby the polymn. is initiated by the use of linearly polarized light, the initial mixt. being cholesteric before polymn. is described. A multiphase

  3. Dilatometer for use in tensile tests

    NARCIS (Netherlands)

    Coumans, W.J.; Heikens, D.

    1980-01-01

    An accurate dilatometer is described which permits simultaneous and automatic recording of sample vol. change during tensile tests on a com. tester. Liq. displacements in the dilatometer capillary, which correspond to vol. changes of the sample, are detected by a cond. meter. Tensile load is

  4. The Effect of Micro-Channels in the MPL on the Predicted Membrane Water Content in a PEMFC – A Modeling Study

    DEFF Research Database (Denmark)

    Berning, Torsten

    2014-01-01

    The micro-porous layer (MPL) in a proton exchange membrane fuel cell is frequently believed to constitute a barrier for the liquid water owing to its low hydraulic permeability compared to the porous substrate. When micro-channels are carved into the MPL on the side facing the catalyst layer, liq...

  5. Structural analysis of Catliq® bio-oil produced by catalytic liquid conversion of biomass

    DEFF Research Database (Denmark)

    Toor, Saqib Sohail; Rosendahl, Lasse; Nielsen, Mads Pagh

    Liq® process compared with combustion is that also wet material can be processed. In the process, the waste is transformed to bio-oil, combustible gases and water-soluble organic compounds. The raw material used in this study was DDGS (Dried Distilled Grain with Solubles), a residual product in 1st generation...

  6. Calorimetric determination of the enthalpy of 1-butyl-3-methylimidazolium bromide synthesis: a key quantity in thermodynamics of ionic liquids.

    Science.gov (United States)

    Paulechka, Yauheni U; Kabo, Andrey G; Blokhin, Andrey V

    2009-11-05

    The enthalpy of the 1-butyl-3-methylimidazolium bromide [C(4)mim]Br ionic liquid synthesis reaction 1-methylimidazole (liq) + 1-bromobutane (liq) --> [C(4)mim]Br (liq) was determined in a homemade small-volume isoperibol calorimeter to be Delta(r)H degrees (298) = -87.7 +/- 1.6 kJ x mol(-1). The activation energy for this reaction in a homogeneous system E(A) = 73 +/- 4 kJ x mol(-1) was found from the results of calorimetric measurements. The formation enthalpies for the crystalline and liquid [C(4)mim]Br were determined from the calorimetric data: Delta(f)H degrees (298)(cr) = -178 +/- 5 kJ x mol(-1) and Delta(f)H degrees (298)(liq) = -158 +/- 5 kJ x mol(-1). The ideal-gas formation enthalpy of this compound Delta(f)H degrees (298)(g) = 16 +/- 7 kJ x mol(-1) was calculated using the methods of quantum chemistry and statistical thermodynamics. The vaporization enthalpy of [C(4)mim]Br, Delta(vap)H degrees (298) = 174 +/- 9 kJ x mol(-1), was estimated from the experimental and calculated formation enthalpies. It was demonstrated that vapor pressure of this ionic liquid cannot be experimentally determined.

  7. Aroma retention during the drying of liquid foods

    NARCIS (Netherlands)

    Menting, L.C.; Hoogstad, B.; Thijssen, H.A.C.

    1970-01-01

    Factors detg. aroma retention during the drying of food liqs. were investigated by a model system. Slabs of an aq. soln. of partially hydrolyzed starch, contg. a small amt. of acetone, were dried in air and the percentage of acetone retained was measured. Acetone was lost almost exclusively during

  8. Physics of plasma etching and plasma deposition

    NARCIS (Netherlands)

    Schram, D.C.; Hoog, de F.J.; Bisschops, T.J.; Kroesen, G.M.W.; Howorka, F.; Lindinger, W.; Maerk, T.D.

    1986-01-01

    The kinetics and mechanism of the title processes are discussed on the basis of a model in which the plasma-surface system is subdivided into 5 regions: (I) plasma prodn., (II) plasma flow plus radicals, (III) gas adsorbed layer, (IV) modified surface, and (V) undisturbed solid (or liq.) state.

  9. Fulltext PDF

    Indian Academy of Sciences (India)

    product is polar or somewhat soluble in water. Also, from the environment and economic point of view, het- erogenization of homogeneous catalytic reactions has attracted much attention.1 Heterogenization of ionic liq- uids is an area of current research, which enables easy recovery and reuse of expensive catalysts.

  10. Palladium catalysed asymmetric alkylation of benzophenone Schiff ...

    Indian Academy of Sciences (India)

    some time in the application of phase transfer catalysis to the preparation of ... to free them from moisture contamination. Ionic liq- ... mined by chiral HPLC analysis (chiracel OD, hexane: 2-propanol ... chromatography on alumina 90 active basic (0.063–. 0.200 mm) ..... ing solubility of ionic liquids in water at 20. ◦. C, for the.

  11. Analysis of heat transfer in a centrifugal film evaporator

    NARCIS (Netherlands)

    Bruin, S.

    1970-01-01

    Heat transfer in a centrifugal film evaporator with a conical heating surface is analyzed. Two regions of transfer can be distinguished: an entrance region, where the temp. profile in the film develops, and an evapn. region, where \\"surface evapn.\\" takes place. Relations are derived for liq.-film

  12. The effect of pH profiles in methanogenic aggregates on the kinetics of acetate conversion

    NARCIS (Netherlands)

    Beer, de D.; Huisman, J.W.; Heuvel, van den J.C.; Ottengraf, S.P.P.

    1993-01-01

    Due to the conversion of acetic acid into the weaker carbonic acid and CH4, the pH inside methanogenic aggregates is higher than in the bulk liq. The pH profiles in aggregates were measured with pH microelectrodes. These profiles strongly det. the macro-kinetics of the aggregate, by their influence

  13. REFLEX CLOSURE OF THE OESOPHAGEAL GROOVE AND ITS ...

    African Journals Online (AJOL)

    reticular-ornasal orifice, thus prevening swallowed fluids entering the reticulum ... the function of leading mixed food particles and liqUids across from the reticulum to .... (1944), that closure was due to mechanical stimulation in the mOllth and ...

  14. Monitoring of originated polymer in pure monomer with gradient polymer elution chromatography (GPEC)

    NARCIS (Netherlands)

    Staal, W.J.; Cools, P.J.C.H.; Herk, van A.M.; German, A.L.

    1994-01-01

    The anal. of the amt. of polymer in pure monomer with cloudpoint measurements gives only a qual. answer. Now by use of a liq. chromatograph and gradient elution a fully automated detn. the amt. of polymer can be measured and an impression of the molar mass can be achieved

  15. Surfactant-aided size exclusion chromatography

    NARCIS (Netherlands)

    Horneman, D.A.; Wolbers, M.; Zomerdijk, M.; Ottens, M.; Keurentjes, J.T.F.; Wielen, van der L.A.M.

    2004-01-01

    The flexibility and selectivity of size exclusion chromatog. (SEC) for protein purifn. can be modified by adding non-ionic micelle-forming surfactants to the mobile phase. The micelles exclude proteins from a liq. phase similar to the exclusion effect of the polymer fibers of the size exclusion

  16. Shifts in microbial populations in Rusitec fermenters as affected by the type of diet and impact of the method for estimating microbial growth (15N v. microbial DNA).

    Science.gov (United States)

    Mateos, I; Ranilla, M J; Saro, C; Carro, M D

    2017-11-01

    Rusitec fermenters are in vitro systems widely used to study ruminal fermentation, but little is known about the microbial populations establishing in them. This study was designed to assess the time evolution of microbial populations in fermenters fed medium- (MC; 50% alfalfa hay : concentrate) and high-concentrate diets (HC; 15 : 85 barley straw : concentrate). Samples from solid (SOL) and liquid (LIQ) content of fermenters were taken immediately before feeding on days 3, 8 and 14 of incubation for quantitative polymerase chain reaction and automated ribosomal intergenic spacer analysis analyses. In SOL, total bacterial DNA concentration and relative abundance of Ruminococcus flavefaciens remained unchanged over the incubation period, but protozoal DNA concentration and abundance of Fibrobacter succinogenes, Ruminococcus albus and fungi decreased and abundance of methanogenic archaea increased. In LIQ, total bacterial DNA concentration increased with time, whereas concentration of protozoal DNA and abundance of methanogens and fungi decreased. Diet×time interactions were observed for bacterial and protozoal DNA and relative abundance of F. succinogenes and R. albus in SOL, as well as for protozoal DNA in LIQ. Bacterial diversity in SOL increased with time, but no changes were observed in LIQ. The incubated diet influenced all microbial populations, with the exception of total bacteria and fungi abundance in LIQ. Bacterial diversity was higher in MC-fed than in HC-fed fermenters in SOL, but no differences were detected in LIQ. Values of pH, daily production of volatile fatty acids and CH4 and isobutyrate proportions remained stable over the incubation period, but other fermentation parameters varied with time. The relationships among microbial populations and fermentation parameters were in well agreement with those previously reported in in vivo studies. Using 15N as a microbial marker or quantifying total microbial DNA for estimating microbial protein synthesis

  17. Analysis of the Electrical Properties of an Electron Injection Layer in Alq3-Based Organic Light Emitting Diodes.

    Science.gov (United States)

    Kim, Soonkon; Choi, Pyungho; Kim, Sangsub; Park, Hyoungsun; Baek, Dohyun; Kim, Sangsoo; Choi, Byoungdeog

    2016-05-01

    We investigated the carrier transfer and luminescence characteristics of organic light emitting diodes (OLEDs) with structure ITO/HAT-CN/NPB/Alq3/Al, ITO/HAT-CN/NPB/Alq3/Liq/Al, and ITO/HAT-CN/NPB/Alq3/LiF/A. The performance of the OLED device is improved by inserting an electron injection layer (EIL), which induces lowering of the electron injection barrier. We also investigated the electrical transport behaviors of p-Si/Alq3/Al, p-Si/Alq3/Liq/Al, and p-Si/Alq3/LiF/Al Schottky diodes, by using current-voltage (L-V) and capacitance-voltage (C-V) characterization methods. The parameters of diode quality factor n and barrier height φ(b) were dependent on the interlayer materials between Alq3 and Al. The barrier heights φ(b) were 0.59, 0.49, and 0.45 eV, respectively, and the diode quality factors n were 1.34, 1.31, and 1.30, respectively, obtained from the I-V characteristics. The built in potentials V(bi) were 0.41, 0.42, and 0.42 eV, respectively, obtained from the C-V characteristics. In this experiment, Liq and LiF thin film layers improved the carrier transport behaviors by increasing electron injection from Al to Alq3, and the LiF schottky diode showed better I-V performance than the Liq schottky diode. We confirmed that a Liq or LiF thin film inter-layer governs electron and hole transport at the Al/Alq3 interface, and has an important role in determining the electrical properties of OLED devices.

  18. Carbohydrate Intake in Form of Gel Is Associated With Increased Gastrointestinal Distress but Not With Performance Differences Compared With Liquid Carbohydrate Ingestion During Simulated Long-Distance Triathlon.

    Science.gov (United States)

    Sareban, Mahdi; Zügel, David; Koehler, Karsten; Hartveg, Paul; Zügel, Martina; Schumann, Uwe; Steinacker, Jürgen Michael; Treff, Gunnar

    2016-04-01

    The ingestion of exogenous carbohydrates (CHO) during prolonged endurance exercise, such as long-distance triathlon, is considered beneficial with regard to performance. However, little is known about whether this performance benefit differs among different forms of CHO administration. To this end, the purpose of our study was to determine the impact of CHO ingestion from a semisolid source (GEL) on measures of performance and gastrointestinal (GI) comfort compared with CHO ingestion from a liquid source (LIQ). Nine well-trained triathletes participated in this randomized crossover study. Each participant completed a 60-min swim, 180-min bike exercise, and a 60-min all-out run in a laboratory environment under 2 conditions, once while receiving 67.2 ± 7.2 g · h-1 (M ± SD) of CHO from GEL and once while receiving 67.8 ± 4.2 g · h-1 of CHO from LIQ. The amount of fluid provided was matched among conditions. Respiratory exchange ratio (RER), blood glucose, and lactate as well as GI discomfort were assessed at regular intervals during the experiment. The distance covered during the final all-out run was not significantly different among participants ingesting GEL (11.81 ± 1.38 km) and LIQ (11.91 ± 1.53 km; p = .89). RER, blood glucose, and lactate did not differ significantly at any time during the experiment. Seven participants reported GI discomfort with GEL, and no athlete reported GI discomfort with LIQ (p = .016). This study suggests that administration of GEL does not alter long-distance triathlon performance when compared with LIQ, but GEL seems to be associated with reduced GI tolerance. Athletes should consider this a potential disadvantage of GEL administration during long-distance triathlon.

  19. PREFACE: The first 21 years of reverse Monte Carlo modelling—a workshop held in Budapest, Hungary (1-3 October 2009) The first 21 years of reverse Monte Carlo modelling—a workshop held in Budapest, Hungary (1-3 October 2009)

    Science.gov (United States)

    Keen, David A.; Pusztai, László

    2010-10-01

    scientific community by showing the current state-of-the-art research opportunities using the RMC method. Furthermore, by including a small number of papers from colleagues working on similar disordered problems with complementary analysis techniques, we hope that the RMC method may be placed in a broader scientific context. The papers have been arranged in order of increasing structural disorder, starting with studies of crystalline systems, through to amorphous materials and liquids, and ending with RMC developments using small-angle scattering. We are very grateful to IOP Publishing for their willingness to publish this collection of papers which celebrates the 21st anniversary of the first RMC publication in a special issue of Journal of Physics: Condensed Matter and for their co-ordination of the refereeing process. References [1] McGreevy R L 2001 J. Phys.: Condens. Matter 13 R877 [2] Keen D A and Pusztai L (ed) 2007 Proc. of RMC-3 (Budapest, Sept. 2006) J. Phys.: Condens. Matter 19 330301-335223 [3] Keen D A, Pusztai L and Dove M T (ed) 2005 Proc. of RMC-2 (Budapest, Oct. 2003) J. Phys.: Condens. Matter 17 S1-S174 [4] Nguyen T X, Cohaut N, Bae J-S and Bhatia S K 2008 Langmuir 24 7912 [5] Zhang H, Chen B and Banfield J F 2008 Phys. Rev. B 78 214106 [6] Goodwin A L, Calleja M, Conterio M J, Dove M T, Evans J S O, Keen D A, Peters L and Tucker M G 2008 Science 319 794 [7] Norberg S T, Tucker M G and Hull S 2009 J. Appl. Cryst. 42 179 [8] See www.RMCProfile.org, www.RMC-forum.org or www.szfki.hu/~nphys/rmc++/opening.html [9] Haines J, Levelut C, Isambert A, Hébert P, Kohara S, Keen D A, Hammouda T and Andrault D 2009 J. Am. Chem. Soc. 131 12333

  20. Spectroscopic characterisation of biological vaterite: relations to synthetic and geological vaterites

    Science.gov (United States)

    Jacob, D. E.; Wehrmeister, U.; Soldati, A. L.; Hofmeister, W.

    2009-04-01

    band ?1 into three distinct bands, activation and splitting of ?2 and splitting of both, ?3 and ?4 into six distinct Raman bands. FWHMs of the lattice modes are large (8 cm-1- 44 cm-1) compared to those of aragonite, implying that the structure is not well ordered and possibly affected by stacking faults, layer shifts or syntactic intergrowth; irregularities that further complicate the crystal structure determination. Correlation of Mg-contents in vaterite areas in freshwater cultured pearls with Raman spectra obtained at the same spots show that the FWHMs are influenced by the magnesium content. Similarly, the spectra for the vaterite samples synthesized with differing Mg contents show successively increasing FWHM with increasing magnesium content both for the lattice modes and the ?1 - symmetric stretching mode. Wehrmeister et al., 2007. J. Gemmology; 31: 269-276, Falini et al., 2005. Eur. J. Inorg. Chem. 2005(1): 162 -167, Meyer, H. 1969. Angew. Chem. 21: 678-679, Kamhi, S., 1963. Acta Cryst. (1963).16: 770 - 772, Meyer, H., 1969. Z. Kristallographie 128: 183 - 212, Lippmann, F., 1973. New York, Springer, Soldati et al., 2008. Min. Mag. 72: 577- 590, Jacob et al., 2008. Geochim. Cosmochim. Acta 72: 5401- 5415, Loges et al., 2006. Langmuir 22: 3073-3080.

  1. EDITORIAL: Nanotechnology in vivo Nanotechnology in vivo

    Science.gov (United States)

    Demming, Anna

    2010-04-01

    of nanoparticles in the tumour vasculature. However, previous reports on techniques to generate nanobubbles have either been slow or problematic due to the resulting development of cardiac dimension reduction, hypotension and tachycardia. Xing and colleagues have now demonstrated the use of polyoxyethylene 40 stearate, which is known to be biocompatible, degradable and non-toxic, as an alternative surfactant for generating nanobubbles. In the early 1980s scanning probe micrographs of nanosized features unleashed the power of imaging to push forward the science of structures and mechanisms at the nanoscale. The continued development of new and increasingly sophisticated nanoparticles and systems looks set to empower medicine in the same way, providing further means to exploit the mechanistic nature of biological organisms for better health and longevity. References [1] Leon R, Petroff P M, Leonard D and Fafard S 1995 Science 267 1966-8 [2] Nie Q, Tan W B and Zhang Y 2006 Nanotechnology 17 140-4 [3] Li L, Chen D, Zhang Y, Deng Z, Ren X, Meng X, Tang F, Ren J and Zhang L 2007 Nanotechnology 18 405102 [4] Fujioka K et al 2008 Nanotechnology 19 415102 [5] Shinoda K, Yangisawa S, Sato K amd Hirakuri K 2006 J. Cryst. Growth 288 84-6 [6] Manzoor K, Johny S, Thomas D, Setua S, Menon D and Nair S 2009 Nanotechnology 20 065102 [7] Hu R, Yong K-T, Roy I, Ding H, Law W-C, Cai H, Zhang X, Vathy L A, Bergey E J and Prasad P N 2010 Nanotechnology 21 145105 [8] Xing, Z, Ke H, Wang J, Zhao B, Yue X, Dai Z and Liu J 2010 Nanotechnology 21 145607

  2. Fractional Consumption of Liquid Hydrogen and Liquid Oxygen During the Space Shuttle Program

    Science.gov (United States)

    Partridge, Jonathan K.

    2011-01-01

    The Space Shuttle uses the propellants, liquid hydrogen and liquid oxygen, to meet part of the propulsion requirements from ground to orbit. The Kennedy Space Center procured over 25 million kilograms of liquid hydrogen and over 250 million kilograms of liquid oxygen during the 3D-year Space Shuttle Program. Because of the cryogenic nature of the propellants, approximately 55% of the total purchased liquid hydrogen and 30% of the total purchased liquid oxygen were used in the Space Shuttle Main Engines. The balance of the propellants were vaporized during operations for various purposes. This paper dissects the total consumption of liqUid hydrogen and liqUid oxygen and determines the fraction attributable to each of the various processing and launch operations that occurred during the entire Space Shuttle Program at the Kennedy Space Center.

  3. The impact of liquidity on bank profitability

    OpenAIRE

    Bordeleau, Etienne; Graham, Christopher

    2010-01-01

    The recent crisis has underlined the importance of sound bank liquidity management. In response, regulators are devising new liquidity standards with the aim of making the financial system more stable and resilient. In this paper, the authors analyse the impact of liquid asset holdings on bank profitability for a sample of large U.S. and Canadian banks. Results suggest that profitability is improved for banks that hold some liquid assets, however, there is a point at which holding further liq...

  4. Thermodynamic and structural properties of high temperature solid and liquid EuBr2

    DEFF Research Database (Denmark)

    Rycerz, L.; Gadzuric, S.; Ingier-Stocka, E.

    2005-01-01

    Heat capacity of solid and liq. EuBr2 was measured by differential scanning calorimetry in the temp. range 300-1100 K. The temp. and enthalpy of fusion were also detd. exptl. By combination of these results with the literature data on the entropy at 298.15 K, S(o,m) (EuBr2, s, 298.15 K) , and the...

  5. Rheology of dense suspensions of non colloidal particles

    OpenAIRE

    Guazzelli , Elisabeth

    2017-01-01

    International audience; Dense suspensions are materials with broad applications both in industrial processes (e.g. waste disposal, concrete, drilling muds, metalworking chip transport, and food processing) and in natural phenomena (e.g. flows of slurries, debris, and lava). Despite its long research history and its practical relevance, the mechanics of dense suspensions remain poorly understood. The major difficulty is that the grains interact both by hydrodynamic interactions through the liq...

  6. Fulltext PDF

    Indian Academy of Sciences (India)

    It is a general knowledge that the defects in solids and liquids play an important role and help one to understand the diffusion mechanism whereas the pressure ..... [14] T Groß, J Buchhauser, W E Price, I N Tarassob and H D Lüdemann, J. Mol. Liq. 73–74, 433 (1997). [15] N Karger, S Wappmann, N Shaker-Gaafar and H D ...

  7. Physics of Beer Tapping

    OpenAIRE

    Rodríguez-Rodríguez , Javier; Casado-Chacón , Almudena; Fuster , Daniel

    2014-01-01

    International audience; The popular bar prank known in colloquial English as beer tapping consists in hitting the top of a beer bottle with a solid object, usually another bottle, to trigger the foaming over of the former within a few seconds. Despite the trick being known for long time, to the best of our knowledge, the phenomenon still lacks scientific explanation. Although it seems natural to think that shock-induced cavitation enhances the diffusion of CO2 from the supersaturated bulk liq...

  8. Pleural liquid and its exchanges.

    Science.gov (United States)

    Agostoni, Emilio; Zocchi, Luciano

    2007-12-15

    After an account on morphological features of visceral and parietal pleura, mechanical coupling between lung and chest wall is outlined. Volume of pleural liquid is considered along with its thickness in various regions, and its composition. Pleural liquid pressure (P(liq)) and pressure exerted by lung recoil in various species and postures are then compared, and the vertical gradient of P(liq) considered. Implications of lower P(liq) in the lung zone than in the costo-phrenic sinus at iso-height are pointed out. Mesothelial permeability to H(2)O, Cl(-), Na(+), mannitol, sucrose, inulin, albumin, and various size dextrans is provided, along with paracellular "pore" radius of mesothelium. Pleural liquid is produced by filtration from parietal pleura capillaries according to Starling forces. It is removed by absorption in visceral pleura capillaries according to Starling forces (at least in some species), lymphatic drainage through stomata of parietal mesothelium (essential to remove cells, particles, and large macromolecules), solute-coupled liquid absorption, and transcytosis through mesothelium.

