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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. Molecular Engineering of Liquid Crystal Polymers by Living Polymerization. 14. Synthesis and Characterization of Binary Copolymers of Omega-4-Cyano-4’-Biphenyl)oxyAlkyl Vinyl Ethers Containing Undecanyl and Hexyl Pentyl and Propyl, and Undecanyl and Propyl Pairs of Alkyl Groups

    Science.gov (United States)

    1991-04-10

    Noel, C. Polym. Bull. 1986, 15, 341; Lacoudre, N.; Le Borgue , A.; Spassky, N.; Vairon, J. P.; Le Barny, P.; Dubois, . C.; Esselin, S.; Friedrich, C...Noel, C. Mol. Cryst. Liq. Cryst. 1988, 155, 113; Spassky, N.; Lacoudre, N.; Le Borgue , A.; Vairon J. P.; Jun, C. L.; Friedrich, C.; Noel, C. Makromol...Chem. Macromol. Symp. 1989, 24, 271; Legrand, C.; Le Borgue , A.; Bunel, C.; Lacoudre, N.; Le Barny, P.; Spassky, N.;Vairon, 3. P. Makromol. Chem

  3. 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

    . To understand how the derepression of the Stellate elements gives rise to these abnormalities, we have expressed the protein encoded by the Stellate sequences in bacteria and produced an antibody against the fusion protein. Immunostaining of crystal- testes has clearly shown that the Stellate protein is a major...

  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. 平面金属螯合物为桥基的类梯形盘状液晶高分子

    Institute of Scientific and Technical Information of China (English)

    谢萍; 申仲荣; 刘宇彪; 范震; 张榕本

    2000-01-01

    [1] Adam D., Closs F., Funhoff D., Haarer D., Ringsdorf H., Schuhmacher P., Siememsmeyer K.,Phys. Rev. Lett., 1993, 70:457[2] Adam D., Schuhmacher P., Simmerer J., Hussling L., Siememsmeyer K., Etzbach K. H.,Ringsdorf H., Haarer D., Nature, 1994, 371:141[3] Giroud-Godquin A. M.,and Billard J.,Mol. Cryst. liq. Cryst., 1981,66:147[4] Kohne B. and Praefcke K., Angew. Chem., 1984, 96:70[5] Liu Yb., Liu Cq., Cui L., Fan Z., Xie P., and Zhang Rb., Liquid Crystals, 2000,27:5.

  6. Solid State Raman Materials Characterization and Raman Shifting Of 1.3 Micron Laser Radiation

    Science.gov (United States)

    2000-06-01

    Cryst. Liq. Cryst. 123 (1985) 295. 5.7. Ichiro Hatta, Thermochimica Acta 304/305 (1997) 27. 5.8. K. Ema, H. Yao, Thermochimica Acta 304/305 (1997) 157...5.9. Yasuo Saruyama, Thermochimica Acta 304/305 (1997) 171. 5.10. M. Castro, J. A. Puertolas, Thermochimica Acta 304/305 (1997) 291. 5.11. D. Finotello...S. Qian, G. S. Iannacchione, Thermochimica Acta 304/305 (1997) 303. 5.12. A.A. Minakov, Yu.V. Bugoslavsky, C. Schick, Thermochimica Acta 317 (1998

  7. 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

    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. In this w...

  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

    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. In this w...

  9. 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

    2010-04-01

    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.

  10. Experimental and theoretical results on electron emission in collisions between He targets and dressed Liq+ (q = 1, 2) projectiles

    Science.gov (United States)

    Fregenal, D.; Monti, J. M.; Fiol, J.; Fainstein, P. D.; Rivarola, R. D.; Bernardi, G.; Suárez, S.