  9. Component Selection, Accelerated Testing, and Improved Modeling of AMTEC Systems for Space Power (abstract)

    Science.gov (United States)

    Williams, R. M.; Jeffries-Nakamura, B.; Ryan, M. A.; Underwood, M. L.; Suitor, J.; O'Connor, D.

    1993-01-01

    Alkali metal thermal to electric converter (AMTEC) designs for space power are numerous, but selection of materials for construction of long-lived AMTEC devices has been limited to electrodes, current collectors, and the solid electrolyte. AMTEC devices with lifetimes greater than 5 years require careful selection and life testing of all hot-side components. The likely selection of a remote condensed design for initial flight test and probable use with a GPHS in AMTEC powered outer planet probes requires the device to be constructed to tolerate T greater than 1150K, as well as exposure to Na(sub (g)), and Na(sub (liq)) on the high pressure side. The temperatures involved make critical high strength and chemical resistance to Na containing Na(sub 2)O. Selection among materials which can be worked should not be driven by ease of fabricability, as high temperature stability is the critical issue. These concepts drive the selection of Mo alloys for Na(sub (liq)) containment in AMTEC cells for T to 1150K operation, as they are significantly stronger than comparable NB or Ta alloys, are less soluble in Na(sub (liq)) containing dissolved Na(sub 2)O, are workable compared to W alloys (which might be used for certain components), and are ductile at the T greater than 500K of proposed AMTEC modules in space applications.

  10. Dosimetric investigation depending on tumor location in patient breast in partial breast irradiation

    International Nuclear Information System (INIS)

    Kim, Min Joo; Park, So Hyun; Jung, Joo Young; Woong, Cho; Suh, Tae Suk

    2012-01-01

    The Partial Breast Irradiation (PBI) technique, which involves radiation beam delivery techniques that use a limited range of treatment volumes, has been a challenging approach that is worthy of consideration compared to whole-breast radiation therapy (WBRT). Because of a small target volumes used in the PBI technique, the radiation dose can be safely delivered to the targeted tissue without the unwanted delivery of radiation to normal breast tissues and organ at risk (OAR), such as contralateral breast, lung and heart.Through PBI technique, better cosmetic outcomes and minimizing damages to OARs could be expected and also the daily dose can be increased with smaller number of fractionation in radiation therapy. The purpose of this study was to evaluate the dosimetric effects according to tumor locations in patient's breast for Partial Breast Irradiation (PBI) technique using three Dimensional Conformal Radiation Therapy (3DCRT), Electron Beam Radiation therapy (EBRT) and Helical-tomotherapy (H-TOMO). Dosimetric comparisons of PBI technique for 3DCRT, EBRT, and H-TOMO depending on the classified tumor locations were performed. H-TOMO delivered the low dose to lager volume to surrounding normal tissue, such as the heart and lungs compared to 3DCRT and EBRT although it had the same degree of target coverage as the other methods (3DCRT, EBRT). EBRT had a curative effect for early-stage breast cancers located in the lower and inner sections (LIQ-S, LIQ-D)

  11. Cooperative and competitive concurrency in scientific computing. A full open-source upgrade of the program for dynamical calculations of RHEED intensity oscillations

    Science.gov (United States)

    Daniluk, Andrzej

    2011-06-01

    problems of this type, the computational and threading layers of the project have been implemented in the form of one design pattern as a part of Model-View-Controller architecture. Reasons for new version: Responding to the users' feedback the Growth09 project has been upgraded to a standard that allows the carrying out of sample computations of the RHEED intensities for a disordered surface for a wide range of single- and epitaxial hetero-structures. The design pattern on which the project is based has also been improved. It is shown that this model can be effectively used for multithreaded growth simulations of thin epitaxial layers and corresponding RHEED intensities for a wide range of single- and hetero-structures. Responding to the users' feedback the present release has been implemented using a well-documented free compiler [1] not requiring the special configuration and installation additional libraries. Summary of revisions: The logical structure of the Growth09 program has been modified according to the scheme showed in Fig. 1. The class diagram in Fig. 1 is a static view of the main platform-specific elements of the GrowthCP architecture. Fig. 2 provides a dynamic view by showing the creation and destruction simplistic sequence diagram for the process. The program requires the user to provide the appropriate parameters in the form of a knowledge base for the crystal structures under investigation. These parameters are loaded from the parameters. ini files at run-time. Instructions to prepare the .ini files can be found in the new distribution. The program enables carrying out different growth models and one-dimensional dynamical RHEED calculations for the fcc lattice with basis of three-atoms, fcc lattice with basis of two-atoms, fcc lattice with single atom basis, Zinc-Blende, Sodium Chloride, and Wurtzite crystalline structures and hetero-structures, but yet the Fourier component of the scattering potential in the TRHEEDCalculations.crystPotUgXXX() procedure

  12. Tumour location within the breast: Does tumour site have prognostic ability?

    Science.gov (United States)

    Rummel, Seth; Hueman, Matthew T; Costantino, Nick; Shriver, Craig D; Ellsworth, Rachel E

    2015-01-01

    Tumour location within the breast varies with the highest frequency in the upper outer quadrant (UOQ) and lowest frequency in the lower inner quadrant (LIQ). Whether tumour location is prognostic is unclear. To determine whether tumour location is prognostic, associations between tumour site and clinicopathological characteristics were evaluated. All patients enrolled in the Clinical Breast Care Project whose tumour site-UOQ, upper inner quadrant (UIQ), central, LIQ, lower outer quadrant (LOQ)-was determined by a single, dedicated breast pathologist were included in this study. Patients with multicentric disease (n = 122) or tumours spanning multiple quadrants (n = 381) were excluded from further analysis. Clinicopathological characteristics were analysed using chi-square tests for univariate analysis with multivariate analysis performed using principal components analysis (PCA) and multiple logistic regression. Significance was defined as P location, 30 had bilateral disease. Tumour location in the UOQ (51.5%) was significantly higher than in the UIQ (15.6%), LOQ (14.2%), central (10.6%), or LIQ (8.1%). Tumours in the central quadrant were significantly more likely to have higher tumour stage (P = 0.003) and size (P location as a prognostic factor revealed that although tumours in the central region are associated with less favourable outcome, these associations are not independent of location but rather driven by larger tumour size. Tumours in the central region are more difficult to detect mammographically, resulting in larger tumour size at diagnosis and thus less favourable prognosis. Together, these data demonstrate that tumour location is not an independent prognostic factor.

  13. Decrease in electrical resistivity on depletion of islands of mobility during aging of a bulk metal glass

    Science.gov (United States)

    Aji, Daisman P. B.; Johari, G. P.

    2018-04-01

    The effect of structural relaxation on electrical resistivity, ρglass, of strain-free Zr46.75Ti8.25Cu7.5Ni10Be27.5 bulk metallic glass was studied during isothermal aging at several temperatures, Tas. Since cooling of a liquid metal increases its resistivity ρliq, one expects ρglass to increase on aging toward ρliq at T = Ta. Instead, ρglass decreased non-exponentially with the aging time. The activation energy of aging kinetics is 189 kJ mol-1, which is higher than the activation energy of the Johari-Goldstein (JG) relaxation. After considering the sample's contraction, phase separation, and crystallization as possible causes of the decrease in ρglass, we attribute the decrease to depletion of islands of atomic mobility, soft spots, or static heterogeneity. Vibrations of the atoms in these local (loosely packed) regions and in the region's interfacial area contribute to electron scattering. As these deplete on aging, the contribution decreases and ρglass decreases, with a concomitant decrease in macroscopic volume, enthalpy, and entropy (V, H, and S). Local regions of faster mobility also decrease on cooling as V, H, and S of a liquid decrease, but structure fluctuations dominate electron scattering of a liquid metal and ρliq increases effectively according to the Ziman-Nagel theory for a homogenously disordered structure. Whether depletion of such local regions initiates the structural relaxation of a glass, or vice versa, may be resolved by finding a glass that physically ages but shows no JG relaxation.

  14. Catalytic Hydrothermal Conversion of Wet Biomass Feedstocks and Upgrading – Process Design and Optimization

    DEFF Research Database (Denmark)

    Hoffmann, Jessica; Toor, Saqib; Rosendahl, Lasse

    Liquid biofuels will play a major role for a more sustainable energy system of the future. The CatLiq® process is a 2nd generation biomass conversion process that is based on hydrothermal liquefaction. Hydrothermal liquefaction offers a very efficient and feedstock flexible way of converting...... biomass to bio-oil. Bio-oils from hydrothermal liquefaction are characterised by their high feedstock flexibility. Upgrading of complete bio-oils derived from hydrothermal conversion has not yet been extensively studied. Purpose of this work is to reduce the oxygen content of the bio-oil to improve...

  15. Randomly grain growth in metallic materials

    Energy Technology Data Exchange (ETDEWEB)

    Ramirez, A. [Instituto Politecnico Nacional, (SEPI-ESIME), Unidad Profesional Ticoman, Av. Ticoman 600, Del. G.A.M., C.P. 07340 Distrito Federal, Mexico (Mexico); Instituto Politecnico Nacional, (SEPI-ESIQIE), Unidad Profesional Zacatenco, Edif. 6 y Edif. Z planta baja C.P.07300, Distrito Federal, Mexico (Mexico)], E-mail: adaramil@yahoo.com.mx; Chavez, F. [Instituto Politecnico Nacional, (SEPI-ESIQIE), Unidad Profesional Zacatenco, Edif. 6 y Edif. Z planta baja C.P.07300, Distrito Federal, Mexico (Mexico); Demedices, L. [Instituto Politecnico Nacional, (SEPI-ESIME), Unidad Profesional Ticoman, Av. Ticoman 600, Del. G.A.M., C.P. 07340 Distrito Federal, Mexico (Mexico); Instituto Politecnico Nacional, (SEPI-ESIQIE), Unidad Profesional Zacatenco, Edif. 6 y Edif. Z planta baja C.P.07300, Distrito Federal, Mexico (Mexico); Cruz, A.; Macias, M. [Instituto Politecnico Nacional, (SEPI-ESIQIE), Unidad Profesional Zacatenco, Edif. 6 y Edif. Z planta baja C.P.07300, Distrito Federal, Mexico (Mexico)

    2009-10-30

    Computational modeling of grain structures is a very important topic in materials science. In this work, the development of the computational algorithms for a mathematical model to predict grain nucleation and grain growth is presented. The model place a number of nucleated points randomly in a liquid pool according with the solid and liquid fractions (X{sub sol} and X{sub liq}) of metal solute and the local temperature distribution (SS{sub I,J}). Then these points grows isotropically until obtain a grain structure with straight interfaces. Different grain morphologies such as columnar and equiaxed can be obtained as a function of the temperature distributions and growth directions.

  16. Identification and Quantification of the Water Soluble Components of JP-4 and a Determination of Their Biological Effects upon Selected Freshwater Organisms.

    Science.gov (United States)

    1981-11-30

    minutes. Absorbances ere read at 630am on a Perkin-Elmer (Coleman 124) double beam speztrophotonater and compared to a standard curve made from para ... aminophenol (PAP), 0.05mg to 0-00oll Q- "lagM.Lnat RfteklpMi4I &&all UndWE 0.5m1 of aninopyrine stock solution (7.0mg/mI buffer) was added to the...on the HPLC column mill be collected and counted in a liq- uid scintillation counter G. Scanning electron microscopy will be used for studying gross

  17. Air Force Operational Medicine: Using the Estimating Supplies Program to Develop Materiel Solutions for the Operational Clinical Requirements of the Expeditionary Medical Support (EMEDS). Volume Three: EMEDS+10

    Science.gov (United States)

    2009-11-01

    1,480.50 D 7420011828535 CALCULATOR ELECTRONIC SOLAR CELL 8 DIGIT LIQ EA 1.00 0.00 1.15 0.15 $12.63 0.00 0.00 0.00 A 7240000893827 CAN WATER MILITARY PLAS...4110014974328 RECORDER TEMP BLD PLASM FRZER 115V 11.5 CU EA 1.00 1.00 120.00 14.00 $7,212.00 120.00 14.00 $7,212.00 A 4110012494476 REFRIGERATOR

  18. Randomly grain growth in metallic materials

    International Nuclear Information System (INIS)

    Ramirez, A.; Chavez, F.; Demedices, L.; Cruz, A.; Macias, M.

    2009-01-01

    Computational modeling of grain structures is a very important topic in materials science. In this work, the development of the computational algorithms for a mathematical model to predict grain nucleation and grain growth is presented. The model place a number of nucleated points randomly in a liquid pool according with the solid and liquid fractions (X sol and X liq ) of metal solute and the local temperature distribution (SS I,J ). Then these points grows isotropically until obtain a grain structure with straight interfaces. Different grain morphologies such as columnar and equiaxed can be obtained as a function of the temperature distributions and growth directions.

  19. Luminescent hybrid materials based on (8-hydroxyquinoline)-substituted metal-organic complexes and lead-borate glasses

    Science.gov (United States)

    Petrova, Olga B.; Anurova, Maria O.; Akkuzina, Alina A.; Saifutyarov, Rasim R.; Ermolaeva, Ekaterina V.; Avetisov, Roman I.; Khomyakov, Andrew V.; Taydakov, Ilya V.; Avetissov, Igor Ch.

    2017-07-01

    Novel luminescent organic-inorganic hybrid materials based on 8-hydroxyquinoline metal complexes (Liq, Kq, Naq, Rbq, Mgq2, Srq2, Znq2, Scq3, Alq3, Gaq3, and Inq3) have been synthesized by a high temperature exchange reaction with 80PbF2-20B2O3 inorganic low-melting glass. The mechanical and optical properties, transmission spectra, emission an excitation photoluminescence, and luminescence kinetic of hybrid materials were studied. All hybrid materials showed a wide luminescence band in the range 400-700 nm.

  20. Ensuring sustainability in developing world biofuel productoin

    CSIR Research Space (South Africa)

    Von Maltitz, Graham P

    2009-06-01

    Full Text Available el N at io n al an d in te rn at io n al liq u id fu el s bl en ds Type 1 projects E.g. Mali Folkecentre Ghana Dumpong Biofuels See text box A and B Type 4 projects E.g. Large scale commercial plantations... approach Mali farmer growing jatropha as a fuel source to fuel 3 X 100 KW generators that will provide power to his village Brazilian ethanol production from large scale mechanised sugar cane fields Is certification and setting...

  1. Mucocele frontal com extensão intracraniana: a propósito de dois casos

    Directory of Open Access Journals (Sweden)

    Oswaldo Ricciardi Cruz

    1960-03-01

    Full Text Available O autor apresenta dois casos de mucocele frontal com extensão intracraniana. Em um dos casos existia hipertensão intracraniana e quadro angiográfico normal; no outro, os valores tensionais do liqüido cefalorraquidiano eram normais e o exame angiográfico demonstrou a presença de um tumor de localização frontal. Em ambos os casos foi utilizada a via frontal - craniotomia osteoplástica - para o acesso intracraniano. O contato do material contido no cisto com as meninges não determinou alterações meningencefalíticas.

  2. Synthesis and characterization of pure and Li⁺ activated Alq₃ complexes for green and blue organic light emitting diodes and display devices.

    Science.gov (United States)

    Bhagat, S A; Borghate, S V; Kalyani, N Thejo; Dhoble, S J

    2014-08-01

    Pure and Li(+)-doped Alq3 complexes were synthesized by simple precipitation method at room temperature, maintaining the stoichiometric ratio. These complexes were characterized by X-ray diffraction, ultraviolet-visible absorption and Fourier transform infrared and photoluminescence (PL) spectra. X-ray diffraction analysis reveals the crystalline nature of the synthesized complexes, while Fourier transform infrared spectroscopy confirm the molecular structure, the completion of quinoline ring formation and presence of quinoline structure in the metal complex. Ultraviolet-visible and PL spectra revealed that Li(+) activated Alq3 complexes exhibit the highest intensity in comparison to pure Alq3 phosphor. Thus, Li(+) enhances PL emission intensity when doped into Alq3 phosphor. The excitation spectra lie in the range of 383-456 nm. All the synthesized complexes other than Liq give green emission, while Liq gives blue emission with enhanced intensity. Thus, he synthesized phosphors are the best suitable candidates for green- and blue-emitting organic light emitting diode, PL liquid-crystal display and solid-state lighting applications. Copyright © 2013 John Wiley & Sons, Ltd.

  3. A thermodynamic investigation of liquid gold-antimony alloys

    International Nuclear Information System (INIS)

    Hayer, E.; Castanet, R.

    1995-01-01

    The enthalpies of mixing of liquid Au-Sb alloys were determined between 906 and 1028 K giving Δ mix H o m = x Sb x Au (-11.234-1.1078x Sb + 5.713x Sb 2 ) kJ mol -1 . The minimum was found at x Sb = 0.45 with Δ mix H o m = -2.62 ± 0.2 kJ mol -1 contrary to published measurements on liquid Au-Sb alloys. The limiting partial molar enthalpy of Au in Sb at 935 K was measured to Δ mix h o m (Au, liq, in ∞Sb, liq) = -6.05 ± 0.4 kJ mol -1 . The enthalpy of formation of the solid compound AuSb 2 determined at 298 K by solution calorimetry in liquid Sb, Δ f H o m (AuSb 2 ) = -5.40 ± 0.6 kJ mol -1 , is found in fair agreement with literature data. DTA measurements were performed on the Au-rich part of the liquidus and a new liquidus curve is suggested between Au and the eutectic concentration. The eutectic point was found at 630.37 ± 0.25 K and x Sb 0.350. (orig.)

  4. Probing of the isospin-dependent mean field and nucleon-nucleon cross section in a medium by nucleon emissions

    International Nuclear Information System (INIS)

    Liu Jianye; Xing Yongzhong; Guo Wenjun

    2003-01-01

    We study the isospin effects of the mean field and two-body collision on the nucleon emissions at the intermediate energy heavy-ion collisions by using an isospin-dependent transport theory. The calculated results show that the nucleon emission number N n depends sensitively on the isospin effect of nucleon-nucleon cross section and weakly on the isospin-dependent mean field for neutron-poor system in higher beam energy region. In particular, the correlation between the medium correction of two-body collision and the momentum-dependent interaction enhances the dependence of nucleon emission number N n on the isospin effect of nucleon-nucleon cross section. On the contrary, the ratio of the neutron-proton ratio of the gas phase to the neutron-proton ratio of the liquid phase, i.e., the degree of isospin fractionation [(N/Z) gas ] b /[(N/Z) liq ] b depends sensitively on the isospin-dependent mean field and weakly on the isospin effect of two-body collision for neutron-rich system in the lower beam energy region. In this case, N n and [(N/Z) gas ] b /[(N/Z) liq ] b are the probes for extracting the information about the isospin-dependent nucleon-nucleon cross section in the medium and the isospin-dependent mean field, respectively

  5. Electron injection mechanisms of green organic light-emitting devices fabricated utilizing a double electron injection layer consisting of cesium carbonate and fullerene

    International Nuclear Information System (INIS)

    Yang, J.S.; Choo, D.C.; Kim, T.W.; Jin, Y.Y.; Seo, J.H.; Kim, Y.K.

    2010-01-01

    Electron injection mechanisms of the luminance efficiency of green organic light-emitting devices (OLEDs) fabricated utilizing a cesium carbonate (Cs 2 CO 3 )/fullerene (C 60 ) heterostructure acting as an electron injection layer (EIL) were investigated. Current density-voltage and luminance-voltage measurements showed that the current densities and the luminances of the OLEDs with a Cs 2 CO 3 or Cs 2 CO 3 /C 60 EIL were higher than that of the OLEDs with a Liq EIL. The luminance efficiency of the OLEDs with a Cs 2 CO 3 EIL was almost three times higher than that of the OLEDs with a Liq EIL. Because the electron injection efficiency of the Cs 2 CO 3 layer in OLEDs was different from that of the C 60 layer, the luminance efficiency of the OLEDs with a double EIL consisting of a Cs 2 CO 3 layer and a C 60 layer was smaller than that of the OLEDs with a Cs 2 CO 3 EIL. The electron injection mechanisms of OLEDs with a Cs 2 CO 3 and C 60 double EIL are described on the basis of the experimental results.

  6. Low-voltage and high-efficiency white organic light emitting devices with carrier balance

    International Nuclear Information System (INIS)

    Wei Fuxiang; Huang, Y.; Fang, L.

    2010-01-01

    White organic light emitting devices with the structure of ITO/m-MTDATA:x%4F-TCNQ/NPB/TBADN:EBDP:DCJTB/Bphen:Liq/LiF/Al have been demonstrated in this paper. High-mobility m-MTDATA:4F-TCNQ is added into the region between ITO and NBP to increase hole injection and transport. The high-mobility Bphen:Liq layer is added into the region between cathode and emission layers to lower cathode barrier and facilitate carrier injection. In the meanwhile, an effective carrier balance (number of holes is equal to number of electrons) between holes and electrons is considered to be one of the most important factors for improving OLEDs. During the experiment, by modulating the doping concentration of 4F-TCNQ, we can control hole injection and transport to make the carriers reach a high-level balance. The maximum current efficiency and power efficiency of devices were 9.3 cd/A and 4.6 lm/A, respectively.

  7. Calculation of Oxygen Fugacity in High Pressure Metal-Silicate Experiments and Comparison to Standard Approaches

    Science.gov (United States)

    Righter, K.; Ghiorso, M.

    2009-01-01

    Calculation of oxygen fugacity in high pressure and temperature experiments in metal-silicate systems is usually approximated by the ratio of Fe in the metal and FeO in the silicate melt: (Delta)IW=2*log(X(sub Fe)/X(sub FeO)), where IW is the iron-wustite reference oxygen buffer. Although this is a quick and easy calculation to make, it has been applied to a huge variety of metallic (Fe- Ni-S-C-O-Si systems) and silicate liquids (SiO2, Al2O3, TiO2, FeO, MgO, CaO, Na2O, K2O systems). This approach has surely led to values that have little meaning, yet are applied with great confidence, for example, to a terrestrial mantle at "IW-2". Although fO2 can be circumvented in some cases by consideration of Fe-M distribution coefficient, these do not eliminate the effects of alloy or silicate liquid compositional variation, or the specific chemical effects of S in the silicate liquid, for example. In order to address the issue of what the actual value of fO2 is in any given experiment, we have calculated fO2 from the equilibria 2Fe (metal) + SiO2 (liq) + O2 = Fe2SiO4 (liq).