    2014-08-01

    We investigate experimentally and theoretically the electron emission in collisions between He atoms and L{{i}^{q+}} (q = 1, 2) projectiles at intermediate to high incident energies. We report on measured absolute values of double-differential cross-sections, as a function of the emitted electron energy and angle, at a collision energy of 440 keV u-1. The different contributions from target ionization, projectile ionization, and simultaneous target-projectile ionization are calculated with the quantum-mechanical continuum distorted wave and continuum distorted wave-eikonal initial state models, and with classical trajectory Monte Carlo simulations. There is an overall good agreement of the calculations with the experimental data for electron emission cross-sections.

  11. 用表面技术研究壳聚糖及其衍生物的胆甾液晶织构

    Institute of Scientific and Technical Information of China (English)

    董炎明; 吴玉松; 袁清; 阮永红; 王勉

    2000-01-01

    [1] Thomas, E. L. and Wood, B. A., Faraday Discuss. Chem. Soc., 1985, 79:229[2] Wood, B. A. and Thomas, E. L., Nature, 1986, 324:665[3] Hudson, S. D., Thomas, E. L. And Lenz, R. W., Mol. Cryst. Liq. Cryst., 1987, 153:63[4] Chen, S., Cai, L., Wu, Y., Jin Y., Zhang, S., Qing Z., Song, W. And Qian R., Kexue Tongbao, 1992, (14): 1284[5] Ford, J. R., Bassett, D. C. and Mitchell, R., Mol. Cryst. Liq. Cryst., 1990, 180B:233[6] Chen, S., Jin, Y., Hu, S. and Xu, M., Polym. Comms., 1987, (28): 209[7] Windle, A. H., Dong, Y., Lemmon, T. J. and Spontak, R. J., in Frontiers of Macromolecular Science, Ed. by Saeguas, T., Higashimura T., Abe, A., IUPAC, Blackwell, London, 1989:343[8] Tsutsui, T. and Tauaka, T., J. Polym. Sci., Polym. Lett. Ed., 1977, 15:475[9] Nishio, Y.,Yamane, T. and Takahashi, T., J. Polym.Sci., Polym. Phys. Ed., 1985, 23:1043[10] Nishio, Y., Yamane, T. and Takahashi, T., J. Polym. Sci., Polym. Phys. Ed., 1985,23:1043[11]Huang, Y., Loos, J., Yang, Y. Q. and Petermann, T., J. Polym. Sci., Polym. Phys. Ed., 1998, 36:439[12]Huang, Y., Yang, Y. Q. and Petermann, T., Polymer, 1998, 39(22):5031[13]Olley, R. H., and Bassett, D. C., Polymer, 1988, 27:344[14]Binnig, G., Quate, C. F. and Gerber, Ch., Phys. Rev. Leu., 1986, 56:930

  12. Plan de manejo ambiental del laboratorio de ingeniería química (liq) de la universidad nacional de colombia, sede bogotá

    OpenAIRE

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

    2010-01-01

    Con el fin de fortalecer el desempeño ambiental del Laboratorio de Ingeniería Química (LIQ), se formuló un Plan de Manejo Ambiental con base en los principios establecidos por la norma ISO 14001. Como primer paso, se propuso la política ambiental; posteriormente, después de una revisión inicial, se identificaron los impactos ambientales significativos relacionados con las actividades que se desarrollan en el laboratorio, los cuales corresponden a acumulación de residuos químicos peligrosos, c...

  13. Aspectos biológicos da neurocisticercose: alterações do liqüido cefalorraquidiano

    Directory of Open Access Journals (Sweden)

    A. Spina-França

    1962-03-01

    sempre acompanha a evolução clínica. Quando esta é satisfatória, costumam desaparecer progressivamente as alterações do LCR; se estas se mantiverem por longo tempo, o prognóstico é mais reservado, especialmente quando aparece hipoglicorraquia. Em alguns casos, após intervenções cirúrgicas há rápida remissão das alterações do LCR; provavelmente isto ocorre nos casos em que a infestação do encéfalo era discreta, ou mesmo única. Quando ocorre rotura da vesícula parasitária durante a intervenção cirúrgica, o liqüido contido em seu interior acarreta exacerbação transitória das alterações do LCR. 5 - As alterações do proteinograma do LCR na neurocisticercose são do tipo verificado em processos inflamatórios subcrônicos e crônicos do SNC e de seus envoltórios, caracterizando-se especialmente por aumento de γ-globulina. Êste aumento está relacionado à intensidade da reação imunopatológica e provavelmente é devido à produção local dessa globulina, que parece ser a carreadora dos anticorpos específicos. O aumento de γ-globulina é precoce, podendo preceder a formação dos anticorpos específicos e costuma regredir lentamente nos casos de evolução satisfatória. Quando a evolução é má, o teor dessa globulina costuma aumentar progressivamente.