  8. Particle processing technology

    Science.gov (United States)

    Sakka, Yoshio

    2014-02-01

    . Mater. 12 013001 [3] Sakka Y and Uchikoshi T 2010 KONA Powder Particle J. 28 74 (kona.or.jp/search/28_074.pdf) [4] Naguib M, Mashtalir O, Carle J, Presser V, Lu J, Hultman L, Gogotsi Y and Barsoum M W 2012 ACS Nano 6 1322 [5] Sakka Y and Suzuki T S 2005 J. Ceram. Soc. Japan 113 26 [6] Grasso S, Sakka Y and Maizza G 2009 Sci. Technol. Adv. Mater. 10 053001 [7] Nakao H, Tokonami S, Hamada T, Shiigi H, Nagaoka T, Iwate F and Takeda Y 2012 Nanoscale 4 6814 [8] Miyazawa K and Hotta K 2010 J. Cryst. Growth 312 2764 [9] Suehiro T, Xie R and Hirosaki N 2013 Indust. Eng. Chem. Res. 52 7453 [10] Zhu Q, Li J-G, Li X, Sun X and Sakka Y 2011 Sci. Technol. Adv. Mater. 12 055001 [11] Li J, Li J-G, Zhang Z, Wu X, Liu S, Li X, Sun X and Sakka Y 2012 Sci. Technol. Adv. Mater. 13 035007 [12] Kawamura F, Yusa H and Taniguchi T 2012 Appl. Phys. Lett. 100 251910 [13] Watanabe K and Taniguchi T 2011 Int. J. Appl. Ceram. Technol. 8 977 [14] Deng Z-Y, Ferreira J M F and Sakka Y 2008 J. Am. Ceram. Soc. 91 3825 [15] Uda M, Okuyama H, Suzuki T S and Sakka Y 2012 Sci. Technol. Adv. Mater. 13 025009 [16] Takeya H, Kato R, Wakahara T, Miyazawa K, Yamaguchi T, Ozaki T, Okazaki H and Takano Y 2013 Mater. Res. Bull. 48 343 [17] Wakahara T, D'Angelo P, Miyazawa K, Nemoto Y, Ito O, Tanigaki N, Bradley D D C and Anthopoulos T D 2012 J. Am. Chem. Soc. 134 7204 [18] Wiecinska P, Sakka Y, Suzuki T S, Uchikoshi T, Mizerski T and Szafran M 2013 J. Ceram. Soc. Japan 121 89 [19] Kawakita M, Uchikoshi T, Kawakita J and Sakka Y 2009 J. Am. Ceram. Soc. 92 984 [20] Hu C, Sakka Y, Grasso S, Nishimura T, Guo S and Tanaka H 2011 Scr. Mater. 64 765 [21] Hu C, Sakka Y, Nishimura T, Guo S, Grasso S and Tanaka H 2011 Sci. Technol. Adv. Mater. 12 044603 [22] Kakisawa H and Sumitomo T 2011 Sci. Technol. Adv. Mater. 12 064710 [23] Grasso S, Hu C F, Maizza G, Kim B N and Sakka Y 2011 J. Am. Ceram. Soc. 94 1405 [24] Grasso S, Kim B N, Hu C F, Maizza G and Sakka Y 2010 J. Am. Ceram. Soc. 93 2460 [25] Zhang H B, Kim B N, Morita K

  9. FOREWORD: Heterogenous nucleation and microstructure formation—a scale- and system-bridging approach Heterogenous nucleation and microstructure formation—a scale- and system-bridging approach

    Science.gov (United States)

    Emmerich, H.

    2009-11-01

    : Springer) [2] Mutaftschiev B 1993 Handbook on Crystal Growth ed D T J Hurle (Amsterdam: North-Holland) p 187 [3] Lacmann R and Schmidt P 1977 Current Topics in Materials Science ed E Kaldis and H J Scheel (Amsterdam: North-Holland) vol 2, pp 301-25 [4] Skripov V P 1977 Current Topics in Materials Scierce ed by E Kaldis and H J Scheel (Amsterdam: North-Holland) 327-78 [5] Chayen N E 1997 J. Appl. Crystallogr. 30 198 [6] Cho J and Thompson C V 1989 Appl. Phys. Lett. 54 2577 [7] Boettinger W J, Coriell S R, Greer A L, Karma A, Kurz W, Rappaz M, and Trivedi R 2000 Acta mater. 48 43 [8] www.spp1296.rwth-aachen.de [9] Volmer M and Weber A 1926 Z. Phys. Chemie. 119 227 [10] Becker R and Döring W 1935 Ann. Phys. 24 719 [11] Turnbull D and Fisher J C 1949 J. Chem. Phys. 17 71 [12] Oxtoby D W 1992 J. Phys.: Condens. Matter 4 7627 [13] Gránásy L and Iglói F 1997 J. Chem. Phys. 107 3634 [14] Gránásy L, Börzsönyi T, Pusztai T 2003 Interface and Transport Dynamics ed H Emmerich, B Nestler and M Schreckenberg (Berlin: Springer) p 190 [15] Emmerich H and Siquieri R 2005 Numerical Heat Transfer ed A Nowack and R A Bialecki [16] Gránásy L 1993 J. Non-Cryst. Solids 162 301 Dragnevski K I, Cochrane R F and Mullis A 2004 Mat. Sci. Eng. A 375-377 479 [17] Sood A K 1991 Solid State Physics 45 1

  10. Temperatures and Melt Water Contents at the Onset of Phenocryst Growth in Quaternary Nepheline-Normative Basalts Erupted along the Tepic-Zacoalco Rift in Western Mexico

    Science.gov (United States)

    Mesa, J.; Lange, R. A.; Pu, X.

    2017-12-01

    Nepheline-normative, high-Mg basalts erupted from the western Mexican arc, along the Tepic-Zacoalco rift (TZR), have a trace-element signature consistent with an asthenosphere source, whereas calc-alkaline basalts erupted from the central Mexican arc in the Michoacan-Guanajuato volcanic field (MGVF) have a trace-element signature consistent with a mantle source strongly affected by subduction fluids. In this study, olivine-melt thermometry and plagioclase-liquid hygrometry are used to constrain the temperature and melt water content of the alkaline TZR basalts. The presence of diffusion-limited growth textures in olivine and plagioclase phenocrysts provide preliminary evidence of rapid growth during ascent. For each basalt sample, a histogram of all analyzed olivines in each sample allows the most Fo-rich composition to be identified, which matches the calculated composition at the liquidus via MELTS (Ghiorso & Sack, 1995; Asimow & Ghiorso, 1998) at fO2 values of QFM +2. Therefore a newly developed olivine-melt thermometer, based on DNiol/liq (Pu et al., 2017) was used to calculate temperature at the onset of olivine crystallization during ascent. Temperatures range from 1076-1247°C, whereas those calculated using an olivine-melt thermometer based on DMgol/liq range from 1141-1236 °C. Olivine-melt thermometers based on DMgol/liq are sensitive to melt H2O content, therefore ΔT = TMg - TNi (≤ 82 degrees) may be used as a qualitative indicator of melt H2O (≤ 2.6 wt% H2O; Pu et al., 2017). When temperatures from the Ni-thermometer are applied to the most calcic plagioclase in each sample (Waters & Lange, 2015), calculated melt H2O contents range from 1.3-1.9 (± 0.4) wt%. These values are significantly lower than those obtained from high-Mg calc-alkaline basalts from the MGVF using similar methods (1.9-5.0 wt%; Pu et al., 2017), consistent with a reduced involvement of slab-derived fluids in the origin of the alkaline TZR basalts from western Mexico.

  11. Model for definition of heat transfer coefficient in an annular two-phase flow

    International Nuclear Information System (INIS)

    Khun, J.

    1976-01-01

    Near-wall heat exchange in a vertical tube at high vapor velocity in a two-phase vapor and liquid flow is investigated. The flow divides inside the tube into a near-wall liquid film and a vapor nucleus containing liquid droplets, with the boundaries being uniform. The liquid film thickness determines the main resistance during heat transfer between the wall and vapor nucleus. The theoretical model presented is verified in water vaporization experiments, the R12 cooling agent and certain hydrocarbons. The loss of friction pressure is determined by the Lockart-Martinelli method. The approximately universal Carman velocity profile is used to evaluate the velocity in film, and basing on this, film thickness is determined. The parameter ranges were: Resub(vap)=10 4 -3x10 6 , Resub(liq.)=0.9-10. The theoretical model ensures good correlation with the experiment

  12. Advanced Motor-Controller Development.

    Science.gov (United States)

    1983-06-22

    STH e. LIIU+-1 A󈧕 i 17 01018:~ AIC’F E:iz 0𔃾t’i2 L(DA A LIQ 0 _3 15 011. F6S 0 4 l LE:A EB 10 nonl~~f cii 1. 6:( 0 t 12.S HY LI0 TI H. E: 1711101 i j...CLAMP 000:1i 0159 67 0B406 STA A CEPR SAVE CEPF’: B1Ss 000 1N_:: :4: 000 382 .1=.- :4: BLOCK:’ 8. PEAC_ FSTAR FSTAP=A <S F.TA : 0.- 0’c’! 3011.7: F6 0...OUTPUTS: 16 BIT PROE:UCT IN ACCA , FiCC:B Oi:t2 -* 0011: 0172 B:7 .04E SIFY STA A MCAN:,* SF,-’E MULTIPLICAND 001t4 0175 iF CLF: A INIT RESUI_I_T AOll5

  13. Study of the heterogeneous reaction of O3 with CH3SCH3 using the wetted-wall flowtube technique

    Directory of Open Access Journals (Sweden)

    M. Barcellos da Rosa

    2003-01-01

    Full Text Available This work presents the heterogeneous kinetics of the reaction of CH3SCH3 (dimethyl sulphide, DMS with O3 (ozone in aqueous solutions of different ionic strengths (0, 0.1 and 1.0M NaCl using the wetted-wall flowtube (WWFT technique. Henry's law coefficients of DMS on pure water and on different concentrations of NaCl (0.1M - 4.0M in the WWFT from UV spectrophotometric measurements of DMS in the gas phase, using a numerical transport model of phase exchange, were determined to be H ±s (M atm-1 = 2.16±0.5 at 274.4 K, 1.47±0.3 at 283.4 K, 0.72±0.2 at 291 K, 0.57±0.1 at 303.4 K and 0.33±0.1 at 313.4 K on water, on 1.0M NaCl to be H = 1.57±0.4 at 275.7 K, 0.8±0.2 at 291 K and on 4.0M NaCl to be H = 0.44±0.1 at 275.7 K and 0.16±0.04 at 291 K, showing a significant effect of ionic strength, m, on the solubility of DMS according to the equation ln (H/M atm-1 = 4061 T-1 - 0.052 m2 - 50.9 m T-1 - 14.0. At concentrations of DMS(liq above 50 mM, UV spectrophotometry of both O3(gas and DMS(gas enables us to observe simultaneously the reactive uptake of O3 on DMS solution and the gas-liquid equilibration of DMS along the WWFT. The uptake coefficient, g (gamma, of O3 on aqueous solutions of DMS, varying between 1 and 15·10-6, showed a square root-dependence on the aqueous DMS concentration (as expected for diffusive penetration into the surface film, where the reaction takes place in aqueous solution. The uptake coefficient was smaller on NaCl solution in accord with the lower solubility of O3. The heterogeneous reaction of O3(gas with DMS(liq was evaluated from the observations of the second order rate constant (kII for the homogeneous aqueous reaction O3(liq + DMS(liq using a numerical model of radial diffusion and reactive penetration, leading to kII ± D kII (in units of 108 M-1 s-1 = 4.1±1.2 at 291.0 K, 2.15±0.65 at 283.4 K and 1.8±0.5 at 274.4 K. Aside from the expected influence on solubility and aqueous-phase diffusion coefficient of both

  14. Cast AlSi9Cu4 alloy with hybride strenghtened by Fe{sub x}Al{sub y}-Al{sub 2}O{sub 3} composite powder

    Energy Technology Data Exchange (ETDEWEB)

    Piatkowski, J [Department of Materials Technology, Silesian University of Technology, Krasinskiego 8, 40-019 Katowice (Poland); Formanek, B, E-mail: jaroslaw.piatkowski@polsl.pl, E-mail: boleslaw.formanek@polsl.pl [Department of Materials Science, Silesian University of Technology, Krasinskiego 8, 40-019 Katowice (Poland)

    2011-05-15

    The main objective of the study was to develop a technology of dispersion strenghtened hypoeutectic Al-Si alloy. The article presented the materials and technology conception for producing aluminium matrix composite AlSi9Cu4Fe alloy with hybride reinforcement of Al{sub x}Fe{sub y} intermetallic and aluminium oxide powders. Composite powder obtained in mechanical agllomerisation mixture of elemental powders. Changes in the structure were confirmed by TA and ATD thermal analyses plotting the solidification curves, which showed a decrease in temperature T{sub liq} compared to the unmodified alloy and an exothermic effect originating from the crystallisation of eutectics with alloying elements. The examinations carried out by SEM and BSE as well as the determination of local chemical composition by EDX technique have characterised the structure of the alloy as containing some binary Al-Si-Al-Cu and Al-Fe eutectics and multicomponent eutectics.

  15. Soluble Model Fluids with Complete Scaling and Yang-Yang Features

    Science.gov (United States)

    Cerdeiriña, Claudio A.; Orkoulas, Gerassimos; Fisher, Michael E.

    2016-01-01

    Yang-Yang (YY) and singular diameter critical anomalies arise in exactly soluble compressible cell gas (CCG) models that obey complete scaling with pressure mixing. Thus, on the critical isochore ρ =ρc , C˜ μ≔-T d2μ /d T2 diverges as |t |-α when t ∝T -Tc→0- while ρd-ρc˜|t |2β where ρd(T )=1/2 [ρliq+ρgas] . When the discrete local CCG cell volumes fluctuate freely, the YY ratio Rμ=C˜μ/CV may take any value -∞ 0 . More general decorated CCGs, including "hydrogen bonding" water models, illuminate energy-volume coupling as relevant to Rμ.

  16. Macrokinetics of carbon nanotubes synthesis by the chemical vapor deposition method

    Science.gov (United States)

    Rukhov, Artem; Dyachkova, Tatyana; Tugolukov, Evgeny; Besperstova, Galina

    2017-11-01

    A new approach to studying and developing basic processes which take place on the surface of a metal catalyst during the thermal decomposition of carbonaceous substances in the carbon nanotubes synthesis by the chemical vapor deposition method was proposed. In addition, an analysis was made of the interrelationships between these thermal, diffusion, hydrodynamic and other synthesis processes. A strong effect of the catalyst regeneration stage on the stage of nanotube formation has been shown. Based on the developed approach, a mathematical model was elaborated. Comparison of the calculation and the experiment carried out with the NiO-MgO catalyst at propane flow rate of 50 mL/min (standard conditions) and ethanol flow rate 0.3 mL/min (liq.) has revealed a discrepancy of less than 10%.

  17. Flexible bottom-emitting white organic light-emitting diodes with semitransparent Ni/Ag/Ni anode.

    Science.gov (United States)

    Koo, Ja-Ryong; Lee, Seok Jae; Lee, Ho Won; Lee, Dong Hyung; Yang, Hyung Jin; Kim, Woo Young; Kim, Young Kwan

    2013-05-06

    We fabricated a flexible bottom-emitting white organic light-emitting diode (BEWOLED) with a structure of PET/Ni/Ag/Ni (3/6/3 nm)/ NPB (50 nm)/mCP (10 nm)/7% FIrpic:mCP (10 nm)/3% Ir(pq)(2) acac:TPBi (5 nm)/7% FIrpic:TPBi (5 nm)/TPBi (10 nm)/Liq (2 nm)/ Al (100 nm). To improve the performance of the BEWOLED, a multilayered metal stack anode of Ni/Ag/Ni treated with oxygen plasma for 60 sec was introduced into the OLED devices. The Ni/Ag/Ni anode effectively enhanced the probability of hole-electron recombination due to an efficient hole injection into and charge balance in an emitting layer. By comparing with a reference WOLED using ITO on glass, it is verified that the flexible BEWOLED showed a similar or better electroluminescence (EL) performance.

  18. Eletroforese em papel das proteínas do líqüido cefalorraquidiano: II. Principais resultados registrados na literatura

    Directory of Open Access Journals (Sweden)

    A. Spina-França

    1958-09-01

    Full Text Available Partindo dos dados referentes à aplicação da eletroforese em papel de filtro na separação das frações proteicas do LCR, apresentados em publicação anterior, são revistos os dados da literatura sob o ponto de vista do laboratório clínico. Tanto os valores relativos normais referentes a cada uma das reações proteicas, como alterações patológicas mais freqüentemente encontradas em diversos tipos de afecções do sistema nervoso são apresentados, ressaltando-se a importância dos achados frente à fisiopatologia do liqüido cefalorraquidiano e frente à Clínica Neurológica.

  19. Preços-sombra no sistema de pagamentos: uma abordagem dual para a política monetária intradiária

    Directory of Open Access Journals (Sweden)

    Rodrigo Andrés de Souza Peñaloza

    2005-12-01

    Full Text Available O funcionamento do sistema de liqüidação pelo valor bruto em tempo real é modelado como uma otimização na qual enfileiramento e fracionamento de pagamentos e acordos de recompra surgem como soluções primais. O problema dual associado à maximização do fluxo de pagamentos é então usado para a determinação dos preços-sombra dos bancos no sistema de pagamentos. Esses preços-sombra podem ser usados para a personalização das políticas monetárias intradiárias tais como requerimentos de reserva inicial, acordos de recompra, extensão bilateral de crédito no mercado interbancário intradiário, etc. de modo a tornar eficiente o uso da liqüidez sistêmica.We model the functioning of real-time gross settlement systems for large-value transfers as a linear programming problem in which queueing arrangements, splitting of payments, and Lombard loans arise as primal solutions. Then we use the dual programming problem associated with the maximization of the total flow of payments in order to determine the shadow-prices of banks in the payment system. We use these shadow-prices to set personalized intraday monetary policies such as reserve requirements, availability of Central Bank credit to temporarilly illiquid banks, extension of intraday interbank credit exposures, etc., so as to make the use of systemic liquidity more efficient.

  20. Preface: Proceedings of the ESF Exploratory Workshop on Glassy Liquids under Pressure: Fundamentals and Applications (Ustroń, Poland, 10-12 October 2007) Proceedings of the ESF Exploratory Workshop on Glassy Liquids under Pressure: Fundamentals and Applications (Ustroń, Poland, 10-12 October 2007)

    Science.gov (United States)

    Drozd-Rzoska, Aleksandra; Rzoska, Sylwester J.; Tamarit, Josep Ll

    2008-06-01

    that the dynamics of (canonical) glasses is almost completely controlled by orientational degrees of freedom 34 and thus, vitrifying orientationally disordered crystals can yield materials with a reduction of complexity. This can be important for reaching a better insight into the glass state and vitrification in general. The European Science Foundation Exploratory Workshop (ESF EW) is a brainstorming panel for the best specialists in the given field of science. Participants of the ESF EW 'Glassy Liquids Under Pressure' arrived at the Institute of Physics, the Silesian University, Katowice, Poland on 10 October 2007. Katowice is the capital of Upper Silesia and of the metropolitan area of Silesia (population ≈ 4 000 000)—the most industrial area of Poland. The conference coach took participants to the Jaskółka Hotel in Ustroń, a tourist resort situated in the beautiful valley at the foot of the Beskidy mountains (a part of West Carpaty), 80 km south from Katowice. The picturesque surroundings together with the delicious local cuisine created a stimulating atmosphere for the three days of lectures and discussions. References [1] Turnbull D 1969 Under what criterion the glass can be formed Contemp. Phys.10 3473 [2] Drozd-Rzoska A, Rzoska S J and Imre A R 2007 On the pressure evolution of the melting temperature and the glass transition temperature J. Non-Cryst. Solids 353 3915 [3]Donth E 1998 The Glass Transition. Relaxation Dynamics in Liquids and Disordered Materials(Springer Series in Materials Science II vol 48) (Berlin: Springer) [4] Johari G P and Goldstein M 1971 Viscous liquids and the glass transition in aliphatic alcohols and other norigid molecules J. Chem. Phys. 55 4245 [5] Roland C M and Casalini R 2004 Viscosity crossover in 0-therphenyl and salol under high pressure Phys. Rev. Lett.92 245702 [6] Novikov V N and Sokolov A P 2003 Universality of the dynamic crossover in glass-forming liquids: A 'magic' relaxation time Phys. Rev. E 67 031507 [7

  1. Coincidence of flowering time and the productivity and quality of cauliflower hybrid seeds Coincidência de florescimento entre linhagens de couve-flor na produtividade e qualidade de sementes híbridas

    Directory of Open Access Journals (Sweden)

    Marcelo Fontanetti Verdial

    2001-09-01

    florescimento das diferentes épocas de semeadura com a linhagem polinizadora. Foram avaliadas as seguintes características: área foliar média, número de flores por planta, número de síliqüas por planta, número de sementes por planta (peso e número, peso médio de 1000 sementes e foi determinado o número de sementes por síliqüa. Foi realizado ainda, o teste padrão de germinação e determinada a pureza genética das sementes para cada tratamento. A coincidência da época de florescimento entre as linhagens de couve-flor afetou diretamente a produtividade e a qualidade genética das sementes híbridas produzidas, sendo que, quanto maior foi o nível de coincidência, maior foi o número de sementes formadas por síliqüa e menor a percentagem de sementes contaminantes. Entretanto, não teve influência na qualidade fisiológica das mesmas.