  14. Experimental and theoretical results on electron emission in collisions between He targets and dressed Li$^{q+}$ (q=1,2) projectiles

    CERN Document Server

    Fregenal, D; Fiol, J; Fainstein, P D; Rivarola, R D; Bernardi, G; Suárez, S

    2014-01-01

    We investigate experimentally and theoretically the electron emission in collisions between He atoms and Li$^{q+}$ (q=1,2) projectiles at intermediate-high incident energies. We report on measured absolute values of double differential cross-sections, as a function of the emitted electron energy and angle, at a collision energy of 440~keV/u. The different contributions from target-ionisation, projectile-ionisation, and simultaneous target-projectile ionisation are calculated with the quantum-mechanical Continuum Distorted Wave and Continuum Distorted Wave -- Eikonal Initial State models, and with Classical Trajectory Monte Carlo simulations. There is an overall good agreement of the calculations with the experimental data for electron emission cross-sections.

  15. 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.

  16. Comparison between two commercial immunoassays: Dr. Fooke ALLERG-O-LIQ versus Phadia ImmunoCA(R) System in detecting allergen-specific IgE and total IgE values

    Institute of Scientific and Technical Information of China (English)

    Baoqing Sun; Mahler Michael; Mei Jiang; Jing Li; Nanshan Zhong

    2008-01-01

    Objective: Beside patient's history and skin prick testing(SPT) the detection of specific IgE(slgE) represents an important tool of allergy diagnostics. In recent years different technologies for the detection of sIgE have been developed. The objective of this study is the comparison of the ALLERG-O-LIQ with the ImmunoCAP System using seven inhalant and four food allergens. Methods: Sera from patients were collected and tested for sIgE to inhalant(d1, d2, d5, i6, el, e5 and m3) and food allergens(fl, 12, f24, t24) by ALLERG-O-LIQ(Dr. Fooke Laboratorien GmbH) and by ImmunoCAP System(Phadia). Further, samples were also tested for total IgE in both systems. Results: Prevalence of positive test results varied between 0/20(124) and 11/20(e5) for ALLERG-O-LIQ and between 3/18(f23) and 11/20(d1/d5) for ImmunoCAP . The qualitative agreement between both methods was found between 75%(f24) and 100%(d2) depending on the allergen. Overall qualitative agreement for inhalant(n = 140), food(n = 78) and all allergens(n = 218) tested was 92.1%(kappa = 0.84), 83.3%(kappa = 0.58), 89.0%(kappa = 0.77), respectively. Sensitivity, specificity, positive predictive value (PPV), negative predictive value(NPV) and diagnostic efficiency(DE) were found at 88.2%, 95.8%, 95.2%, 89.6%, 92.1%(inhalant allergens), 62.5%, 92.6%, 78.9%, 84.7%, 83.3%(food allergens) and 81.5%, 94.4%, 91.5%, 87.5%, 89.0%(all allergens). Conclusion: Good to excellent qualitative agreement between ALLERG-O-LIQ and ImmunoCAP for the detection of specific and total IgE could be observed. The degree of agreement depended on the allergen and was higher in the group of inhalant allergens. The ALLERG-O-LIQ System represents a reliable test for the detection of specific and total IgE.

  17. Orientational order parameter studies in two symmetric dimeric liquid crystals - an optical study

    Science.gov (United States)

    Pardhasaradhi, P.; Datta Prasad, P. V.; Madhavi Latha, D.; Pisipati, V. G. K. M.; Padmaja Rani, G.