  2. A GROMOS-Compatible Force Field for Small Organic Molecules in the Condensed Phase: The 2016H66 Parameter Set.

    Science.gov (United States)

    Horta, Bruno A C; Merz, Pascal T; Fuchs, Patrick F J; Dolenc, Jozica; Riniker, Sereina; Hünenberger, Philippe H

    2016-08-09

    This article reports on the calibration and validation of a new GROMOS-compatible parameter set 2016H66 for small organic molecules in the condensed phase. The calibration is based on 62 organic molecules spanning the chemical functions alcohol, ether, aldehyde, ketone, carboxylic acid, ester, amine, amide, thiol, sulfide, and disulfide, as well as aromatic compounds and nucleic-acid bases. For 57 organic compounds, the calibration targets are the experimental pure-liquid density ρliq and the vaporization enthalpy ΔHvap, as well as the hydration free energy ΔGwat and the solvation free energy ΔGche in cyclohexane, at atmospheric pressure and at (or close to) room temperature. The final root-mean-square deviations (RMSD) for these four quantities over the set of compounds are 32.4 kg m(-3), 3.5 kJ mol(-1), 4.1 kJ mol(-1), and 2.1 kJ mol(-1), respectively, and the corresponding average deviations (AVED) are 1.0 kg m(-3), 0.2 kJ mol(-1), 2.6 kJ mol(-1), and 1.0 kJ mol(-1), respectively. For the five nucleic-acid bases, the parametrization is performed by transferring the final 2016H66 parameters from analogous organic compounds followed by a slight readjustment of the charges to reproduce the experimental water-to-chloroform transfer free energies ΔGtrn. The final RMSD for this quantity over the five bases is 1.7 kJ mol(-1), and the corresponding AVED is 0.8 kJ mol(-1). As an initial validation of the 2016H66 set, seven additional thermodynamic, transport, and dielectric properties are calculated for the 57 organic compounds in the liquid phase. The agreement with experiment in terms of these additional properties is found to be reasonable, with significant deviations typically affecting either a specific chemical function or a specific molecule. This suggests that in most cases, a classical force-field description along with a careful parametrization against ρliq, ΔHvap, ΔGwat, and ΔGche results in a model that appropriately describes the liquid in terms of

  3. Thermal decomposition mechanism of 1-ethyl-3-methylimidazolium bromide ionic liquid.

    Science.gov (United States)

    Chambreau, Steven D; Boatz, Jerry A; Vaghjiani, Ghanshyam L; Koh, Christine; Kostko, Oleg; Golan, Amir; Leone, Stephen R

    2012-06-21

    In order to better understand the volatilization process for ionic liquids, the vapor evolved from heating the ionic liquid 1-ethyl-3-methylimidazolium bromide (EMIM(+)Br(-)) was analyzed via tunable vacuum ultraviolet photoionization time-of-flight mass spectrometry (VUV-PI-TOFMS) and thermogravimetric analysis mass spectrometry (TGA-MS). For this ionic liquid, the experimental results indicate that vaporization takes place via the evolution of alkyl bromides and alkylimidazoles, presumably through alkyl abstraction via an S(N)2 type mechanism, and that vaporization of intact ion pairs or the formation of carbenes is negligible. Activation enthalpies for the formation of the methyl and ethyl bromides were evaluated experimentally, ΔH(‡)(CH(3)Br) = 116.1 ± 6.6 kJ/mol and ΔH(‡)(CH(3)CH(2)Br) = 122.9 ± 7.2 kJ/mol, and the results are found to be in agreement with calculated values for the S(N)2 reactions. Comparisons of product photoionization efficiency (PIE) curves with literature data are in good agreement, and ab initio thermodynamics calculations are presented as further evidence for the proposed thermal decomposition mechanism. Estimates for the enthalpy of vaporization of EMIM(+)Br(-) and, by comparison, 1-butyl-3-methylimidazolium bromide (BMIM(+)Br(-)) from molecular dynamics calculations and their gas phase enthalpies of formation obtained by G4 calculations yield estimates for the ionic liquids' enthalpies of formation in the liquid phase: ΔH(vap)(298 K) (EMIM(+)Br(-)) = 168 ± 20 kJ/mol, ΔH(f, gas)(298 K) (EMIM(+)Br(-)) = 38.4 ± 10 kJ/mol, ΔH(f, liq)(298 K) (EMIM(+)Br(-)) = -130 ± 22 kJ/mol, ΔH(f, gas)(298 K) (BMIM(+)Br(-)) = -5.6 ± 10 kJ/mol, and ΔH(f, liq)(298 K) (BMIM(+)Br(-)) = -180 ± 20 kJ/mol.

  4. On exergy analysis of industrial plants and significance of ambient temperature

    Energy Technology Data Exchange (ETDEWEB)

    Rian, Berit

    2011-07-01

    The exergy analysis has been a relatively mature theory for more than 30 years. However, it is not that developed in terms of procedures for optimizing systems, which partly explains why it is not that common. Misconceptions and prejudices, even among scientists, are also partly to blame.The main objective of this work was to contribute to the development of an understanding and methodology of the exergy analysis. The thesis was mainly based on three papers, two of which provided very different examples from existing industrial systems in Norway, thus showing the societal perspective in terms of resource utilization and thermodynamics. The last paper and the following investigation were limited to certain aspects of ambient conditions. Two Norwegian operational plants have been studied, one operative for close to 30 years (Kaarstoe steam production and distribution system), while the other has just started its expected 30 years of production (Snoehvit LNG plant). In addition to mapping the current operational status of these plants, the study of the Kaarstoe steam production and distribution system concluded that the potential for increasing the thermodynamic performance by rather cautious actions was significant, whereas the study of the Snoehvit LNG plant showed the considerable profit which the Arctic location provided in terms of reduced fuel consumption. The significance of the ambient temperature led to the study of systems with two ambient bodies (i.e. ambient water and ambient air) of different temperatures, here three different systems were investigated: A regenerative steam injection gas turbine (RSTIG), a simple Linde air liquefaction plant (Air Liq) and an air-source heat pump water heater (HPWH). In particular, the effect of the chosen environment on exergy analysis was negligible for RSTIG, modest for Air Liq and critical for HPWH. It was found that the amount of exergy received from the alternative ambient body, compared to the main exergy flow of

  5. High-temperature superconducting conductors and cables

    International Nuclear Information System (INIS)

    Peterson, D.E.; Maley, M.P.; Boulaevskii, L.; Willis, J.O.; Coulter, J.Y.; Ullmann, J.L.; Cho, Jin; Fleshler, S.

    1996-01-01

    This is the final report of a 3-year LDRD project at LANL. High-temperature superconductivity (HTS) promises more efficient and powerful electrical devices such as motors, generators, and power transmission cables; however this depends on developing HTS conductors that sustain high current densities J c in high magnetic fields at temperatures near liq. N2's bp. Our early work concentrated on Cu oxides but at present, long wire and tape conductors can be best made from BSCCO compounds with high J c at low temperatures, but which are degraded severely at temperatures of interest. This problem is associated with thermally activated motion of magnetic flux lines in BSCCO. Reducing these dc losses at higher temperatures will require a high density of microscopic defects that will pin flux lines and inhibit their motion. Recently it was shown that optimum defects can be produced by small tracks formed by passage of energetic heavy ions. Such defects result when Bi is bombarded with high energy protons. The longer range of protons in matter suggests the possibility of application to tape conductors. AC losses are a major limitation in many applications of superconductivity such as power transmission. The improved pinning of flux lines reduces ac losses, but optimization also involves other factors. Measuring and characterizing these losses with respect to material parameters and conductor design is essential to successful development of ac devices

  6. Lexicon Reduction for Urdu/Arabic Script Based Character Recognition: A Multilingual OCR

    Directory of Open Access Journals (Sweden)

    Saeeda Naz

    2016-04-01

    Full Text Available Arabic script character recognition is challenging task due to complexity of the script and huge number of ligatures. We present a method for the development of multilingual Arabic script OCR (Optical Character Recognition and lexicon reduction for Arabic Script and its derivative languages. The objective of the proposed method is to overcome the large dataset Urdu and similar scripts by using GCT (Ghost Character Theory concept. Arabic and its sibling script languages share the similar character dataset i.e. the character set are difference in diacritic and writing styles like Naskh or Nasta?liq. Based on the proposed method, the lexicon for Arabic and Arabic script based languages can be minimized approximately up to 20 times. The proposed multilingual Arabic script OCR approach have been evaluated for online Arabic and its derivative language like Urdu using BPNN. The result showed that proposed method helps to not only the reduction of lexicon but also helps to develop the Multilanguage character recognition system for Arabic Script.

  7. BOILER-SUPERHEATED REACTOR

    Science.gov (United States)

    Heckman, T.P.

    1961-05-01

    A nuclear power reactor of the type in which a liquid moderator-coolant is transformed by nuclear heating into a vapor that may be used to drive a turbo- generator is described. The core of this reactor comprises a plurality of freely suspended tubular fuel elements, called fuel element trains, within which nonboiling pressurized liquid moderator-coolant is preheated and sprayed through orifices in the walls of the trains against the outer walls thereof to be converted into vapor. Passage of the vapor ovcr other unwetted portions of the outside of the fuel elements causes the steam to be superheated. The moderatorcoolant within the fuel elements remains in the liqUid state, and that between the fuel elements remains substantiaily in the vapor state. A unique liquid neutron-absorber control system is used. Advantages expected from the reactor design include reduced fuel element failure, increased stability of operation, direct response to power demand, and circulation of a minimum amount of liquid moderatorcoolant. (A.G.W.)

  8. Synthesis and electroluminescent properties of anthracene derivatives containing electron-withdrawing oxide moieties

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Jhin-yeong; Na, Eun Jae; Park, Soo Na [Department of Chemistry, Sungkyunkwan University, Suwon, 440-746 (Korea, Republic of); Lee, Seok Jae [Department of Information Display, Hongik University, Seoul, 121-791 (Korea, Republic of); Kim, Young Kwan, E-mail: kimyk@wow.hongik.ac.kr [Department of Information Display, Hongik University, Seoul, 121-791 (Korea, Republic of); Yoon, Seung Soo, E-mail: ssyoon@skku.edu [Department of Chemistry, Sungkyunkwan University, Suwon, 440-746 (Korea, Republic of)

    2014-10-15

    Highlights: • Blue fluorescent material is important for application in full-color displays. • We have synthesized emitters based on anthracene connected with oxide moieties. • 1C shows a highly efficient blue EL emission due to electron-injection property. - Abstract: A series of new blue-emitting materials: (4-(10-(naphthalen-2-yl)anthracen-9-yl)phenyl)(phenyl)methanone (1); 9-(naphthalen-2-yl)-10-(4-((diphenyl)phosphine oxide)phenyl)anthracene (2); 9-(naphthalen-2-yl)-10-(4-(phenylsulfonyl)phenyl)anthracene (3) were designed and synthesized via Suzuki cross-coupling reaction. Multilayer OLEDs were fabricated in the following sequence: ITO (180 nm)/NPB (50 nm)/blue materials 1–3 (30 nm)/TPBi (15 nm)/Liq (2 nm)/Al (100 nm). All devices showed the efficient blue EL emissions. In particular, the device using 1 as an emitter exhibited efficient blue electroluminescent properties with a maximum luminous, power, external quantum efficiency and CIE coordinates of 0.36 cd/A, 0.90 lm/W, 0.55% at 20 mA/cm{sup 2} and (x = 0.16, y = 0.20) at 10.0 V, respectively.

  9. Organic light-emitting diodes based on 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit as the deep-blue emitting layer

    Energy Technology Data Exchange (ETDEWEB)

    Song, Ji Young; Lee, Seul Bee [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Lee, Seok Jae [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Kim, Young Kwan, E-mail: kimyk@wow.hongik.ac.kr [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Yoon, Seung Soo, E-mail: ssyoon@skku.edu [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

    2015-02-27

    A series of 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit, which prevented molecular aggregation and self-quenching effect, was designed and synthesized. By using various bridges between the 9-(2-naphthyl)anthracene group and the triphenylsilane unit, five deep-blue emitters were obtained and applied as non-doped emitting materials in organic light-emitting diodes (OLEDs) with a device structure of indium–tin-oxide (ITO) (180 nm)/4,4-bis(N-(1-naphthyl)-N-phenylamino)biphenyl (NPB) (50 nm)/emitting materials (30 nm)/4,7-diphenyl-1,10-phenanthroline (Bphen) (30 nm)/lithium quinolate (Liq) (2 nm)/Aluminium (100 nm). All devices showed blue emissions and their electroluminescence efficiencies are sensitive to the structural changes of the emitting materials. In particular, a device using 9-(2-naphthalenyl)-10-[6-(triphenylsilyl)-2-naphthalenyl]-anthracene (4) exhibited high luminous, power and quantum efficiencies of 2.28 cd/A, 1.42 lm/W and 2.40% at 20 mA/cm{sup 2}, respectively, and this device showed the deep blue emission with the CIE coordinates of (0.16, 0.10) at 6.0 V. - Highlights: • We synthesized 9-(2-naphthyl)anthracene derivatives with a triphenylsilane unit. • We study the conjugation-length effect on the electroluminescence properties. • The bulky triphenylsilane-anthracene derivatives show resistance to self-aggregation.

  10. Blue Organic Light-Emitting Diodes Based on Triphenylene Derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seul Ong; Jang, Heung Soo; Yoon, Seung Soo [Sungkyunkwan Univ., Suwon (Korea, Republic of); Lee, Seok Jae; Kim, Young Kwan [Hongik Univ., Seoul (Korea, Republic of)

    2013-08-15

    A series of blue fluorescent emitters based on triphenylene derivatives were synthesized via the Diels -Alder reaction in moderate yields. The electronic absorption and emission characteristics of the new functional materials were affected by the nature of the substituent on the triphenylene nucleus. Multilayered OLEDs were fabricated with a device structure of: ITO/NPB (50 nm)/EML (30 nm)/Bphen (30 nm)/Liq (2.0 nm)/Al (100 nm). All devices showed efficient blue emissions. Among those, a device using 1 gives the best performances with a high brightness (978 cd m{sup -2} at 8.0 V) and high efficiencies (a luminous efficiency of 0.80 cd/A, a power efficiency of 0.34 lm/W and an external quantum efficiency of 0.73% at 20 mA/cm{sup 2}). The peak wavelength of the electroluminescence was 455 nm with CIE{sub x,y} coordinates of (0.17, 0.14) at 8.0 V.

  11. Highly efficient blue OLEDs based on diphenylaminofluorenylstyrenes end-capped with heterocyclic aromatics

    Energy Technology Data Exchange (ETDEWEB)

    Oh, Suhyun [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Lee, Kum Hee; Kim, Young Kwan [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Yoon, Seung Soo, E-mail: ssyoon@skku.edu [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

    2012-10-15

    In this paper, we have designed four diphenylaminofluorenylstyrene derivatives end-capped with heterocyclic aromatic groups, such as 9-phenylcabazole, 4-dibenzofuran, 2-benzoxazole, 2-quinoxaline, respectively. These materials showed blue to red fluorescence with maximum emission wavelengths of 476–611 nm, respectively, which were dependent on the structural and electronic nature of end-capping groups. To explore the electroluminescent properties of these materials, multilayer OLEDs were fabricated in the following sequence: ITO/DNTPD (40 nm)/NPB (20 nm)/2% doped in MADN (20 nm)/Alq{sub 3} (40 nm)/Liq. (1 nm)/Al. Among those, a device exhibited a highly efficient blue emission with the maximum luminance of 14,480 cd/m{sup 2} at 9 V, the luminous efficiency of 5.38 cd/A at 20 mA/cm{sup 2}, power efficiency of 2.77 lm/W at 20 mA/cm{sup 2}, and CIE{sub x,y} coordinates of (0.147, 0.152) at 8 V, respectively.

  12. Infecção piógena do espaço epidural raquidiano em criança

    Directory of Open Access Journals (Sweden)

    Antonio B. Lefèvre

    1960-03-01

    Full Text Available Registro de um caso de infecção piógena do espaço epidural raquidiano, provavelmente originada de lesão purulenta da pele, o início da sintomatologia ocorrendo após traumatismo da coluna vertebral. Os autores acentuam a importância dos seguintes fatos para o diagnóstico: 1 sintomatologia neurológica limitada à lesão das estruturas contidas no canal raquidiano; 2 as diferenças citoquímicas do liqüido cefalorraquidiano colhido em punções combinadas, suboccipital e lombar; 3 os resultados da mielografia mostrando a lentidão do trânsito da substância contrastante. O tratamento clínico, à base de antibióticos em doses intensas e glicocorticóides por via oral, deu excelentes resultados, demonstrando que, nesses casos agudos, o tratamento conservador deve ser preferido à intervenção cirúrgica.

  13. Crystal structure and superconductivity of YBa2(Cu1-xFex)3Oy prepared by various heat treatments

    International Nuclear Information System (INIS)

    Katsuyama, Shigeru; Kosuge, Koji; Ueda, Yutaka

    1989-01-01

    The heat treatments of (a) slow cooling from 850 C in O 2 gas, which is an ordinary one, (b) quenching into liq. N 2 from 930 C in air followed by oxidation below 400 C in O 2 gas and (c) heating at 800 C in N 2 gas followed by oxidation below 400 C in O 2 gas stabilize the orthorhombic phase up to x=0.02, 0.04 and 0.12, respectively. The extension of the orthorhombic region seems to be due to the change of ratio of Fe1 to Fe2 and clustering for Fe ions in the Cu1-0 planes, which has been deduced from the results of 57 Fe Moessbauer measurements etc. The order of T c of the samples with the same iron concentration prepared by the above heat treatments is T c (c) T c (a) T c (b). The experimental results seem to show that one-dimensional Cu1-0 chains play a very important role in superconductivity as well as the two-dimensional Cu2-0 planes

  14. The Solar System According to General Relativity: The Sun's Space Breaking Meets the Asteroid Strip

    Directory of Open Access Journals (Sweden)

    Borissova L.

    2010-04-01

    Full Text Available This study deals with the exact solution of Einstein’s field equations for a sphere of incompressible liquid without the additional limitation initially introduced in 1916 by Schwarzschild, by which the space-time metric must have no singularities. The ob- tained exact solution is then applied to the Universe, the Sun, and the planets, by the assumption that these objects can be approximated as spheres of incompressible liq- uid. It is shown that gravitational collapse of such a sphere is permitted for an object whose characteristics (mass, density, and size are close to the Universe. Meanwhile, there is a spatial break associated with any of the mentioned stellar objects: the break is determined as the approaching to infinity of one of the spatial components of the metric tensor. In particular, the break of the Sun’s space meets the Asteroid strip, while Jupiter’s space break meets the Asteroid strip from the outer side. Also, the space breaks of Mercury, Venus, Earth, and Mars are located inside the Asteroid strip (inside the Sun’s space break.

  15. Theoretical Calculation of Jet Fuel Thermochemistry. 1; Tetrahydrodicylopentadiene (JP10) Thermochemistry Using the CBS-QB3 and G3(MP2)//B3LYP Methods

    Science.gov (United States)

    Zehe, Michael J.; Jaffe, Richard L.

    2010-01-01

    High-level ab initio calculations have been performed on the exo and endo isomers of gas-phase tetrahydrodicyclopentadiene (THDCPD), a principal component of the jet fuel JP10, using the Gaussian Gx and Gx(MPx) composite methods, as well as the CBS-QB3 method, and using a variety of isodesmic and homodesmotic reaction schemes. The impetus for this work is to help resolve large discrepancies existing between literature measurements of the formation enthalpy Delta (sub f)H deg (298) for exo-THDCPD. We find that use of the isodesmic bond separation reaction C10H16 + 14CH4 yields 12C2H6 yields results for the exo isomer (JP10) in between the two experimentally accepted values, for the composite methods G3(MP2), G3(MP2)//B3LYP, and CBS-QB3. Application of this same isodesmic bond separation scheme to gas-phase adamantane yields a value for Delta (sub f)H deg (298) within 5 kJ/mol of experiment. Isodesmic bond separation calculations for the endo isomer give a heat of formation in excellent agreement with the experimental measurement. Combining our calculated values for the gas-phase heat of formation with recent measurements of the heat of vaporization yields recommended values for Delta (sub f)H deg (298)liq of -126.4 and -114.7 kJ/mol for the exo and endo isomers, respectively.

  16. Improvement of efficiency roll-off in blue phosphorescence OLED using double dopants emissive layer

    Energy Technology Data Exchange (ETDEWEB)

    Yoo, Seung Il; Yoon, Ju An; Kim, Nam Ho; Kim, Jin Wook; Kang, Jin Sung; Moon, Chang-Bum [Department of Green Energy & Semiconductor Engineering, Hoseo University, Asan (Korea, Republic of); Kim, Woo Young, E-mail: wykim@hoseo.edu [Department of Green Energy & Semiconductor Engineering, Hoseo University, Asan (Korea, Republic of); Department of Engineering Physics, McMaster University, Hamilton, Ontario L8S 4L7 (Canada)

    2015-04-15

    Blue phosphorescent organic light-emitting diodes (PHOLEDs) were fabricated using double dopants FIrpic and FIr6 in emissive layer (EML) with structure of ITO/NPB (700 Å)/mCP:FIrpic-8%:FIr6-x% (300 Å)/TPBi (300 Å)/Liq (20 Å)/Al (1200 Å). We optimized concentration of the second dopant FIr6 in the presence of a fixed FIrpic to observe its effect on electrical performance of PHOLED device. 24.8 cd/A of luminous efficiency was achieved by the device with dopant ratio of 8%FIrpic:4%FIr6 in EML. Efficiency roll-off was also improved 20% compared to the PHOLED device singly dopped with FIrpic or FIr6 only. Second doping proved its effect in stabilizing charge balance in EML and enhancing energy transfer of triplet excitons between two dopants. - Highlights: • We fabricated blue PHOLED with double blue phosphorescent dopants in single EML. • Efficiency roll-off was improved by using double dopant in single EML. • The host–dopant transfer is discussed by analyzing the photo-absorption and photoluminescence. • The spectroscopic analysis using multi-peak fits with a Gaussian function.

  17. [A novel yellow organic light-emitting device].

    Science.gov (United States)

    Ma, Chen; Wang, Hua; Hao, Yu-Ying; Gao, Zhi-Xiang; Zhou, He-Feng; Xu, Bing-She

    2008-07-01

    The fabrication of a novel organic yellow-light-emitting device using Rhodamine B as dopant with double quantum-well (DQW) structure was introduced in the present article. The structure and thickness of this device is ITO/CuPc (6 nm) /NPB (20 nm) /Alq3 (3 nm)/Alq3 : Rhodamine B (3 nm) /Alq3 (3 nm) /Al q3 : Rhodamine B(3 nm) /Alq3 (30 nm) /Liq (5 nm)/Al (30 nm). With the detailed investigation of electroluminescence of the novel organic yellow-light-emitting device, the authors found that the doping concentration of Rhodamine B (RhB) had a very big influence on luminance and efficiency of the organic yellow-light-emitting device. When doping concentration of Rhodamine B (RhB) was 1.5 wt%, the organic yellow-light-emitting device was obtained with the maximum current efficiency of 1.526 cd x A(-1) and the maximum luminance of 1 309 cd x m(-2). It can be seen from the EL spectra of the devices that there existed energy transferring from Alq3 to RhB in the organic light-emitting layers. When the doping concentration of RhB increased, lambda(max) of EL spectra redshifted obviously. The phenomenon was attributed to the Stokes effect of quantum wells and self-polarization of RhB dye molecules.