    2012-12-01

    The optical technique developed by [W. Kuczynski, B. Zywucki, and J. Malecki, Determination of orientational order parameter in various liquid-crystalline phases, Mol. Cryst. Liq. Cryst. 381 (2002), pp. 1-19; B.J. Zywucki and W. Kuczynski, IEEE transactions on optical phenomena - The orientational order in nematic liquid crystals from birefringence measurements, Dielectr. Electr. Insul. 8 (2001), pp. 512-515] is fabricated and used to determine the orientational order parameter in two dimeric liquid crystalline compounds nematic and SmA phases of α,ω-bis(4-alkylanilinebenzylidene-4‧-oxy)alkane (m.OnO.m) homologous series. The compounds studied are 5.O8O.5 and 5.O10O.5 which exhibit nematic and SmA, and nematic phases, respectively. The orientational order parameter in both the phases of nematic and SmA phases of the compound one and the nematic phase of the compound two are obtained using the principle of Newton's rings which gives directly the birefringence, δn of the liquid crystal dimer. The merits of the technique used are presented over the conventional techniques for the determination of orientational order parameter. The results for the two compounds are compared with those values estimated from n e, n o and density using the two internal field models due to Vuks and Neugebauer applicable to nematic phase.

  18. Acoustic waves in compressible planar layered smectic liquid crystals

    Science.gov (United States)

    Walker, A. J.; Stewart, I. W.

    2010-08-01

    A dynamic theory for compressible smectic C (SmC) liquid crystals is postulated following previous work by Leslie et al (1991 Mol. Cryst. Liq. Cryst. 198 443-54), Nakagawa (1996 J. Phys. Soc. Japan 65 100-6 2004 J. Non-Newtonian Fluid Mech. 119 123-9) and de Gennes and Prost (1993 The Physics of Liquid Crystals 2nd edn (Oxford: Oxford University Press)). This theory is then implemented with a constructed bulk elastic energy and asymmetric stress tensor to describe a system of planar layered SmC liquid crystals undergoing various modes of undulation. We show that previous work on smectic A (SmA) liquid crystals by de Gennes and Prost (1993 The Physics of Liquid Crystals 2nd edn (Oxford: Oxford University Press)) can be expanded for SmC and consolidated. Novel and confirming estimates for SmC material parameter values are produced by considering the dependence of the system on these parameters.

  19. 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.

  20. A second polymorph of (2E-1-(4-fluorophenyl-3-(3,4,5-trimethoxyphenylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    Jerry P. Jasinski

    2009-08-01

    Full Text Available The crystal structure of the title compound, C18H17FO4, reported here is a polymorph of the structure first reported by Patil et al. [Mol. Cryst. Liq. Cryst. Sci. Technol. Sect. A (2007, 461, 123–130]. It is a chalcone analog and consists of substituted phenyl rings bonded at the opposite ends of a propenone group, the biologically active region. The dihedral angle between the mean planes of the aromatic rings within the 4-fluorophenyl and trimethoxyphenyl groups is 28.7 (1° compared to 20.8 (6° in the published structure. The angles between the mean plane of the prop-2-ene-1-one group and the mean plane of aromatic rings within the 4-fluorophenyl and trimethoxyphenyl groups are 30.3 (4 and 7.4 (7°, respectively, in contast to 10.7 (3 and 12.36° for the polymorph. While the two 3-methoxy groups are in the plane of the trimethoxy-substituted ring, the 4-methoxy group is in a synclinical [−sc = −78.1 (2°] or anticlinical [+ac = 104.0 (4°] position, compared to a +sc [53.0 (4°] or −ac [−132.4 (7°] position. While no classical hydrogen bonds are present, weak intermolecular C—H...π-ring interactions are observed which contribute to the stability of the crystal packing. The two polymorphs crystallize in the same space group, P21/c, but have different cell parameters for the a, b and c axes and the β angle. A comparison of the molecular geometries of both polymorphs to a geometry optimized density functional theory (DFT calculation at the B3-LYP/6–311+G(d,p level for each structure provides additional support to these observations.

  1. μ-Oxalato-bis[bis(triphenylphosphinecopper(I] dichloromethane disolvate. Corrigendum

    Directory of Open Access Journals (Sweden)

    Andrew D. Royappa

    2014-10-01

    Full Text Available An erroneous claim in the paper by Royappa et al. [Acta Cryst. (2013, E69, m126] is corrected and a reference added for a previously published report of a closely related structure.

  2. A neo-clerodane diterpene from Teucrium tomentosum. Corrigendum

    Directory of Open Access Journals (Sweden)

    S. Soundarya Devi

    2009-06-01

    Full Text Available The chemical name of the title compound in the paper by Devi, Malathi, Rajan, Aravind, Krishnakumari & Ravikumar [Acta Cryst. (2004, E60, o117–o119] is corrected and the structural diagram is updated.

  3. A neo-clerodane diterpene from Teucrium tomentosum. Corrigendum

    Science.gov (United States)

    Devi, S. Soundarya; Malathi, R.; Rajan, S. S.; Aravind, S.; Krishnakumari, G. N.; Ravikumar, K.

    2009-01-01

    The chemical name of the title compound in the paper by Devi, Malathi, Rajan, Aravind, Krishnakumari & Ravikumar [Acta Cryst. (2004), E60, o117–o119] is corrected and the structural diagram is updated. PMID:21582975

  4. Abstracts: Sagmore 9 Conference on Charge, Spin and Momentum Densities Held in Luso-Bussaco, Portugal on 26 June-2 July 1988

    Science.gov (United States)

    1988-07-01

    counter, for two different orientations (a vertical , then b vertical ) of the same single crystal, at 21 under an applied field of 5 tels.. The whole set...Cnyst.33z.1777 (I)Shbs.Eikhawa A Salto (1985) Acts Cryst. C41.1l C)1Ikkhemjehh.Sl to.ia~ts A luota(SU7 Act& Cryst. 343. 83. 28 P2.4 L. BRAMMER and K.D

  5. The Exploitation of Versatile Building Blocks for the Self-Assembly of Novel Molecular Magnets

    Science.gov (United States)

    Pilkington, M.; Gross, M.; Franz, P.; Biner, M.; Decurtins, S.; Stoeckli-Evans, H.; Neels, A.

    2001-07-01

    Using molecular building blocks to self-assemble lattices supporting long-range magnetic order is currently an active area of solid-state chemistry. Consequently, it is the realm of supramolecular chemistry that synthetic chemists are turning to in order to develop techniques for the synthesis of structurally well-defined supramolecular materials. In recent years we have investigated the versatility and usefulness of two classes of molecular building blocks, namely, tris-oxalato transition-metal (M. Pilkington and S. Decurtins, in "Magnetoscience-From Molecules to Materials," Wiley-VCH, 2000), and octacyanometalate complexes (Pilkington and Decurtins, Chimia 54, 593 (2001)), for applications in the field of molecule-based magnets. Anionic, tris-chelated oxalato building blocks are able to build up two-dimensional honeycomb-layered structural motifs as well as three-dimensional decagon frameworks. The discrimination between the crystallization of the two- or three-dimensional structures relies on the choice of the templating counterions (Decurtins, Chimia 52, 539 (1998); Decurtins et al. Mol. Cryst. Liq. Cryst. 273, 167 (1995); New J. Chem. 117 (1998)). These structural types display a range of ferro, ferri, and antiferromagnetic properties (Pilkington and Decurtins, in "Magnetoscience-From Molecules to Materials"). Octacyanometalate building blocks self-assemble to afford two new classes of cyano-bridged compounds namely, molecular clusters and extended three dimensional networks (J. Larionova et al., Angew. Chem. Int. Ed. 39, 1605 (2000); Pilkington et al., in preparation). The molecular cluster with a MnII9MoV6 core has the highest ground state spin value, S=51/2, reported to-date (Larionova et al., Angew. Chem. Int. Ed. 39, 1605 (2000)). In the high-temperature regime, the magnetic properties are characterized by ferromagnetic intracluster coupling. In the magnetic range below 44 K, the magnetic cluster signature is lost as possibly a bulk behavior starts to