  18. Color optimization of single emissive white OLEDs via energy transfer between RGB fluorescent dopants

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Nam Ho; Kim, You-Hyun; Yoon, Ju-An; Lee, Sang Youn [Department of Green Energy and Semiconductor Engineering, Hoseo University, Asan (Korea, Republic of); Ryu, Dae Hyun [Department of Information Technology, Hansei University, Gunpo (Korea, Republic of); Wood, Richard [Department of Engineering Physics, McMaster University, Hamilton, Ontario, Canada L8S 4L7 (Canada); Moon, C.-B. [Department of Green Energy and Semiconductor Engineering, Hoseo University, Asan (Korea, Republic of); Kim, Woo Young, E-mail: wykim@hoseo.edu [Department of Green Energy and Semiconductor Engineering, Hoseo University, Asan (Korea, Republic of); Department of Engineering Physics, McMaster University, Hamilton, Ontario, Canada L8S 4L7 (Canada)

    2013-11-15

    The electroluminescent characteristics of white organic light-emitting diodes (WOLEDs) were investigated including single emitting layer (SEL) with an ADN host and dopants; BCzVBi, C545T, and DCJTB for blue, green and red emission, respectively. The structure of the high efficiency WOLED device was; ITO/NPB(700 Å)/ADN: BCzVBi-7%:C545T-0.05%:DCJTB-0.1%(300 Å)/Bphen(300 Å)/Liq(20 Å)/Al(1200 Å) for mixing three primary colors. Luminous efficiency was 9.08 cd/A at 3.5 V and Commission Intenationale de L’eclairage (CIE{sub x,y}) coordinates of white emission was measured as (0.320, 0.338) at 8 V while simulated CIE{sub x,y} coordinates were (0.336, 0.324) via estimation from each dopant's PL spectrum. -- Highlights: • This paper observes single-emissive-layered white OLED using fluorescent dopants. • Electrical and optical properties are analyzed. • Color stability of white OLED is confirmed for new planar light source.

  19. Direct evidence of the existence of Mn3+ ions in MnTiO3

    Science.gov (United States)

    Maurya, R. K.; Sharma, Priyamedha; Patel, Ashutosh; Bindu, R.

    2017-08-01

    We investigate the room temperature electronic properties of MnTiO3 synthesised by different preparation conditions. For this purpose, we prepared MnTiO3 under two different cooling rates, one is naturally cooled while the other is quenched in liq.nitrogen. The samples were studied using optical absorbance, photoemission spectroscopy and band structure calculations. We observe significant changes in the structural parameters as a result of quenching. Interestingly, in the parent compound, our combined core level, valence band and optical absorbance studies give evidence of the Mn existence in both 2+ and 3+ states. The fraction of Mn3+ ions has been found to increase on quenching MnTiO3 suggests an increase in oxygen non-stoichiometry. The increase in the fraction of the Mn3+ ions has been manifested a) as slight enhancement in the intensity of the optical absorbance in the visible region. There occurs persistent photo-resistance when the incident light is terminated after shining; b) in the behaviour of the features (close to Fermi level) in the valence band spectra. Hence, the combined analysis of the core level, valence band and optical absorbance spectra suggests that the charge carriers are hole like which further leads to the increase in the electrical conductivity of the quenched sample. The present results provide a recipe to tune the optical absorption in the visible range for its applications in optical sensors, solar cell, etc.

  20. Electronic processes in uniaxially stressed p-type germanium

    Energy Technology Data Exchange (ETDEWEB)

    Dubon, Jr., Oscar Danilo [Univ. of California, Berkeley, CA (United States)

    1996-02-01

    Effect of uniaxial stress on acceptor-related electronic processes in Ge single crystals doped with Ga, Be, and Cu were studied by Hall and photo-Hall effect measurements in conjunction with infrared spectroscopy. Stress dependence of hole lifetime in p-type Ge single crystals is used as a test for competing models of non-radiative capture of holes by acceptors. Photo-Hall effect shows that hole lifetime in Ga- and Be-doped Ge increases by over one order of magnitude with uniaxial stress at liq. He temps. Photo-Hall of Ge:Be shows a stress-induced change in the temperature dependence of hole lifetime. This is consistent with observed increase of responsivity of Ge:Ga detectors with uniaxial stress. Electronic properties of Ge:Cu are shown to change dramatically with uniaxial stress; the results provide a first explanation for the performance of uniaxially stressed, Cu-diffused Ge:Ga detectors which display a high conductivity in absence of photon signal and therefore have poor sensitivity.

  1. AUSTRALIAN COMPETITION AND CONSUMER COMMISSION v ACN 117 372 915: SHOULD CONSUMER LAW REGULATE DOCTOR-PATIENT RELATIONS IN A CORPORATISED HEALTH CARE SYSTEM?

    Science.gov (United States)

    Wallace, Jessica; Pyman, Ella; Faunce, Thomas

    2015-09-01

    In April 2015, North J of the Federal Court of Australia made a finding of unconscionable conduct against Advanced Medical Institute, a promoter and provider of erectile dysfunction treatment, in a case concerning unfair contract terms (Australian Competition and Consumer Commission vACN 117 372 915 Pty Ltd (in liq) (formerly Advanced Medical Institute Pty Ltd) [2015] FCA 368). The contract required a minimum 12-month commitment, with costs exceeding treatments available from general practitioners, and made refunds available only after all possible treatment plans were exhausted which included penile injections. This column analyses that case, particularly in respect to the consumer law standards of practice under which it was litigated. Those standards refer to patients as "consumers" yet North J made extensive reference to the Good Medical Practice: A Code of Conduct for Doctors in Australia, a text which refers to "patients", as evidence of what constitutes appropriate professional conduct or practice for the health profession. This column considers whether legislative and judicial categorisation of patients (a class of people presumptively suffering, sick and vulnerable) as "consumers" undermines the formal and informal protections accorded to patients under normative systems of medical ethics such as those represented by the Code. The case, it is argued, also illuminates the contemporary tensions between the ethical, legal and human rights standards required of doctors in their treatment of patients and the commercial interests of businesses.

  2. Conditions to minimize soft single biomolecule deformation when imaging with atomic force microscopy.

    Science.gov (United States)

    Godon, Christian; Teulon, Jean-Marie; Odorico, Michael; Basset, Christian; Meillan, Matthieu; Vellutini, Luc; Chen, Shu-Wen W; Pellequer, Jean-Luc

    2017-03-01

    A recurrent interrogation when imaging soft biomolecules using atomic force microscopy (AFM) is the putative deformation of molecules leading to a bias in recording true topographical surfaces. Deformation of biomolecules comes from three sources: sample instability, adsorption to the imaging substrate, and crushing under tip pressure. To disentangle these causes, we measured the maximum height of a well-known biomolecule, the tobacco mosaic virus (TMV), under eight different experimental conditions positing that the maximum height value is a specific indicator of sample deformations. Six basic AFM experimental factors were tested: imaging in air (AIR) versus in liquid (LIQ), imaging with flat minerals (MICA) versus flat organic surfaces (self-assembled monolayers, SAM), and imaging forces with oscillating tapping mode (TAP) versus PeakForce tapping (PFT). The results show that the most critical parameter in accurately measuring the height of TMV in air is the substrate. In a liquid environment, regardless of the substrate, the most critical parameter is the imaging mode. Most importantly, the expected TMV height values were obtained with both imaging with the PeakForce tapping mode either in liquid or in air at the condition of using self-assembled monolayers as substrate. This study unambiguously explains previous poor results of imaging biomolecules on mica in air and suggests alternative methodologies for depositing soft biomolecules on well organized self-assembled monolayers. Copyright © 2016 Elsevier Inc. All rights reserved.

  3. UV lamp for photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Cardoso, M.J.B.; Landers, R.; Sundaram, V.S.

    1983-01-01

    An UV lamp and a differential pumping system which enables to couple the lamp to an ultra-high vacuum chamber (10 -9 torr) without using windows, are described. The differential between the pressure inside the discharge chamber and the one in de UHV region, which is of 10 8 -10 9 , is achieved with two pumping states separated by pyrex capillaries having an internal diameter of 0.6 mm. In the first stage, a mechanical pump (10 -3 torr) is used; in the second stage, a diffusor pump with a cryogenic trap (N 2 liq - 10 -7 torr) is employed. The lamp produces, when used with high purity He, narrow lines almost clear at 21.2 eV and 40.8 eV, depending on the discharge chamber pressure, thus eliminating the need of a monochromator. As a high voltage source (3 KV), a commercial unit with a good current control was used, ensuring UV beam stability - an essential characteristic for this lamp if it is employed for photoelectron excitation of crystalline samples. (C.L.B.) [pt

  4. Behaviour of fluoropolymers in presence of tritiated water

    International Nuclear Information System (INIS)

    Bubueanu, Gh.; Postolache, C.; Tuta, C.

    2011-01-01

    Complete text of publication follows. One of the most used methods for tritium recovery from tritiated water relies on combined electrolysis with catalytic isotope exchange techniques. The electrolytic cell converts the tritiated water or tritiated heavy water into a hydrogen, deuterium and tritium mixture. The mixture is purified and then tritium is recovered by catalytic isotopic separation techniques. Tritium presence in the system induces an intense radiation field especially at aqueous solution interface. This can generate significant structural modifications with potentially negative effects. In this paper work it is followed the study of radiolytic phenomena in Pt/C/PTFE isotopic exchange catalyst, NAFION membranes and VITON fluoroelastomer in presence of tritiated water with high radioactive concentration. Radiolytical processes were analyzed by: Exposure of fluoropolymers samples immersed in H 2 O at gamma radiation field (60-Co source) in vacuum, at liq. Nitrogen temperature and at ambient temperature respectively; Immersing of NAFION, Pt/C/PTFE catalyst and VITON samples in tritiated water with high activity (3.7 and 37 TBq/L) for different time period. In both cases the samples were characterized by FT IR ATR, and fluoride ions emission from polymeric matrix. Experimental results were correlated with quantum-chemical simulations.

  5. Biological methanation of hydrogen within biogas plants: A model-based feasibility study

    International Nuclear Information System (INIS)

    Bensmann, A.; Hanke-Rauschenbach, R.; Heyer, R.; Kohrs, F.; Benndorf, D.; Reichl, U.; Sundmacher, K.

    2014-01-01

    Highlights: • Simulation study about direct methanation of hydrogen within biogas plants. • In stationary operation two limitations, namely biological and transfer limit. • Biological limit at 4m H2 3 /m CO2 3 due to stoichiometry. • Dynamic behaviour shows three qualitatively different step responses. • A simple control scheme to meet the output quality was developed. - Abstract: One option to utilize excess electric energy is its conversion to hydrogen and the subsequent methanation. An alternative to the classical chemical Sabatier process is the biological methanation (methanogenesis) within biogas plants. In conventional biogas plants methane and carbon dioxide is produced. The latter can be directly converted to methane by feeding hydrogen into the reactor, since hydrogenotrophic bacteria are present. In the present contribution, a comprehensive simulation study with respect to stationary operating conditions and disturbances is presented. It reveals two qualitative different limitations, namely a biological limit (appr. at 4m H2 3 /m CO2 3 corresponds to 4.2m H2,STP 3 /m liq 3 /d) as well as a transfer limit. A parameter region for a safe operation was defined. The temporary operation with stationary unfeasible conditions was analysed and thereby three qualitatively different disturbances can be distinguished. In one of these the operation for several days is possible. On the basis of these results, a controller was proposed and tested that meets the demands on the conversion of hydrogen and also prevents the washout of the microbial community due to hydrogen overload

  6. Color optimization of single emissive white OLEDs via energy transfer between RGB fluorescent dopants

    International Nuclear Information System (INIS)

    Kim, Nam Ho; Kim, You-Hyun; Yoon, Ju-An; Lee, Sang Youn; Ryu, Dae Hyun; Wood, Richard; Moon, C.-B.; Kim, Woo Young

    2013-01-01

    The electroluminescent characteristics of white organic light-emitting diodes (WOLEDs) were investigated including single emitting layer (SEL) with an ADN host and dopants; BCzVBi, C545T, and DCJTB for blue, green and red emission, respectively. The structure of the high efficiency WOLED device was; ITO/NPB(700 Å)/ADN: BCzVBi-7%:C545T-0.05%:DCJTB-0.1%(300 Å)/Bphen(300 Å)/Liq(20 Å)/Al(1200 Å) for mixing three primary colors. Luminous efficiency was 9.08 cd/A at 3.5 V and Commission Intenationale de L’eclairage (CIE x,y ) coordinates of white emission was measured as (0.320, 0.338) at 8 V while simulated CIE x,y coordinates were (0.336, 0.324) via estimation from each dopant's PL spectrum. -- Highlights: • This paper observes single-emissive-layered white OLED using fluorescent dopants. • Electrical and optical properties are analyzed. • Color stability of white OLED is confirmed for new planar light source

  7. On-line determination of ammonia at low pptv mixing ratios in the CLOUD chamber

    CERN Document Server

    Bianchi, F; Mathot, S; Baltensperger, U

    2012-01-01

    A new instrument for the on-line determination of ammonia was developed. Since ammonia is a rather sticky compound, sampling losses were minimised with a new sam- pling device where the ammonia was transferred to the liq- uid phase only 5 mm after the inlet tip. The liquid phase was then analyzed by long pathlength absorption spectrophotom- etry using the Berthelot reaction with phenol and hypochlo- rite as reagents. The measurements were made during the CLOUD3 campaign at CERN where the influence of ammo- nia on the nucleation rate was studied. At stable conditions the detection limit reached with this instrument was 35 pptv (air flow rate of 2 l min − 1 , liquid flow rate of 0.3 ml min − 1 ), although occasionally the instrument was affected by back- ground problems. The range of mixing ratios during this campaign was varied from the background contamination ( < 35 pptv) up to around 2 ppbv. The measured ammonia concentration was correlated with the rate of ammonia in- jected into the chamber, but wi...

  8. Study of Sequential Dexter Energy Transfer in High Efficient Phosphorescent White Organic Light-Emitting Diodes with Single Emissive Layer

    Science.gov (United States)

    Kim, Jin Wook; You, Seung Il; Kim, Nam Ho; Yoon, Ju-An; Cheah, Kok Wai; Zhu, Fu Rong; Kim, Woo Young

    2014-11-01

    In this study, we report our effort to realize high performance single emissive layer three color white phosphorescent organic light emitting diodes (PHOLEDs) through sequential Dexter energy transfer of blue, green and red dopants. The PHOLEDs had a structure of; ITO(1500 Å)/NPB(700 Å)/mCP:Firpic-x%:Ir(ppy)3-0.5%:Ir(piq)3-y%(300 Å)/TPBi(300 Å)/Liq(20 Å)/Al(1200 Å). The dopant concentrations of FIrpic, Ir(ppy)3 and Ir(piq)3 were adjusted and optimized to facilitate the preferred energy transfer processes attaining both the best luminous efficiency and CIE color coordinates. The presence of a deep trapping center for charge carriers in the emissive layer was confirmed by the observed red shift in electroluminescent spectra. White PHOLEDs, with phosphorescent dopant concentrations of FIrpic-8.0%:Ir(ppy)3-0.5%:Ir(piq)3-0.5% in the mCP host of the single emissive layer, had a maximum luminescence of 37,810 cd/m2 at 11 V and a luminous efficiency of 48.10 cd/A at 5 V with CIE color coordinates of (0.35, 0.41).

  9. FeNbB bulk metallic glass with high boron content

    Energy Technology Data Exchange (ETDEWEB)

    Stoica, M.; Das, Jayanta; Eckert, Juergen [IFW Dresden, Institute for Complex Materials, P.O. Box 270016, D-01171 Dresden (Germany); Hajlaoui, Khalil; Yavari, Alain Reza [LTPCM-CNRS, I.N.P. Grenoble, 1130 Rue de la Piscine, BP 75, F-38402 University Campus (France)

    2007-07-01

    Fe-based alloys able to form magnetic bulk metallic glasses (BMGs) are of the type transition metal - metalloid and often contain 5 or more elements. Usually, the metalloid content is around 20 atomic %. Very recently, the Fe{sub 66}Nb{sub 4}B{sub 30} alloy was found to be able to form BMG by copper mold casting technique, despite its high metalloid content. Several composition with boron contents around 30 at. % or even higher were calculated since 1993 as possible compositions of the remaining amorphous matrix after the first stage of nanocrystallization of Finemet-type Fe{sub 77}Si{sub 14}B{sub 9} glassy ribbons with 0.5 to 1 atomic % Cu and a few percent Nb addition. Melt-spun ribbons of all calculated compositions were found to be glassy. The composition of the ternary Fe-based BMG investigated in the present study resulted as an optimization of all possibilities. The alloy is ferromagnetic with glass transition temperature T{sub g}=845 K, crystallisation temperature T{sub x}=876 K, liquidus temperature T{sub liq}=1451 K and mechanical strength of 4 GPa. The coercivity of as-cast samples is very low, around 1.5 A/m. The present contribution aims at discussing the thermal stability, mechanical and magnetic properties of the Fe{sub 66}Nb{sub 4}B{sub 30} BMG.

  10. Stacking multiple connecting functional materials in tandem organic light-emitting diodes

    Science.gov (United States)

    Zhang, Tao; Wang, Deng-Ke; Jiang, Nan; Lu, Zheng-Hong

    2017-02-01

    Tandem device is an important architecture in fabricating high performance organic light-emitting diodes and organic photovoltaic cells. The key element in making a high performance tandem device is the connecting materials stack, which plays an important role in electric field distribution, charge generation and charge injection. For a tandem organic light-emitting diode (OLED) with a simple Liq/Al/MoO3 stack, we discovered that there is a significant current lateral spreading causing light emission over an extremely large area outside the OLED pixel when the Al thickness exceeds 2 nm. This spread light emission, caused by an inductive electric field over one of the device unit, limits one’s ability to fabricate high performance tandem devices. To resolve this issue, a new connecting materials stack with a C60 fullerene buffer layer is reported. This new structure permits optimization of the Al metal layer in the connecting stack and thus enables us to fabricate an efficient tandem OLED having a high 155.6 cd/A current efficiency and a low roll-off (or droop) in current efficiency.

  11. Líquido cefalorraqueano em infecção do sistema nervoso central por leveduras do gênero Candida: análise de 11 casos

    Directory of Open Access Journals (Sweden)

    J. A. Livramento

    1989-09-01

    Full Text Available Foram estudadas 44 amostras de liqüido cefalorraqueano (LCR de 11 pacientes em que foi possível fazer diagnóstico etiológico de comprometimento do sistema nervoso central (SNC por leveduras do gênero Candida. Todos os pacientes apresentavam fatores de risco para a afecção. Cinco apresentavam quadro de meningite crônica a esclarecer; dois, síndrome de imunodeficiência adquirida; dois, traumatismo crânioencefálico seguido de meningite crônica; um, coagulação intravascular disseminada seguida de septicemia; um, candi-díase sistêmica pós-transplante renal. O diagnóstico etiológico foi feito pelo exame do LCR, possibilitando em 9 o isolamento da levedura por crescimento em meio de cultura. Em dois o diagnóstico foi feito pela presença das leveduras ao exame direto e, em um deles, também pela positividade da reação de fixação de complemento para Candida realizada em três amostras sucessivas de LCR. Discute-se a importância das alterações encontradas no exame do LCR na candidíase do SNC.

  12. Kiloampere, Variable-Temperature, Critical-Current Measurements of High-Field Superconductors.

    Science.gov (United States)

    Goodrich, L F; Cheggour, N; Stauffer, T C; Filla, B J; Lu, X F

    2013-01-01

    We review variable-temperature, transport critical-current (I c) measurements made on commercial superconductors over a range of critical currents from less than 0.1 A to about 1 kA. We have developed and used a number of systems to make these measurements over the last 15 years. Two exemplary variable-temperature systems with coil sample geometries will be described: a probe that is only variable-temperature and a probe that is variable-temperature and variable-strain. The most significant challenge for these measurements is temperature stability, since large amounts of heat can be generated by the flow of high current through the resistive sample fixture. Therefore, a significant portion of this review is focused on the reduction of temperature errors to less than ±0.05 K in such measurements. A key feature of our system is a pre-regulator that converts a flow of liquid helium to gas and heats the gas to a temperature close to the target sample temperature. The pre-regulator is not in close proximity to the sample and it is controlled independently of the sample temperature. This allows us to independently control the total cooling power, and thereby fine tune the sample cooling power at any sample temperature. The same general temperature-control philosophy is used in all of our variable-temperature systems, but the addition of another variable, such as strain, forces compromises in design and results in some differences in operation and protocol. These aspects are analyzed to assess the extent to which the protocols for our systems might be generalized to other systems at other laboratories. Our approach to variable-temperature measurements is also placed in the general context of measurement-system design, and the perceived advantages and disadvantages of design choices are presented. To verify the accuracy of the variable-temperature measurements, we compared critical-current values obtained on a specimen immersed in liquid helium ("liquid" or I c liq) at 5

  13. Analysis and separation of boron isotopes; Analyse et separation des isotopes du bore

    Energy Technology Data Exchange (ETDEWEB)

    Perie, M [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1966-11-01

    The nuclear applications of boron-10 justify the study of a method of measurement of its isotopic abundance as well as of very small traces of boron in different materials. A systematic study of thermionic emission of BO{sub 2}Na{sub 2}{sup +} has been carried out. In the presence of a slight excess of alkalis, the thermionic emission is considerably reduced. On the other hand, the addition of a mixture of sodium hydroxide-glycerol (or mannitol) to borax permits to obtain an intense and stable beam. These results have permitted to establish an operative method for the analysis of traces of boron by isotopic dilution. In other respects, the needs of boron-10 in nuclear industry Justify the study of procedures of separation of isotopes of boron. A considerable isotopic effect has been exhibited in the chemical exchange reaction between methyl borate and borate salt in solution. In the case of exchange between methyl borate and sodium borate, the elementary separation factor {alpha} is: {alpha}=(({sup 11}B/{sup 10}B)vap.)/(({sup 11}B/{sup 10}B)liq.)=1.03{sub 3}. The high value of this elementary effect has been multiplied in a distillation column in which the problem of regeneration of the reactive has been resolved. An alternative procedure replacing the alkali borate by a borate of volatile base, for example diethylamine, has also been studied ({alpha}=1,02{sub 5} in medium hydro-methanolic with 2,2 per cent water). (author) [French] Les applications nucleaires du bore 10 justifient l'etude d'une methode de mesure de son abondance isotopique dans divers materiaux ainsi que le dosage de tres faibles traces de bore. Une etude systematique de l'emission thermoionique de BO{sub 2} Na{sub 2}{sup +} a ete effectuee. En presence d'un leger exces d'alcalins, l'emission thermoionique est considerablement reduite. Par contre l'addition au borax d'un melange soude-glycerol (ou mannitol) permet d'obtenir un faisceau stable et intense. Ces resultats ont permis d'etablir un mode

  14. The MERIT High-Power Target Experiment at the CERN PS

    CERN Document Server

    McDonald, K T; Park, H; Tsang, T; Efthymiopoulos, I; Fabich, A; Haug, F; Lettry, J; Palm, M; Pereira, H; Mokhov, N; Striganov, S; Carroll, A J; Graves, V B; Spampinato, P T; Bennett, J R J; Caretta, O; Loveridge, P

    2010-01-01

    The MERIT (MER­cury In­tense Tar­get) ex­per­i­ment was run in the fall of 2007 using 14 and 24 GeV in­tense pro­ton beams from the CERN PS. It is a proof-of-prin­ci­ple ex­per­i­ment de­signed to val­i­date a tar­get con­cept for pro­duc­ing an in­tense muon source for a fu­ture muon col­lid­er or neu­tri­no fac­to­ry. The ex­per­i­ment suc­cess­ful­ly demon­strat­ed a tar­get tech­nique for mul­ti-MW pro­ton beams that uti­lizes a free-flow­ing liq­uid metal jet with­in the con­fines of a high-field solenoid. We de­scribe the ex­per­i­men­tal strat­e­gy and pa­ram­e­ters, as well as the re­sults ob­tained and their im­pli­ca­tions for fu­ture muon-based ac­cel­er­a­tor fa­cil­i­ties.