  6. Crystal structure and Hirshfeld surface analysis of 1-carboxy-2-(3,4-dihydroxyphenyl)ethan-1-aminium chloride 2-ammonio-3-(3,4-dihydroxyphenyl)propanoate: a new polymorph of l-dopa HCl and isotypic with its bromide counterpart

    OpenAIRE

    Perumal Kathiravan; Thangavelu Balakrishnan; Perumal Venkatesan; Kandasamy Ramamurthi; María Judith Percino; Subbiah Thamotharan

    2016-01-01

    The title molecular salt, C9H12NO4+·Cl−·C9H11NO4, is isotypic with that of the bromide counterpart [Kathiravan et al. (2016). Acta Cryst. E72, 1544–1548]. The title salt is a second monoclinic polymorph of the l-dopa HCl structure reported earlier in the monoclinic space group P21 [Jandacek & Earle (1971). Acta Cryst. B27, 841–845; Mostad & Rømming (1974). Acta Chemica Scand. B28, 1161–1168]. In the title compound, monoclinic space group I2, one of the dopa molecules has a positive charge wit...

  7. Crystal structure and Hirshfeld surface analysis of 1-carb­oxy-2-(3,4-di­hydroxy­phen­yl)ethan-1-aminium chloride 2-ammonio-3-(3,4-di­hydroxy­phen­yl)propano­ate: a new polymorph of l-dopa HCl and isotypic with its bromide counterpart

    OpenAIRE

    Kathiravan, Perumal; Balakrishnan, Thangavelu; Venkatesan, Perumal; Ramamurthi, Kandasamy; Percino, María Judith; Thamotharan, Subbiah

    2016-01-01

    The title mol­ecular salt, C9H12NO4 +·Cl−·C9H11NO4, is isotypic with that of the bromide counterpart [Kathiravan et al. (2016 ▸). Acta Cryst. E72, 1544–1548]. The title salt is a second monoclinic polymorph of the l-dopa HCl structure reported earlier in the monoclinic space group P21 [Jandacek & Earle (1971 ▸). Acta Cryst. B27, 841–845; Mostad & Rømming (1974 ▸). Acta Chemica Scand. B28, 1161–1168]. In the title compound, monoclinic space group I2, one of the dopa mol­ecules has a positive c...

  8. Hardness and incipient plasticity in silicate glasses

    DEFF Research Database (Denmark)

    Kjeldsen, Jonas; Smedskjær, Morten Mattrup; Mauro, John C.;

    2014-01-01

    The scaling of Vickers hardness (Hv) in oxide glasses with varying network modifier/modifier ratio is manifested as either a positive or negative deviation from linearity with a maximum deviation at the ratio of about 1:1. In an earlier study [J. Kjeldsen et al., J. Non-Cryst. Solids 369,61(2013)......The scaling of Vickers hardness (Hv) in oxide glasses with varying network modifier/modifier ratio is manifested as either a positive or negative deviation from linearity with a maximum deviation at the ratio of about 1:1. In an earlier study [J. Kjeldsen et al., J. Non-Cryst. Solids 369...