  15. FEATURES AND PROSPECTS FOR USE OF WIND-POWERED DRIVE ON AGRICULTURAL AIRPLANE

    Directory of Open Access Journals (Sweden)

    2016-01-01

    Full Text Available The article deals with the wind-powered drive location and functioning pecularities of agricultural airplane special equipment. The data on the advantages and prospects of the use of the wind-powered drive on agricultural aircraft as well as the experimental and analytical data on discontinuity of the wind stream in the zone of the wind-powered drive installa- and parameters of its operation at aerial spraying on the example of specially equipped An-2 are presented. A mathe- matical model of a wind propeller in discontinuous wind stream is developed. Software package to comprehensively assess wind-powered drive conditions and performance indicators is generated and tested taking into account experimental data, as well as airplane performance and flight modes. The typical data on the wind propeller and the wind-powered drive in the spraying process are received; specific features of the dynamics at the wind-powered drive turning-on and the wind propel- ler rotation at zero load are determined and the data on the wind-propeller blades load imbalance at spraying and transient processes are defined. The author made a quantitative estimation of how the standard change of flight parameters and the operation of the aircraft power plant at spraying influence on the factors of wind-powered drive operation and working liq- uids suppey. The main tendencies, qualitative and quantitative aspects of a wind-powered drive use are defined when per- forming aerial works and the proposals and recommendations for improving and using it in the future are made. The find- ings of the work can be used in the wind-powered drive of agricultural airplane special equipment designing and moderni- zation and drilling of the operational and technological procedures of aerial works performance in agriculture and forestry.

  16. Esquistossomose do sistema nervoso central relato de um caso

    Directory of Open Access Journals (Sweden)

    M. S. Ferreira

    1990-09-01

    Full Text Available O comprometimento do sistema nervoso na esquistossomose mansônica é evento raramente diagnosticado na evolução desta parasitose. Os autores descrevem o caso de uma paciente de 23 anos, natural de São Francisco-MG, que apresentava há duas semanas quadro de ceíaléia, vômitos em jato, febre e sonolência; o exame neurológico mostrava rigidez de nuca, paresia com hipertonia muscular bilateral em membros superiores, perda de motricidade e sensibilidade em membros inferiores. Não se palpava hepato-esplenomegalia. O exame do liqüido cefalorraquidiano (LCR mostrou hipoglicorraquia (28 mg%, hiperproteinorraquia (113 mg% e pleocitose acentuada (949 células/mm3, com predomínio de neutrófilos (70%, além de eosinofilorraquia (9%. A reação de imunofluorescência indireta para esquistossomose, no LCR, realizada em cortes de fígado com granuloma peri-ovular foi reagente (IgG: 1/16; IgM: 1/4. As pesquisas de fungos e b.a.a.r. no LCR, assim como a cultura para b.a.a.r. (após 60 dias e as reações imunológicas para neurocisticercose foram negativas. Uma tomografia computadorizada do cérebro e medula espinhal não evidenciou anormalidades. No exame parasitologico das fezes foi identificada a presença de ovos viáveis de S. mansoni. Instituiu-se tratamento com corticóides e praziquantel (60 mg/kg/dia; 7 dias tendo havido regressão das alterações do LCR, permanecendo entretanto seqüelas neurológicas graves (paraplegia e bexiga neurogênica.

  17. Reactor de película líquida descendente para la sulfonación de ésteres metílicos con trióxido de azufre

    Directory of Open Access Journals (Sweden)

    Jesús Alfonso Torres Ortega

    2009-09-01

    Full Text Available Se realizó un conjunto de experimentos de sulfonación de dodecilbenceno (DDB y ésteres metílicos (ME derivados de la esteari- na hidrogenada de palma, con SO3 gaseoso desorbido del óleum, en un reactor de sulfonación en película líquida descendente a escala banco de 40 cm de longitud y ½ pulgada de diámetro interno. Mediante titulaciones volumétricas se determinaron los porcentajes de materia sulfonada y contenido de ácido sulfúrico, así como el porcentaje de aceite libre mediante extracciones con éter de petróleo. La funcionalidad del reactor se verificó efectuando ensayos a condiciones reportadas por Gutiérrez y cola- boradores para dodecilbenceno sulfonado (DDBS, para lo cual fueron determinadas las técnicas de análisis en el Laboratorio de Ingeniería Química (LIQ de la Universidad Nacional de Colombia, sede Bogotá, con el acompañamiento de la empresa Química Básica Colombiana (Caloto, Cauca. Finalmente, se procedió a evaluar la influencia de diferentes variables de proce- so sobre la sulfonación de la mezcla de ésteres metílicos. Los resultados obtenidos en el sulfonador se ajustaron por regresión li- neal múltiple a ecuaciones empíricas, obteniendo expresiones que muestran de forma directa el efecto de variables como la re- lación molar SO3/ME, concentración de SO3 en la corriente gaseosa y flujo másico de ME.

  18. Tumor da região do terceiro ventrículo diagnóstico eletrencefalográfico

    Directory of Open Access Journals (Sweden)

    Paulino W. Longo

    1948-06-01

    Full Text Available Depois de rápidas considerações sobre as dificuldades do diagnóstico topográfico dos tumores da região do terceiro ventrículo e sobre as aquisições recentes da eletrencefalografia nesse sentido, os AA. apresentam a observação de uma paciente de 36 anos de idade, com história de 4 meses, portadora de uma síndrome de hipertensão intracraniana grave, acompanhada de hemiparesia esquerda muito discreta e alterações psíquicas. O exame do liqüido cefalorraquidiano revelou hipertensão e a eletrencefalografia evidenciou alterações difusas e bilaterais, ao lado de surtos persistentes e repetidos de ritmo teta, simétrica e sincronicamente reproduzidos, em áreas centrais e parietais de ambos os hemisférios, bem como ondas de ritmo delta focal, no lobo frontal direito, com típicas figuras de reversão. Os primeiros foram atribuídos ao edema cerebral e à hipertensão intracraniana, enquanto que estas (as ondas de ritmo teta acompanhadas de ritmo delta focal frontal direito foram interpretadas como dependentes de tumor cerebral profundamente situado, mediano, da região do terceiro ventrículo, comprometendo secundariamente o lobo frontal direito. A ventriculografia, em parte, e a intervenção cirúrgica subseqüente, confirmaram o diagnóstico, revelando a existência de um tumor cístico pediculado, que, da sela turca invadia o terceiro ventrículo e a parte profunda do lobo frontal direito (craniofaringioma.

  19. Twinning microstructure and charge ordering in the colossal magnetoresistive manganite Nd1/2Sr1/2MnO3

    International Nuclear Information System (INIS)

    Luo, Z.P.; Miller, D.J.; Mitchell, J.F.

    2000-01-01

    Charge ordering (C.O.) in the colossal magnetoresistive (CMR) manganites gives rise to an insulating, high-resistance state. This charge ordered state can be melted into a low-resistance metallic-like state by the application of magnetic field. Thus, the potential to attain high values of magnetoresistance with the application of small magnetic fields may be aided by a better understanding of the charge-ordering phenomenon. This study focused on microstructural characterization in Nd 1/2 Sr 1/2 MnO 3 . In Nd 1/2 Sr 1/2 MnO 3 , the nominal valence of Mn is 3.5+. On cooling, charge can localize and lead to a charge ordering between Mn 3+ and Mn 4+. The ordering of charge results in a superlattice structure and a reduction in symmetry. Thin foil specimens were prepared from bulk samples by conventional thinning and ion milling (at LiqN 2 temperature) methods. The room temperature TEM observation of Nd 1/2 Sr 1/2 MnO 3 reveals that it contains a highly twinned microstructure, together with a small number of stacking faults (SFS). A figure shows the same area of the specimen at different zone axes obtained by tilting around two perpendicular directions as indicated. Three grains A, B and C are labeled for each of the zone axes. The room temperature EDPs from the matrix and twins shows an approximate 90degree rotation suggesting a 90degree twin orientation. These results are further confirmed by C.O. at low temperatures. The twinning planes can be determined by tilting with large angles

  20. Synthesis and Electroluminescent Properties of Julolidine-π-Juloidine Type Materials with the Bulky Adamantane Groups

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Kum Hee; Yoon, Seung Soo [Sungkyunkwan Univ., Suwon (Korea, Republic of); Lee, Seok Jae; Kim, Young Kwan [Hongik Univ., Seoul (Korea, Republic of)

    2012-11-15

    A main problem of red emitting material, which contributes to their low EL performances, is the concentration quenching due to the effective self aggregation and the consequent formation of excimers. To avoid this drawback and thus improve the EL properties of red fluorescent OLED devices, many synthetic efforts have been conducted to develop new emitting materials with the structural motifs to suppress self-aggregation by the weakening intermolecular attractive interactions. Particularly, the introduction of bulky moieties in the emitters would provide the steric hindrance between emitting materials in solid state devices and thus reduce the self-aggregation. Nevertheless, EL performances of red materials still need to be improved for the practical applications. In conclusion, we designed and synthesized three julolidine-π-juloidine type emitting materials (1-3) with the bulky adamantane groups. To study their electroluminescent properties, the multilayered OLED devices with the structure of ITO/NPB (40 nm)/ADN : 1-3 (x%) (20 nm)/Alq{sub 3} (40 nm)/Liq (2 nm)/Al were fabricated. All devices using emitters 1-3 showed the efficient emissions, in which their EL performances depend on the structure of emitters sensitively. Particularly, a device using emitter 3 exhibited the efficient orange-red emission with the luminous and power efficiencies of 4.79 cd/A and 1.76 lm/W at 20 mA/cm{sup 2}, respectively. The CIE coordinates of this device was (0.57, 0.42) at 7.0 V.

  1. Measurement Properties of the Brazilian-Portuguese Version of the Lumbar Spine Instability Questionnaire.

    Science.gov (United States)

    Araujo, Amanda Costa; da Cunha Menezes Costa, Lucíola; de Oliveira, Crystian Bittencourt Soares; Morelhão, Priscila Kalil; de Faria Negrão Filho, Rúben; Pinto, Rafael Zambelli; Costa, Leonardo Oliveira Pena

    2017-07-01

    Cross-cultural adaptation and analysis of measurement properties. To translate and cross-culturally adapt the Lumbar Spine Instability Questionnaire (LSIQ) into Brazilian-Portuguese and to test its measurement properties in Brazilian patients with low back pain. The selection of subgroup of patients that respond better to specific interventions is the top research priority in the field of back pain. The LSIQ is a tool able to stratify patients with low back pain who responds better to motor control exercises. There is no Brazilian-Portuguese version of the LSIQ available. The original version of the LSIQ was translated and cross-culturally adapted. We collected data from 100 patients with low back pain. In addition to LSIQ, we also collected information about physical activity levels (measured by the International Physical Activity Questionnaire short version), disability (measured by the Roland Morris Disability Questionnaire), pain intensity (measured by the Pain numerical Rating Scale), kinesiophobia (measured by the Tampa Scale of Kinesiophobia), and depression (measured by the Beck Depression Inventory). The measurement properties tested were internal consistency, reproducibility (reliability and agreement), construct validity, and ceiling and floor effects. The Brazilian-Portuguese version of the LSIQ showed good measurement properties with a Cronbach alpha of 0.79, an intraclass correlation coefficient of 0.75, a standard error of measurement of 1.65 points, and a minimal detectable change of 3.54 points. We did not detect ceiling and floor effects. The construct validity analysis was observed a moderate correlation between the LSIQ and Pain Numerical Rating Scale r = 0.46, Roland Morris Disability Questionnaire r = 0.66, Tampa Scale of Kinesiophobia r = 0.49, and Beck Depression Inventory r = 0.44. The Brazilian-Portuguese version of LIQ has adequate measurement properties and can be used in clinical practice and research. NA.

  2. Shell model calculation of the nuclear moments of 9Li in a 2hω space

    International Nuclear Information System (INIS)

    Chang, Y.; Meder, M.R.

    1984-01-01

    A recent measurement of the magnitude of quadrupole moment of the ground state of 9 Li, Q( 9 Li), finds that Vertical BarQ( 9 Li)/Q( 7 Li)Vertical Bar = 0.88 +- 0.18. A variety of shell-model calculations, using p-shell wave functions, predict Q( 9 Li)approx. =1.3Q( 7 Li) and yield quadrupole moments whose magnitudes are approximately half the experimental values. Agreement between theory and experiment is improved when effective charges are used, although the results are still not completely satisfactory. A calculation of the wave functions of the low-lying states of 7 Li and 9 Li using a modified version of the Sussex matrix elements in a model space, including all 0hω and 2hω excitations, has been performed. The resulting value for Q( 9 Li) was -3.46 fm 2 as ray transitions in /sup 52,53/Cr and /sup 54,55/Mn have been observed using 7 Li( 51 V,xn yp zα γ) fusion-evaporation reactions and γ-particle coincidence techniques. The experiment involved the same reaction at the same center-of-mass energy as the earlier work of Poletti et al., but with target and projectile interchanged. In the present work, eight additional transitions have been identified as occurring in 52 Cr. This provides corroboration of results obtained more recently via 50 Ti(α,2nγ) 52 Cr reaction studies. A simple, efficient approach to the spectroscopy of weakly populated nuclear states which provides for unambiguous isotopic assignments is thus demonstrated

  3. Esquistossomose com lesões meningo-radículo-medulares

    Directory of Open Access Journals (Sweden)

    Horacio M. Canelas

    1951-03-01

    Full Text Available Os autores apresentam o caso de um paciente originário de Pernambuco, com antecedentes sugestivos de contaminação por furcocercárias e portador de hepatosplenomegalia, no qual se desenvolveu déficit motor generalizado, predominando nos membros inferiores, com arreflexia e hipotonia, hipoestesia superficial nas mãos e membros inferiores, e desordens da sensibilidade profunda consciente nos segmentos distais dos membros. O diagnóstico de esquistossomose sistêmica foi confirmado pelo encontro de ovos de Schistosoma mansoni nas fezes e pela positividade das reações intradèrmica e de fixação de complemento no sangue. O diagnóstico clínico de provável esquistossomose medular foi reforçado pelas alterações meningo-parenquimatosas do liqüido cefalorraqueano, destacando-se hiperci-tose média com eosinofilorraquia e, particularmente, a alta positividade da reação de fixação de complemento para bilharziose. Antes que pudesse ser instituído tratamento antimonial o paciente faleceu. À necropsia foram verificadas lesões que costumam ocorrer na esquistossomose visceral, mantendo-se o diagnóstico clínico, apesar de não terem sido encontrados ovos nos tecidos. Encèfalo normal; na medula foi comprovada a existência de aracnoidite produtiva, radiculite, degeneração bilateral de raízes da cauda eqüina e degeneração secundária dos fascículos gráceis.

  4. Study of energy transfer in single and multi-emissive layer using Gaussian peak fitting

    International Nuclear Information System (INIS)

    Yoon, Ju-An; Kim, You-Hyun; Kim, Nam Ho; Moon, Chang-Bum; He, Gufeng; Kim, Woo Young

    2014-01-01

    White organic light-emitting diodes(WOLEDs) were fabricated with the device structure of ITO(1800 Å)/NPB(700 Å)/emissive layer(300 Å)/Bphen(300 Å)/Liq(20 Å)/Al(1200 Å) using the two complementary colors method. Then, we investigated their electrical and optical characteristics to determine luminous efficiency, luminance and color coordinates of single, double, triple and quadruple emissive layered-WOLED. Thickness of emissive layer was fixed at 30 Å, and DPASN and BAlq were used for blue emissive host material and DCJTB was added as red dopant in the emissive layer. Then, we investigated the performance of OLEDs via its charge blocking structure and its different emissive region with emissive layers. Luminous efficiency of 5.30 cd/A at 50 mA/cm 2 of current density is obtained in WOLED device with double emissive layer of DPASN:DCJTB-0.1% (150 Å)/BAlq:DCJTB-0.1% (150 Å) and these are 80% higher than WOLED device with single emissive layer of DPASN:DCJTB-0.1% (300 Å). - Highlights: • White OLEDs with multiple-emissive layer were fabricated using p- and n-type emissive materials. • We fabricated WOLEDs only using a small quantity of fluorescent red dopant materials. • The spectroscopic analysis using multi-peak fits with a Gaussian function. • The explain electroluminescence spectra of white OLEDs with the multiple-emissive layer. • We examine changes in the number of emissive layer about white OLEDs performance

  5. Effects of Noise and Vibration on the Solid to Liquid Fluidization Transition in Small Dense Granular Systems Under Shear

    Science.gov (United States)

    Melhus, Martin Frederic

    2011-07-01

    Granular materials exhibit bulk properties that are distinct from conventional solids, liq- uids, and gases, due to the dissipative nature of the inter-granular forces. Understanding the fundamentals of granular materials draws upon and gives insight into many fields at the current frontiers of physics, such as plasticity of solids, fracture and friction, com- plex systems such as colloids, foams and suspensions, and a variety of biological systems. Particulate flows are widespread in geophysics, and are also essential to many industries. Despite the importance of these phenomena, we lack a theoretical model that explains most behaviors of granular materials. Since granular assemblies are highly dissipative, they are often far from mechanical equilibrium, making most classical analyses inappli- cable. A theory for dilute granular systems exists, but for dense granular systems (by far the majority of granular systems in the real world) no comparable theory is accepted. We approach this problem by examining the fluidization, or transition from solid to liquid, in dense granular systems. In this study, the separate effects of random noise and vibration on the static to flowing transition of a dense granular assembly under planar shear is studied numerically using soft contact particle dynamics simulations in two dimensions. We focus on small systems in a thin planar Couette cell, examining the bistable region while increasing shear, with varying amounts of random noise or vibration, and determine the statistics of the shear required for the onset of flow. We find that the applied power is the key parameter in determining the magnitude of the effects of the noise or vibration, with vibration frequency also having an influence. Similarities and differences between noise and vibration are determined, and the results compare favorably with a two phase model for dense granular flow.

  6. Neurocisticercose: formas clínicas pouco frequentes. II - formas do ângulo pontocerebelar

    Directory of Open Access Journals (Sweden)

    Horácio M. Canelas

    1962-06-01

    Full Text Available A localização de cisticercos no recesso lateral da cisterna pontina poderá levar à constituição de uma síndrome do ângulo pontocerebelar, simulando eventualmente um neurinoma do acústico. São revistos os casos dessa forma clínica de neurocisticercose descritos na literatura. O problema do diagnóstico diferencial com os tumores (neurinomas do acústico é discutido sob os pontos de vista clínico e radiológico. Os autores apresentam 7 casos de cisticercose do ângulo pontocerebelar. O diagnóstico etiológico foi estabelecido pela positividade da reação de fixação do complemento para cisticercose no liqüido cefalorraqueano em 5 casos e, em 2, pela cirurgia e/ou necropsia. Em todos os pacientes havia sintomas de lesão coclear, bilaterais em 2; lesão vestibular foi comprovada em 4 casos. Em 6 pacientes ocorreram sinais indicativos de lesão unilateral do nervo trigêmeo. Comprometimento do nervo facial foi observado em 4 casos. Existia faringoplegia em 3 casos e estrabismo interno em 2. Em 3 casos não foram observados sinais cerebelares, o que faria com que o diagnóstico propendesse para o de tumor do acústico, não fôssem outras características clínicas e subsidiárias. A síndrome de hipertensão intracraniana era nítida em 5 pacientes. Convulsões ocorreram em 2 casos. A propósito do resultado dos exames radiológicos, os autores salientam que, num dos casos, foi verificada amputação da ponta do rochedo ipsolateral à síndrome do ângulo pontocerebelar; outros comemorativos do caso levaram, porém, a rejeitar a hipótese de tumor (neurinoma do acústico, tendo a cirurgia comprovado o acêrto do diagnóstico clínico.