  9. Proceedings of Symposium F on New Aspects on the Growth, Characterization and Applications of CdTe and Related Cd Rich Alloys of the 1992 E-MRS Spring Conference held in Strasbourg, France on June 2 - 5, 1992

    Science.gov (United States)

    1992-01-01

    diffusion-induced changes in the low energy part of the bound-exciton The authors are indebted to M. Wienecke and C. Albers from the Humboldt-Universitit...Neubert, T. Boeck, P. M6ck, L. Parthier, K. Jacobs and E. Kropp, J. Cryst. Growth, 118 (1992)204. 11 C. Albers and M. Wienecke, Cryst. Res. Technol., 22...process. In fact, the space charge field is anni - levels induces a periodic distribution of free electrons hilated and free carriers can diffuse again

  10. CREDO: a structural interactomics database for drug discovery.

    Science.gov (United States)

    Schreyer, Adrian M; Blundell, Tom L

    2013-01-01

    CREDO is a unique relational database storing all pairwise atomic interactions of inter- as well as intra-molecular contacts between small molecules and macromolecules found in experimentally determined structures from the Protein Data Bank. These interactions are integrated with further chemical and biological data. The database implements useful data structures and algorithms such as cheminformatics routines to create a comprehensive analysis platform for drug discovery. The database can be accessed through a web-based interface, downloads of data sets and web services at http://www-cryst.bioc.cam.ac.uk/credo. Database URL: http://www-cryst.bioc.cam.ac.uk/credo.

  11. Practical approach for production of bacteria-based agent-contained light weight aggregates to make concrete self-healing

    NARCIS (Netherlands)

    Mors, R.M.; Jonkers, H.M.

    2013-01-01

    A functional experimental concrete system has been developed in our lab, in which a two component bacteria-based healing agent contained in a protective reservoir is included in the concrete mixture. Incorporated bacteria have the potential to produce copious amounts of calcium carbonate based cryst

  12. 75 FR 6424 - Self-Regulatory Organizations; NYSE Amex LLC; Notice of Filing and Immediate Effectiveness of...

    Science.gov (United States)

    2010-02-09

    .... 166 ANF Abercrombie & 187 MMM 3M Co. Fitch Co. 172 APC Anadarko Petroleum 140 MU Micron Technology... Occidental Petroleum Corp. 190 BCRX BioCryst 158 PARD Poniard Pharmaceuticals Pharmaceuticals Inc. Inc. 218... principles of trade, remove impediments to and perfect the mechanisms of a free and open market and...

  13. Vacancy ordering and superstructure formation in dry and hydrated strontium tantalate perovskites: A TEM perspective

    DEFF Research Database (Denmark)

    Ashok, Anuradha M.; Haavik, Camilla; Norby, Poul

    2014-01-01

    Crystal structures of Sr4(Sr2Ta2)O11 and Sr4(Sr1.92Ta2.08)O11.12, synthesized by solid state reaction technique in dry and hydrated state have been studied mainly using Transmission Electron Microscopy. Due to the lesser ability of X-rays to probe details in oxygen sublattice, the change in cryst...

  14. Neutron and X-ray diffraction study of ferrite nanocrystals obtained by microwave-assisted growth. A structural comparison with the thermal synthetic route. Corrigendum

    Science.gov (United States)

    Solano, Eduardo; Frontera, Carlos; Puente Orench, Inés; Puig, Teresa; Obradors, Xavier; Ricart, Susagna; Ros, Josep

    2014-01-01

    In the paper by Solano et al. ▶ [J. Appl. Cryst. (2014), 47, 414–420], Inés Puente Orench is missing from the list of authors. The complete list of authors should be Eduardo Solano, Carlos Frontera, Inés Puente Orench, Teresa Puig, Xavier Obradors, Susagna Ricart and Josep Ros. PMID:25242916

  15. European Symposium on X-Ray Topography and High Resolution Diffraction (2nd) Held in Berlin, Germany on 5-7 September 1994. Programme and Abstracts

    Science.gov (United States)

    1994-09-07

    N L Andrew Philips Research Laboratories, Cross-Oak Lane, Redhill, RH! 5HA, U.K. A Saced6n, E Calleja Dept. Ingenieria Electr6nica, E. T. S. I. T.. U...Matematica e Fisica - 62032 CAMERINO (Italy) * I lnst. Cryst. Russian Acad. of Science, MOSCOW (Rlussia) Si/Ge superlattices (SL) have recently

  16. A test on the statistics of derived intensities

    NARCIS (Netherlands)

    de With, G.; Feil, D.