  7. Endoscopic endonasal transsphenoidal approach for pituitary adenomas: technical aspects and report of casuistic Abordagem endoscópica endonasal para adenomas de hipófise: aspectos técnicos e relato de casuística

    Directory of Open Access Journals (Sweden)

    Américo Rubens Leite dos Santos

    2010-08-01

    Full Text Available OBJECTIVE: Analyse technical aspects, effectiveness and morbidity of the endoscopic endonasal transphenoidal approach for pituitary adenomas. METHOD: From January 2005 to September 2008, 30 consecutive patients underwent endoscopic endonasal resection of pituitary adenomas with a follow up from 3 to 36 months. Their medical charts were retrospectively analysed. RESULTS: There were 18 women and 12 men, mean age 44 years (range 17-65 yr. Among the 30 patients, 23 had macroadenomas and 7 microadenomas. Twelve patients had non-functioning tumors, 9 had ACTH-secreting tumors, 8 had GH-secreting tumors and 1 prolactinoma. Complete resection and hormonal control was achieved in all microadenomas. Macroadenomas were completely removed in 6 patients, subtotal resection in 6 and partial resection in 11. Three patients had diabetes insipidus and 5 had CSF leaks treated with lumbar drainage. CONCLUSION: The endonasal endoscopic approach for pituitary tumors is effective and has low morbidity.OBJETIVO: Analisar aspectos técnicos, eficácia e morbidade do acesso transesfenoidal endonasal endoscópico para adenomas hipofisários. MÉTODO: Estudo retrospectivo de trinta pacientes consecutivos submetidos à ressecção endoscópica endonasal de adenomas hipofisários, entre janeiro de 2005 e setembro de 2008, com seguimento pós-operatório entre três e 36 meses. RESULTADOS: Foram operados 18 mulheres e 12 homens com idades variando entre 17 e 65 anos (média 44 anos. Entre os 30 casos operados, 23 eram macroadenomas e sete microadenomas. Doze pacientes apresentavam adenomas não-funcionantes, nove tumores secretores de ACTH, oito tumores secretores de GH e um prolactinoma. Ressecção macroscópica completa e controle endócrino foram conseguidos em todos microadenomas. Ressecção dos macroadenomas foi completa em seis pacientes, subtotal em seis e parcial em seis casos. Três pacientes desenvolveram diabetes insipidus e cinco tiveram fístula liqüórica p

  8. Mieloses funiculares considerações a propósito de 110 casos

    Directory of Open Access Journals (Sweden)

    Horacio Martins Canelas

    1960-06-01

    Full Text Available O autor, revendo o conceito atual da etiopatogenia das mieloses funiculares, conclui que, na determinação do processo desmielinizante, além da carência de vitamina B12 e da acloridria gástrica, participam outros fatores, carenciais e/ou alérgicos. Baseado no estudo de 110 casos com lesões gástricas constitucionais (100 casos ou adquiridas (10 casos, o autor discute o problema do diagnóstico. São consideradas as síndromes periférica, funicular dorsal, "piramidal" e encefálica. É ressaltada a importância do exame da sensibilidade vibratória, particularmente por método quantitativo, que revelou, em elevada percentagem dos casos, distúrbios da palestesia também nas mãos. Entre os exames complementares, é salientado o valor do hemograma, do mielograma, da dosagem da acidez gástrica, da determinação da absorção da vitamina B12 radioativa; são também consideradas as alterações electrencefalográficas e do liqüido cefalorraqueano. Os resultados terapêuticos em 44 casos são avaliados através do estudo semiquantitativo da sintomatologia neurológica. Embora a vitamina B12 tenha proporcionado maiores índices de melhora, os demais medicamentos (extrato hepático, ácido fólico e adrenocorticotropina também influenciaram favoravelmente o quadro neurológico. Em vista da pequena representação numérica da casuística nos grupos correspondentes aos quatro esquemas terapêuticos, o autor não emite conclusão definitiva. Salienta, porém, que êsses resultados demonstram a necessidade de prosseguir nos estudos sôbre a etiopatogenia das mieloses funiculares, no sentido de esclarecer as numerosas incógnitas que ainda perduram.

  9. Phase equilibria and the thermodynamic properties of methyl and ethyl esters of carboxylic acids. 1. Methyl n-butanoate and ethyl propanoate

    International Nuclear Information System (INIS)

    Agafonova, Luba E.; Varushchenko, Raisa M.; Druzhinina, Anna I.; Polyakova, Olga V.

    2012-01-01

    Highlights: ► Heat capacities, fusion properties of CH 3 OC(O)C 3 H 7 measured by adiabatic calorimetry. ► The temperature dependence of vapour pressure determined by comparative ebulliometry. ► The thermodynamic functions derived from experiment and calculated by DFT method. ► Extending vapour pressure of moderate interval to entire region of liquid. ► An increment of the entropy of carbonyl group was defined from experimental data. - Abstract: The heat capacity of methyl n-butanoate in crystalline and liquid states was measured by vacuum adiabatic calorimetry over the temperature range from (8 to 372) K. The triple point temperature, the enthalpy and entropy of fusion, and the purity of the sample were determined. The saturated vapour pressure and the boiling temperatures were determined by comparative ebulliometry in the “atmospheric” pressure range 10.8 ⩽ (p/kPa) ⩽ 99.6. The normal boiling temperature, T n.b , and the enthalpy of vaporization at T = 298.15 K and T n.b were derived. The thermodynamic functions (absolute entropy and changes of the enthalpy, and Gibbs free energy) were derived for the solid and liquid states in the temperature range studied and for the ideal gas state at T = 298.15 K. The ideal gas heat capacities and the absolute entropies of methyl n-butanoate (MeBu) and ethyl propanoate (EtPr) were calculated by statistical thermodynamics on the basis of the molecular constants determined by the use of density functional theory on the B3LYP level. The experimental vapour pressure of MeBu and EtPr of moderate temperature intervals, Δ exp T = (59/65) K, were extended to the entire range of the liquids, Δ liq T = (364.7/345.7) K by the methods of the corresponding states law and simultaneous treatment of the pT-parameters and low-temperature heat capacities of the ideal gas and liquid, respectively. An additive contribution of the carbonyl group CO–(C, O) connected with C and O atoms was determined for calculation of the

  10. Hidrocefalia ou hidranencefalia: valor da transiluminação do crânio no diagnóstico diferencial. Estudo anátomo-clínico de dois casos

    Directory of Open Access Journals (Sweden)

    Antonio B. Lefèvre

    1955-12-01

    Full Text Available São apresentados dois casos anátomo-clínicos, um de hidranencefalia e outro de hidrocefalia congênita por estenose do aqueduto de Sylvius. O exame neurológico revelou, nos dois casos, um quadro semelhante, cujas caracte- rísticas lembram as encontradas em um recém-nascido normal. Nos dois casos foi feita a transiluminação do crânio e o estudo da circulação cerebral por meio de carótido-angiografia. Dos fatos observados podem ser destacados os seguintes aspectos: 1 A transiluminação não parece ser elemento seguro para o diagnóstico diferencial entre a hidrocefalia e a hidranencefalia, pois, no caso de hidrocefalia (caso 2 foi obtida nítida transparência, enquanto que no caso de hidranencefalia (caso 1 esta prova foi completamente negativa; deve notar-se que o liqüido contido no interior do crânio do paciente de hidranencefalia era fortemente turvo, o que talvez explique não ter sido obtida a transiluminação. 2 Não houve correspondência entre a distribuição arterial observada pela carótido-angiografia e os achados anátomo-patológicos verificados no caso de hidranencefalia; as artérias cerebral anterior e cerebral média foram nitidamente visualizadas e não obstante havia falta das porções dos hemisférios que seriam supridas por estas artérias; ao contrário, o território irrigado pela cerebral posterior estava relativamente bastante desenvolvido, embora esta artéria estivesse representada apenas por penachos de vasos tortuosos, curtos e muito delgados. 3 As presentes observações não permitem avaliar a importância da eletrencefalografia no diagnóstico diferencial entre hidrocefalia e hidranencefalia, pois não foi possível realizar o traçado no caso 2 (hidranencefalia.

  11. Liquid Metallic Hydrogen II. A Critical Assessment of Current and Primordial Helium Levels in the Sun

    Directory of Open Access Journals (Sweden)

    Robitaille P.-M.

    2013-04-01

    Full Text Available Before a solar model becomes viable in astrophysics, one mus t consider how the ele- mental constitution of the Sun was ascertained, especially relative to its principle com- ponents: hydrogen and helium. Liquid metallic hydrogen has been proposed as a solar structural material for models based on condensed matter (e .g. Robitaille P.-M. Liq- uid Metallic Hydrogen: A Building Block for the Liquid Sun. Progr. Phys. , 2011, v. 3, 60–74. There can be little doubt that hydrogen plays a d ominant role in the uni- verse and in the stars; the massive abundance of hydrogen in t he Sun was established long ago. Today, it can be demonstrated that the near isointe nse nature of the Sun’s Balmer lines provides strong confirmatory evidence for a dis tinct solar surface. The situation relative to helium remains less conclusive. Stil l, helium occupies a prominent role in astronomy, both as an element associated with cosmol ogy and as a byproduct of nuclear energy generation, though its abundances within the Sun cannot be reliably estimated using theoretical approaches. With respect to th e determination of helium lev- els, the element remains spectroscopically silent at the le vel of the photosphere. While helium can be monitored with ease in the chromosphere and the prominences of the corona using spectroscopic methods, these measures are hig hly variable and responsive to elevated solar activity and nuclear fragmentation. Dire ct assays of the solar winds are currently viewed as incapable of providing definitive in formation regarding solar helium abundances. As a result, insight relative to helium r emains strictly based on the- oretical estimates which couple helioseismological appro aches to metrics derived from solar models. Despite their “state of the art” nature, heliu m estimates based on solar models and helioseismology are suspect on several fronts, i ncluding their reliance on solar opacities. The best knowledge can only come from the so

  12. Dependence of surface morphology on molecular structure and its influence on the properties of OLEDs

    Energy Technology Data Exchange (ETDEWEB)

    Lim, S.H. [Department of Chemical Engineering, Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of); Ryu, G.Y. [Department of Electric Information and Control Engineering, Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of); Seo, J.H.; Park, J.H. [Center for Organic Materials and Information Devices (COMID), Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of); Department of Information Display, Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of); Youn, S.W. [Department of Chemical Engineering, Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of); Kim, Y.K. [Center for Organic Materials and Information Devices (COMID), Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of); Department of Information Display, Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of); Shin, D.M. [Department of Chemical Engineering, Hongik University, 72-1, Sangsu-Dong, Mapo-Gu, Seoul 121-791 (Korea, Republic of)], E-mail: shindm@wow.hongik.ac.kr

    2008-09-15

    Most organic light-emitting diodes (OLEDs) have a multilayer structure composed of organic layers such as a hole injection layer (HIL), a hole transport layer (HTL), an emission layer (EML), an electron transport layer (ETL) and an electron injection layer (EIL) sandwiched between two electrodes. The organic layers are thin solid films with a thickness from a few nano meters to a few tenths nano meter, respectively. Surface morphology of an organic thin solid film in OLEDs depends on the molecular structure of the organic material and has an affect on device performance. To analyze the effect of surface morphology of an organic thin solid film on fluorescence and electroluminescence (EL) properties, thin solid films of 4-(dicyanomethylene)-2-methyl-6-(julolidin-4-yl-vinyl)-4H-pyran (DCM2) and new red fluorophores, (2E,2'E)-3,3'-[4,4''-bis(dimethylamino)-1,1':4',1''-terphenyl-2',5'-diyl] bis[2= -(2-thienyl)acrylonitrile] (ABCV-Th) and (2Z,2'Z)-3,3'-[4,4''-bis(dimethylamino)-1,1':4',1''-terphenyl-2',5'-diyl] bis(2-phenylacrylonitrile) (ABCV-P) were investigated by atomic force microscopy (AFM). The samples for EL and AFM measurement were fabricated by the high-vacuum thermal deposition (8x10{sup -7} Torr) of organic materials onto the surface of indium tin oxide (ITO)-coated glass substrate, in which the layer structures of samples for AFM measurement and those for EL measurement were ITO/NPB (40 nm)/red emitters (80 nm) and ITO/NPB (40 nm)/red emitters (80 nm)/BCP (30 nm)/Liq (2 nm)/Al (100 nm), respectively. The analysis based on AFM measurements well supported that the photoluminescence properties and the device performance were very much dependent upon surface morphology of an organic thin layer.

  13. Balance the Carrier Mobility To Achieve High Performance Exciplex OLED Using a Triazine-Based Acceptor.

    Science.gov (United States)

    Hung, Wen-Yi; Chiang, Pin-Yi; Lin, Shih-Wei; Tang, Wei-Chieh; Chen, Yi-Ting; Liu, Shih-Hung; Chou, Pi-Tai; Hung, Yi-Tzu; Wong, Ken-Tsung

    2016-02-01

    A star-shaped 1,3,5-triazine/cyano hybrid molecule CN-T2T was designed and synthesized as a new electron acceptor for efficient exciplex-based OLED emitter by mixing with a suitable electron donor (Tris-PCz). The CN-T2T/Tris-PCz exciplex emission shows a high ΦPL of 0.53 and a small ΔET-S = -0.59 kcal/mol, affording intrinsically efficient fluorescence and highly efficient exciton up-conversion. The large energy level offsets between Tris-PCz and CN-T2T and the balanced hole and electron mobility of Tris-PCz and CN-T2T, respectively, ensuring sufficient carrier density accumulated in the interface for efficient generation of exciplex excitons. Employing a facile device structure composed as ITO/4% ReO3:Tris-PCz (60 nm)/Tris-PCz (15 nm)/Tris-PCz:CN-T2T(1:1) (25 nm)/CN-T2T (50 nm)/Liq (0.5 nm)/Al (100 nm), in which the electron-hole capture is efficient without additional carrier injection barrier from donor (or acceptor) molecule and carriers mobilities are balanced in the emitting layer, leads to a highly efficient green exciplex OLED with external quantum efficiency (EQE) of 11.9%. The obtained EQE is 18% higher than that of a comparison device using an exciplex exhibiting a comparable ΦPL (0.50), in which TCTA shows similar energy levels but higher hole mobility as compared with Tris-PCz. Our results clearly indicate the significance of mobility balance in governing the efficiency of exciplex-based OLED. Exploiting the Tris-PCz:CN-T2T exciplex as the host, we further demonstrated highly efficient yellow and red fluorescent OLEDs by doping 1 wt % Rubrene and DCJTB as emitter, achieving high EQE of 6.9 and 9.7%, respectively.

  14. Modification in the assembly technique of histological sections for analysis of spatial distribution of boron by autoradiography

    International Nuclear Information System (INIS)

    Portu, A; Carpano, M; Dagrosa, A; Pozzi, E; Thorp, S; Curotto, P; Cabrini, R L; Saint Martin, G

    2012-01-01

    The Boron Neutron Capture Therapy (BNCT) is a modality for the treatment of cancer, based on the capture reaction 10 B(n,α) 7 Li. The emitted particles are highly transferred linear of energy and have a short range in tissue (10 μ). Therefore, if the boron is selectively accumulates in tumor cellulo, the damage will be limited to preserving normal cellulo. Thus, the knowledge of the location of 10 B in the different structures of biological tissues as tumor and surrounding tissue, is essential when considering BNCT treatment (Barth et al., 2005). Neutron autoradiography is one of the few methods that allow studying the distribution spatial of elements emitters in a material containing such. As part of BNCT, the first step in performing autoradiography involves placing a freeze tissue section on a nuclear track detector (SSNTD) (Wittig et al., 2008). For this purpose, tissue samples are fixed in N 2 (liq) when they are resected after infusion boronated compound. The sample-detector arrangement is irradiated with thermal neutrons and elements cast in the capture reaction zones produce latent damage SSNTD. Chemically attacking the detector, this latent trace level can be amplified by optical microscopy. Thus, the distribution of 10 B in biological samples can be evaluated, so that this technique is suitable for studying the uptake of boron compounds for the different histological structures. In our laboratory, we have developed neutron autoradiography and has been applied to the study of different biological models (Portu et al., 2011a). In particular, the study conducted by the micro-distribution 10 B in tumors from nude mice model of cutaneous melanomas injected with boronophenylalanine (BPA) (Carpano et al, 2010;. Portu et al, 2011b.). Still using means of support for the sample to be cut, as OCTTM, the lack of structure of necrotic areas of tumors such causes tearing of these regions in the cutting process, which prevents achieving adequate for analysis sections

  15. Sôbre as paraplegias cifoscolióticas: tratamento neurocirúrgico

    Directory of Open Access Journals (Sweden)

    Roberto Melaragno Filho

    1951-03-01

    exame do liqüido cefalorraquidiano, em punção lombar, revelou bloqueio completo do canal vertebral e liqüido com característica dissociação albumino-citológica. As radiografias demonstraram uma cifoscoliose dorsal alta, dextro-convexa, com ápice em T4; hemivertebra triangular, correspondendo a T4, de base direita articulada em T3 e T5; ausência da 5.ª costela esquerda, enquanto que a 5.ª costela direita, de curto trajeto, se achava fundida com a 6.ª costela. Os exames mieloscópicos e mielográficos vieram comprovar o bloqueio, pela parada do lipiodol entre T3 e T4. Decidiu-se então o tratamento neurocirúrgico, cujos tempos essenciais foram os seguintes: retirada das apó-fises espinhosas e lâminas de C5 a T4; feitura de novo leito ósseo entre T3 e T5, para a medula, através da escavação de uma porção dos processos transversos à esquerda, bem como dos ligamentos interósseos, dos tubérculos costais e de uma porção correspondendo ao colo das costelas (esse leito ósseo foi recoberto com oxicel ; transposição da medula para seu leito mediante a secção, entre clips, das raízes T1 a T4 bilateralmente; abertura da dura-máter e sondagem do canal; fechamento, conservando-se a dura-máter aberta. Dois dias após a intervenção, o paciente já conseguia executar alguns movimentos débeis de flexão e de extensão dos pés. Cerca de 30 dias depois da laminectomia, o paciente já ficava de pé, amparado O exame neurológico, realizado 48 dias após o ato cirúrgico, revelou ausência de qualquer paralisia muscular, embora os movimentos fossem realizados com diminuição de energia; hiperreflexia profunda, sinal de Babinski à direita e inconstante à esquerda; sensibilidade superficial quase normalizada, persistência do bloqueio e liquor com as características de estase. Não obstante, as melhoras progrediram, de modo que o paciente consegue hoje exercer suas atividades normais. O exame neurológico está normalizado, com exceção de ligeiros

  16. Volume de iogurte light e sensações subjetivas do apetite de homens eutróficos e com excesso de peso Volume of light yogurt and subjective appetite sensations in normal-weight and overweight men

    Directory of Open Access Journals (Sweden)

    Luciana Neri Nobre

    2006-10-01

    Full Text Available OBJETIVO: Avaliar, independentemente de outras variáveis, o efeito do volume de iogurte light sobre os parâmetros de ingestão alimentar de homens saudáveis. MÉTODOS: Foi feita incorporação de ar ao iogurte por adição de um produto comercialmente disponível -Emustab® - (6g/300ml com posterior homogeneização em liqüidificador semi-industrial. Utilizaram-se três volumes de iogurte: 300, 450 e 600ml. Trabalhou-se com 20 participantes saudáveis, sendo 10 eutróficos, com índice de massa corporal entre 19 e 24,9kg/m² e 10 com excesso de peso, índice de massa corporal >25kg/m². Cada um deles recebeu um volume de iogurte em três diferentes dias, pela manhã, em jejum de 12 horas. Uma escala de analogia visual foi utilizada, num período de 4 horas e 30 minutos após ingestão de cada volume do iogurte, para avaliar sensações subjetivas de saciedade, fome e desejo por alimentos específicos. RESULTADOS: Os volumes do iogurte light afetaram a saciedade dos dois grupos estudados, sendo que o maior volume exerceu melhor essa ação (pOBJECTIVE: This study aimed to evaluate the effect of light yogurt volume on the food intake of healthy men regardless of other variables. METHODS: Air was added to the yogurt by mixing it with a commercially available product, Emustab®, (6g/300ml and homogenized in a semi-industrial blender. Three volumes of yogurt were used: 300, 450 and 600ml. Twenty healthy volunteers participated in the study, 10 with normal weight, Body Mass Index from 19 to 24.9kg/m² and 10 with excess weight, Body Mass Index >25kg/m². Each one of them was given a yogurt volume in three different days in the morning, after a 12 hour fast. After the intake of each yogurt volume, a visual analog scale was used to assess the subjective sensations of satiety, hunger and desire for specific foods. RESULTS: Light yogurt volumes affected the satiety of both studied groups and the greater volume was more effective (p<0.01. The highest

  17. A novel titanium-containing catalyst for PET bottle flake%新型钛系催化剂合成瓶用聚酯切片的研究

    Institute of Scientific and Technical Information of China (English)

    关震宇; 熊金根; 周文乐

    2016-01-01

    采用均一的液相新型钛系催化剂STiC-B1,在2 L间歇式聚合反应釜中制备钛系瓶用聚对苯二甲酸乙二醇酯( PET)切片;考察了催化剂中主要成分对 PET 切片色相及乙醛含量的影响,以及不同催化体系的PET切片的结晶性能及热性能;并进行了工业化应用评价。结果表明:在相同的聚合工艺条件下,STiC-B1钛用量为5μg/g(相对于PET)时的催化活性及其所得PET切片乙醛含量与乙二醇锑锑用量为180μg/g时相当;钛系PET切片结晶速度较锑系PET切片的慢,较慢的结晶速度可避免PET切片降温时出现结晶过快,从而有利于吹瓶;工业化应用表明钛系PET瓶片质量指标基本达到锑系PET瓶片的水平,其瓶坯乙醛含量低于锑系PET瓶坯的乙醛含量。%A bottle-grade titanium-containing polyethylene terephthalate ( PET) chip was prepared by using a novel uniform liq-uid-phase titanium-containing catalyst STiC-B1 on a two-liter batch polymerization reactor .The effects of the main components in the catalyst on the hue and acetaldehyde content of PET chip were investigated .The crystallization behavior and thermal proper-ties of PET chips were studied with different catalyst systems .The industrial application was evaluated .The results showed that STiC-B1 and ethylene glycol antimony provided the equal catalytic activity and the same acetaldehyde content of PET chips when the titanium content was 5 μg/g or the antimony content was 180μg/g based on PET;the crystallization rate of titanium-contai-ning PET chips was lower than that of antimony-containing PET chips , which avoided the extremely rapid crystallization behavior while cooling and thus helped the bottle blowing .And the industrial application showed that the titanium-containing catalyst pro-vided the close quality index of PET bottle flake and the lower acetaldehyde content of bottle blank as compared with antimony -containing catalyst .

  18. HIDROLISADO DE FÉCULA DE MANDIOCA COMO ADJUNTO DE MALTE NA FABRICAÇÃO DE CERVEJA: AVALIAÇÃO QUÍMICA E SENSORIAL

    Directory of Open Access Journals (Sweden)

    Waldemar G. VENTURINI FILHO

    1998-05-01

    Full Text Available Em virtude da progressiva substituição dos adjuntos amiláceos pelos xaropes com alta concentração de maltose nas cervejarias brasileiras, o presente trabalho teve por objetivo comparar hidrolisados de milho e de mandioca, como adjunto de malte, na fabricação de cerveja tipo Pilsen, em escala de laboratório. Os hidrolisados foram produzidos a partir de amido de milho e fécula de mandioca, sendo que na liqüefação e sacarificação da fração amilácea destes produtos foram utilizadas, respectivamente, as enzimas comerciais Termamil (alfa amilase bacteriana e Fungamil (alfa amilase fúngica. Na fabricação das cervejas, a proporção de malte e hidrolisado foi de 2 para 1, na base do extrato. O mosto foi produzido pelo processo de infusão e após resfriamento e clarificação foi inoculado com levedura cervejeira de baixa fermentação. A fermentação transcorreu a 10 °C até 90% de atenuação do extrato aparente fermentável. As cervejas foram engarrafadas e, em seguida, maturadas a 0 °C, por 14 dias. Terminado o processo de fabricação, as cervejas foram analisadas química e sensorialmente. A semelhança na composição química dos hidrolisados de milho e de mandioca refletiu na composição química dos mostos e das cervejas. Não houve diferença estatística entre os mostos e entre as cervejas testadas para todos os parâmetros químicos analisados. Também, não existiu diferença sensorial entre as cervejas produzidas com hidrolisado de milho e hidrolisado de mandioca. Concluiu-se que a fécula de mandioca apresenta potencial de uso como matéria prima para a fabricação de xarope de maltose de uso cervejeiro e que há elevada probabilidade de sucesso no uso desse xarope para a fabricação de cervejas.The brazilians breweries replace progressively starchy adjuncts by sugary liquid adjuncts made with maize. Thus, the objective of present work was saccharify cassava and maize and use them as malt adjunct on Pilsen beer

  19. Neurocisticercose: formas clínicas pouco freqüentes. I - formas hemiplégicas

    Directory of Open Access Journals (Sweden)

    Horácio M. Canelas

    1962-06-01

    Full Text Available Os autores salientam a raridade dos déficits motores com distribuição mono ou hemiplégica, conseqüentes a lesões encefálicas de natureza cisticer-cótica. Ressaltam, outrossim, a dificuldade dos problemas diagnósticos que eventualmente se impõem nesses casos. Discutindo a patogenia dêsses processos, apontam dois mecanismos principais: as paralisias determinadas por focos encefálicos, constituídos por granulomas, cisticercóticos ou à distância, e os acidentes cerebrovasculares ocasionadas pelas alterações vasculares, cuja importância é realçada. São apresentados 19 casos de neurocisticercose, incluindo 17 formas hemiplégicas e 2 monoplégicas. Em todos, o diagnóstico etiológico foi estabelecido pela positividade da reação de fixação do complemento para cisticercose no liqüido cefalorraqueano, corroborado, em 2 casos, pela cirurgia e pela necropsia. Convulsões foram registradas em 10 casos (focais em 7 e generalizadas em 3. Sintomas de hipertensão intracraniana foram assinalados em 4 pacientes. A hemiplegia instalou-se sob forma de icto em 14 pacientes. Em 3 casos houve elementos altamente sugestivos de patogenia predominantemente vascular; em 3, a sintomatologia relacionou-se diretamente ao granuloma parasitário, embora deva ter havido participação do processo angiopático; em 1 caso, tratava-se, provavelmente, de paralisia pós-convulsiva; em 3, embora não houvesse suficientes dados complementares, os elementos clínicos levaram a salientar a importância do fator vascular na determinação da hemiplegia. Em 5 pacientes o déficit motor instalou-se de modo lento e progressivo. Em 2 casos foram encontrados e extirpados cisticercos situados no córtex cerebral, tendo a necropsia revelado, em um deles, amolecimento isquêmico na região parietal contralateral à hemiplegia; em 1 havia eisticercose da fossa craniana posterior, associada a lesão cortical traduzida por intensas alterações eletrencefalográficas; 2

  20. Blastomicose do sistema nervoso

    Directory of Open Access Journals (Sweden)

    Horácio M. Canelas

    1951-09-01

    Full Text Available Os autores chamam a atenção sôbre os erros de diagnóstico nos casos de neuroblastomicose, seja nas formas meningoencefálicas, seja nas tumorais. São focalizadas a paracoccidioidose e a criptococose. Depois de caracterizarem clìnicamente a paracoccidioidose, acentuam a raridade das formas nervosas (1,2% dos casos dessa micose autopsiados no Departamento de Anatomia Patológica da Faculdade de Medicina da Universidade de São Paulo. Pela revisão da literatura foi verificado haver apenas 12 casos registrados. 0 caso de Casiello e Klass é o único em que o diagnóstico foi feito em vida; os demais, ou constituem achado de necropsia, ou foram inesperadamente revelados pelo exame histopatológico realizado após intervenções cirúrgicas. Os autores registram 2 casos de paracoccidioidose do sistema nervoso. No primeiro, tratava-se de meningomielorra-diculite crônica, sendo o parasito identificado no escarro; o segundo era portador de síndrome de compressão medular, cuja patogenia é discutida pelos autores, tendo sido a etiologia paracoccidióidica comprovada pelo exame da polpa e biópsia ganglionares. Considerações clínicas sôbre a criptococose precedem o relato de um caso de meningoencefalomielite subaguda, no qual fôra feito em vida o diagnóstico de paracoccidioidose, pelo exame micológico do liqüido cefalorraqueano; êste paciente, embora medicado com doses maciças de sulfa e tiossemicarbarsona, veio a falecer, tendo o exame anátomo-patológico revelado tratar-se, na realidade, de lesões nervosas produzidas pelo Crypíococcus neo-formans. Nos três casos era incisivo o caráter neurocirúrgico da sintomatologia. Entretanto, ante o diagnóstico de paracoccidioidose, foi instituído tratamento pelas sulfas, vacina específica e tiossemicarbarsona. Os resultados foram excelentes no caso 2, em que a terapêutica pôde ser instituída mais precocemente; melhoras também foram obtidas no caso 1. No caso 3, foram verificadas

  1. Chapter 8: Plasma operation and control

    Science.gov (United States)

    ITER Physics Expert Group on Disruptions, Control, Plasma, and MHD; ITER Physics Expert Group on Energetic Particles, Heating, Current and Drive; ITER Physics Expert Group on Diagnostics; ITER Physics Basis Editors

    1999-12-01

    well as in plasma periphery and divertor. The planned diagnostics (Chapter 7) serve as sensors for kinetic control, while gas and pellet fuelling, auxiliary power and angular momentum input, impurity injection, and non-inductive current drive constitute the control actuators. For example, in an ignited plasma, core density controls fusion power output. Kinetic control algorithms vary according to the plasma state, e.g. H- or L-mode. Generally, present facilities have demonstrated the kinetic control methods required for a reactor scale device. Plasma initiation - breakdown, burnthrough and initial current ramp - in reactor scale tokamaks will not involve physics differing from that found in present day devices. For ITER, the induced electric field in the chamber will be ~0.3V· m-1 - comparable to that required by breakdown theory but somewhat smaller than in present devices. Thus, a start-up 3MW electron cyclotron heating system will be employed to assure burnthrough. Simulations show that plasma current ramp up and termination in a reactor scale device can follow procedures developed to avoid disruption in present devices. In particular, simulations remain in the stable area of the li-q plane. For design purposes, the resistive V·s consumed during initiation is found, by experiments, to follow the Ejima expression, 0.45μ0 RIp. Advanced tokamak control has two distinct goals. First, control of density, auxiliary power, and inductive current ramping to attain reverse shear q profiles and internal transport barriers, which persist until dissipated by magnetic flux diffusion. Such internal transport barriers can lead to transient ignition. Second, combined use poloidal field shape control with non-inductive current drive and NBI angular momentum injection to create and control steady state, high bootstrap fraction, reverse shear discharges. Active n = 1 magnetic feedback and/or driven rotation will be required to suppress resistive wall modes for steady state plasmas

  2. On Solar Granulations, Limb Darkening, and Sunspots: Brief Insights in Remembrance of Father Angelo Secchi

    Directory of Open Access Journals (Sweden)

    Robitaille P.-M.

    2011-07-01

    support the idea of a condensed Sun. With respect to sunspots, the decrease in emis- sivity with increasing magnetic field strength lends powerful observational support to the idea that these structures are comprised of liquid metallic hydrogen. In this model, the inter-atomic lattice dimensions within sunspots are reduced. This increases the den- sity and metallic character relative to photospheric material, while at the same time decreasing emissivity. Metals are well known to have lowered directional emissivities with respect to non-metals. Greater metallicity produces lower emissivity. The idea that density is increased within sunspots is supported by helioseismology. Thus, a liq- uid metallic hydrogen model brings with it many advantages in understanding both the emissivity of the solar surface and its vast array of structures. These realities reveal that Father Secchi, like Herbert Spencer and Gustav Kirchhoff, was correct in his insistence that condensed matter is present on the photosphere. Secchi and his contemporaries were well aware that gases are unable to impart the observed structure.

  3. Complicações neurológicas por osteomas dos seios paranasais: A propósito de um caso de pneumatocele extradural por osteoma do seio frontal

    Directory of Open Access Journals (Sweden)

    R. Melaragno Filho

    1951-06-01

    Full Text Available Os autores relatam o caso de um homem de 38 anos de idade que apresentava uma hemiparesia direita nítida, sem afasia, datando de cerca de um mês. O déficit motor no dimídio direito se iniciara com violenta cefaléia, rebelde ao uso de analgésicos, mas que, pouco a pouco, cedeu completamente. O exame clínico não revelou qualquer causa capaz de explicar a hemiparesia. Liqüido cefaiorraquidiano e exame oftalmoscòpico inteiramente normais. As radiografias simples do crânio mostravam opacificação de consistência compacta no seio frontal e imagem aérea, volumosa, ocupando a maior parte do hemicrânio esquerdo. Os cortes planigráficos sagitais revelaram erosão da parede posterior e do assoalho do seio frontal, sem continuidade com a coleção de ar. Durante a operação foi verificada integridade da dura mater. Dias após a intervenção, a motricidade voluntária do hemicorpo direito já havia melhorado consideravelmente e, um mês após, o exame neurológico foi totalmente negativo. Tratava-se de osteoma ebùrneo. Após estudar os aspectos otorrinolaringológicos dos osteomas dos seios frontais, os autores consideram as suas eventuais complicações. Assim, se o tumor crescer para o lado, poderá invadir a órbita, causando exoftalmo, proptose e diplopia; expandindo-se para trás, poderá erosar a parede posterior do seio frontal, ocasionando pneumatocele extradural, como ocorreu no caso registrado neste trabalho; sucessivamente, poderá também perfurar a dura mater (pneumatocele subdural, invadir o tecido cerebral (pneumatocele intracerebral e mesmo se comunicar com o ventrículo lateral (pneumatocele ventricular. Essas coleções aéreas intracranianas (pneumocéfalos são eventualidades excepcionais em doença também rara. De fato, até 1941, haviam sido registrados 321 casos de osteomas, dos quais apenas 8 se complicaram de pneumocéfalo: 2 extradurais, 4 intracerebrais e 2 ventriculares. Por outro lado, essas complica

  4. Average Potential Temperature of the Upper Mantle and Excess Temperatures Beneath Regions of Active Upwelling

    Science.gov (United States)

    Putirka, K. D.

    2006-05-01

    The question as to whether any particular oceanic island is the result of a thermal mantle plume, is a question of whether volcanism is the result of passive upwelling, as at mid-ocean ridges, or active upwelling, driven by thermally buoyant material. When upwelling is passive, mantle temperatures reflect average or ambient upper mantle values. In contrast, sites of thermally driven active upwellings will have elevated (or excess) mantle temperatures, driven by some source of excess heat. Skeptics of the plume hypothesis suggest that the maximum temperatures at ocean islands are similar to maximum temperatures at mid-ocean ridges (Anderson, 2000; Green et al., 2001). Olivine-liquid thermometry, when applied to Hawaii, Iceland, and global MORB, belie this hypothesis. Olivine-liquid equilibria provide the most accurate means of estimating mantle temperatures, which are highly sensitive to the forsterite (Fo) contents of olivines, and the FeO content of coexisting liquids. Their application shows that mantle temperatures in the MORB source region are less than temperatures at both Hawaii and Iceland. The Siqueiros Transform may provide the most precise estimate of TpMORB because high MgO glass compositions there have been affected only by olivine fractionation, so primitive FeOliq is known; olivine thermometry yields TpSiqueiros = 1430 ±59°C. A global database of 22,000 MORB show that most MORB have slightly higher FeOliq than at Siqueiros, which translates to higher calculated mantle potential temperatures. If the values for Fomax (= 91.5) and KD (Fe-Mg)ol-liq (= 0.29) at Siqueiros apply globally, then upper mantle Tp is closer to 1485 ± 59°C. Averaging this global estimate with that recovered at Siqueiros yields TpMORB = 1458 ± 78°C, which is used to calculate plume excess temperatures, Te. The estimate for TpMORB defines the convective mantle geotherm, and is consistent with estimates from sea floor bathymetry and heat flow (Stein and Stein, 1992), and

  5. Past, Present, and Future Production of Bio-oil

    Energy Technology Data Exchange (ETDEWEB)

    Steele, Philip; Yu, Fei; Gajjela, Sanjeev

    2009-04-01

    Bio-oil is a liquid product produced by fast pyrol-ysis of biomass. The fast pyrolysis is performed by heating the biomass rapidly (2 sec) at temperatures ranging from 350 to 650 oC. The vapors produced by this rapid heating are then condensed to produce a dark brown water-based emulsion composed of frag-ments of the original hemicellulose, cellulose and lignin molecules contained in the biomass. Yields range from 60 to 75% based on the feedstock type and the pyrolysis reactor employed. The bio-oil pro-duced by this process has a number of negative prop-erties that are produced mainly by the high oxygen content (40 to 50%) contributed by that contained in water (25 to 30% of total mass) and oxygenated compounds. Each bio-oil contains hundreds of chemi-cal compounds. The chemical composition of bio-oil renders it a very recalcitrant chemical compound. To date, the difficulties in utilizing bio-oil have limited its commercial development to the production of liq-uid smoke as food flavoring. Practitioners have at-tempted to utilize raw bio-oil as a fuel; they have also applied many techniques to upgrade bio-oil to a fuel. Attempts to utilize raw bio-oil as a combustion engine fuel have resulted in engine or turbine dam-age; however, Stirling engines have been shown to successfully combust raw bio-oil without damage. Utilization of raw bio-oil as a boiler fuel has met with more success and an ASTM standard has recently been released describing bio-oil characteristics in relation to assigned fuel grades. However, commercialization has been slow to follow and no reports of distribution of these bio-oil boiler fuels have been reported. Co-feeding raw bio-oil with coal has been successfully performed but no current power generation facilities are following this practice. Upgrading of bio-oils to hydrocarbons via hydroprocessing is being performed by several organizations. Currently, limited catalyst life is the obstacle to commercialization of this tech-nology. Researchers

  6. Refrigerated water dispersion at the São Sebastião Channel

    Directory of Open Access Journals (Sweden)

    Jacyra Soares

    1999-01-01

    Full Text Available This study examines numericaIly the fate of cooled ocean water discharged into the coastal oceano The ocean water wiIl eventuaIly be used to warm up petroleum liquid gas during transference ftom ship tanks to land tanks, being cooled during the processo The reftigerated water wiIl then be released verticaIly through a single port located at 2 meters below the surface in 15 m of water. The proposed operations wiIl take place at the São Sebastião Channellocated between the continent and the São Sebastião Island, at about 23º48'S, 045º22'W. Estimated mean temperature differences between the eflluent and the recipient sea water wiIl be at most 3ºC. The problem is treated by analogy to an upside-down (buoyant thermal discharge using established initial mixing models developed by the US Environmental Protection Agency. During summer, when ambient stratification is high, the eflluent plume is evanescent: it reaches the bottom with a temperature greater than the ambient, bounces back towards the surface and reaches equilibrium 10m below the surface. During winter, on the other hand, the plume is bottom confined: it reaches the bottom with a temperature slightly lower than the ambient, remaining at that level. Model results also show that for any ambient ocean conditions the mixing time scale is of order of minutes and the final plume concentration obtained by mixing is smaIler than 10%.Este estudo examina numericamente a descarga de água reftigerada em águas oceânicas costeiras. A água do mar será utilizada para aquecimento do gás liqüefeito de petróleo durante sua transferência dos tanques do navio para o continente, sendo resftiada durante esse processo. A água reftigerada será liberada, através de um único duto localizado a 2 metros abaixo da superficie, em um local cuja profundidade é de 15 metros. Essa operação será realizada no Canal de São Sebastião, localizado entre o continente e a ilha de São Sebastião, em

  7. Some of the properties of plutonium and the aluminium-plutonium alloy; Quelques proprietes du plutonium et de l'alliage aluminium-plutonium

    Energy Technology Data Exchange (ETDEWEB)

    Abramson, R; Boucher, R; Fabre, R; Monti, H [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1959-07-01

    1- Study of the physical properties of plutonium. 1) Study of the allotropy of plutonium. a) Thermal analysis: the apparatus used and the measurement technique are briefly described. The transition point temperatures and the corresponding heats of transformation have been determined. Finally, the results of the particular study of certain transition points are given. b) Dilatometry. The dilatometric analysis of the phase changes of plutonium has been carried out by means of the Chevenard dilatometer with photographic recording. The testing conditions (heating and cooling speeds, isotherm plateaux) have been varied in order to determine accurately the characteristics of each transition, particularly the {delta} {yields} {gamma} transition on cooling. 2) Micrography of plutonium. For the accurate preparation of metallographic samples the electrolytic polishing must be rapid, which implies a mechanical polishing of excellent quality. Information is given on new attacking reagents which show the structure of the metal very clearly. 2- Study of aluminium-plutonium alloys. Comparative study of Al-Pu and Al-U alloys rich in aluminium. a) Thermal analysis. The liquids and fusion temperatures of the eutectic Al-XAl{sub 4}, have been accurately determined. From the measurement of the heats of fusion the exact composition of the eutectic alloy has been determined. b) Thermal treatments. The eutectic coalescence kinetics have been studied by a micrographic method and by following the evolution of hardness. The results obtained show that the phenomenon is more rapid in Al-Pu alloys than in Al-U alloys. c) Micrographic study of the transition XAl{sub 3} {yields} XAl{sub 4}. The peritectic reaction XAl{sub 3} + liq. {yields} XAl{sub 4} has been suppressed by quenching. The transformation of the XAl{sub 3} phase to the solid phase has been studied as well as the effect of small additions of silicon on the kinetics of this reaction. (author) [French] 1- Etude des proprietes

  8. Caracterización florística e hidrológica de turberas de la Isla Grande de Chiloé, Chile Floristic and hydrological characterization of Chiloé Island peatlands, Chile

    Directory of Open Access Journals (Sweden)

    MARÍA F DÍAZ

    2008-12-01

    Full Text Available Las turberas son ecosistemas reconocidos mundialmente por actuar como grandes reservorios de agua dulce, afectando el clima y la hidrología local; por ser sumideros de carbono; por albergar especies únicas, contribuyendo así a la biodiversidad; y porque significan un recurso económico para la sociedad. La vegetación de las turberas es dominada por plantas que crecen a ras de suelo formando densas poblaciones, en especial musgos del género Sphagnum o plantas vasculares de la familia de las Ciperáceas o Juncáceas. Presentan altos niveles freáticos y una profunda capa de materia orgánica (turba bajo la capa viva de plantas. La tala y quema de bosques en sitios con drenaje pobre han generado un tipo de ecosistema similar a las turberas donde crece principalmente el musgo Sphagnum (turberas antropogénicas o "pomponales", pero donde la acumulación de turba aún es muy baja. Mientras las turberas naturales son utilizadas para la extracción de turba, en las turberas antropogénicas se cosecha el musgo vivo que se encuentra en la superficie. Las consecuencias ecológicas después de ambas actividades extractivas son distintas. El objetivo de este trabajo es hacer una comparación de la composición florística y de los niveles freáticos entre turberas naturales y antropogénicas. Fueron estudiadas turberas naturales y antropogénicas con y sin extracción de Sphagnum. Se registraron 74 taxa (ocho liqúenes, 19 briófitas y 47 de plantas vasculares. Las diferencias en composición florística nos permiten distinguir entre turberas naturales y antropogénicas. Los niveles freáticos también difieren entre sitios, siendo menos superficiales en turberas naturales y antropogénicas sin extracción, que en turberas antropogénicas con extracción de Sphagnum. Debido a la inexistencia de nieves eternas en la Isla de Chiloé, la alteración hidrológica de estos reservorios de agua dulce proveniente de las lluvias puede traer graves consecuencias

  9. Vitamina C em "cabeludinha" (Myrciaria glomerata Berg Vitamin C content in fruits of Myrciaria glomerata

    Directory of Open Access Journals (Sweden)

    J. Soubihe Sobrinho

    1955-01-01

    Full Text Available Êste trabalho faz parte do estudo do melhoramento genético das mirtáceas frutíferas, que vem sendo realizado pela Seção de Frutas Tropicais do Instituto Agronômiso e pela Seção de Genética da Escola Superior de Agricultura "Luiz de Queiroz", em Piracicaba. Colaboraram na parte analítica a Seção Técnica "Química Agrícola" e a Cadeira de Química, da "Luiz de Queiroz''. A extração de vitamina C foi feita num liqüidificador durante dois minutos, utilizando-se o ácido oxálico a quatro por mil como solução protetora. A determinação se fez no "EEL. portable colorimeter". A determinação do conteúdo de vitamina C no fruto integral de plantas expostas ao pleno sol revelou o seguinte : planta 1, 2147 mg/100 g ; planta 2, 2389 mg/100 g ; planta 3, 2322 mg/100 g de fruto (vêr figura 1-A. Os teores de ácido ascórbico encontrados nos graus de maturação foram : fruto verde, 2716 mg/100 g ; fruto de vez, 2391 mg/100 g; fruto maduro, 2417 mg/100 g. O fruto verde tem o teor mais alto, enquanto o de vez e o maduro não diferem entre si. Também foram analisadas as diversas partes do fruto maduro, encontrando-se na casca 2482 mg/100 g e na polpa 3018 mg/100 g. Isto quer dizer que na "cabeludinha" a riqueza em ácido ascórbico aumenta da periferia para o centro. Tal fato é de suma importância, uma vez que só é aproveitada a polpa, portanto, a parte mais rica do fruto. Determinou-se também o conteúdo de vitamina C no fruto integral e maduro, de plantas sombreadas, encontrando-se na planta 1, 717, 28 mg/100 g; na planta 2, 838,66 mg/100 g ; na planta 3, 560,83 mg/100 g ; na planta 4, 713, 28 mg/100 g. Êstes resultados indicam, provavelmente, que as plantas localizadas à sombra são bem mais pobres em ácido ascórbico que aquelas crescendo ao sol; indicam ainda, que entre as plantas sombreadas há diferenças significativas, talvez de origem genética. As figuras dos gráficos 3 e 4 mostram, respectivamente, que a "cabeludinha