    1976-01-01

    Variances of X-ray reflexions calculated with the procedure as proposed by McCandlish, Stout & Andrews [Acta Cryst. (1975), A31, 245-249] have been tested against variances determined in an independent way. A satisfying agreement is obtained

  17. 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...

  18. Domain Modeling: NP_001002912.3 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001002912.3 chr1 CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chr1/NP_001002912.3/NP_001002912.3_apo_256-533.pdb psi-blast 0 ...

  19. Domain Modeling: NP_001095133.1 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001095133.1 chr1 CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chr1/NP_001095133.1/NP_001095133.1_apo_7-270.pdb psi-blast 0 ...

  20. Domain Modeling: NP_001001924.1 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001001924.1 chr8 CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chr8/NP_001001924.1/NP_001001924.1_apo_2-263.pdb psi-blast 0 ...

  1. Domain Modeling: NP_001032519.1 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001032519.1 chr4 CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chr4/NP_001032519.1/NP_001032519.1_apo_251-515.pdb psi-blast 0 ...

  2. Domain Modeling: NP_001001924.1 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001001924.1 chr8 CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chr8/NP_001001924.1/NP_001001924.1_apo_729-1013.pdb psi-blast 0 ...

  3. Domain Modeling: NP_001035089.1 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001035089.1 chr6 CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chr6/NP_001035089.1/NP_001035089.1_apo_1285-1557.pdb psi-blast 0 ...

  4. Domain Modeling: NP_001078823.1 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001078823.1 chrX CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chrX/NP_001078823.1/NP_001078823.1_apo_249-522.pdb psi-blast 0 ...

  5. Domain Modeling: NP_001018001.1 [SAHG[Archive

    Lifescience Database Archive (English)

    Full Text Available NP_001018001.1 chr1 CRYSTAL STRUCTURE OF TROPOMYOSIN AT 7 ANGSTROMS RESOLUTION IN THE SPERMINE-INDUCED CRYST...AL FORM c1c1gd_ chr1/NP_001018001.1/NP_001018001.1_apo_3-274.pdb psi-blast 0 ...

  6. 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

    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...

  7. 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...

  8. Solid State Research.

    Science.gov (United States)

    2007-11-02

    Kobayashi and T. Makimoto , Jpn. J. Appl. Phys. 24, L824 (1985). 12. A. C. Jones and S. A. Rushworth, J. Cryst. Growth 106, 253 (1990). 13. W. S. Hobson, T... going to HBr at low chuck power the oxide etch rate is reduced even further. In addition, a small amount of oxygen was added in the overetch step. This

  9. 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 performan...

  10. Comment on `Magic strains in face-centered and body-centered cubic lattices'

    NARCIS (Netherlands)

    Waal, van de Benjamin W.

    1990-01-01

    The six symmetry-related so-called magic strain tensors that transform a f.c.c. lattice (or a b.c.c. lattice) into itself, which have been reported recently by Boyer [Acta Cryst. (1989), A45, FC29-FC32] are not unique: an infinite number of displacement tensors can be constructed that transform one

  11. Lithium Hydroxide Dihydrate: A New Type of Icy Material at Elevated Pressure

    Science.gov (United States)

    2011-01-01

    M. Jansen, J. Appl. Crystallogr. 32, 864 (1999). 17A. L. Speck, PLATON , a multipurpose crystallographic tool Utrecht University, Utrecht, The...Netherlands, 2001. See http://www.cryst.chem. uu.nl/ platon /. 18G. Kresse and J. Furthmuller, Comput. Mater. Sci. 6, 15 (1996). 19G. Kresse and J. Hafner, J

  12. Electrostatic Molecular Interaction from X-ray Diffraction Data. II. Test on Theoretical Pyrazine Data

    NARCIS (Netherlands)

    Feil, Dirk; Moss, Grant

    1983-01-01

    In a previous paper [Moss & Feil (1981). Acta Cryst. A37, 414-421] a method was reported to calculate the electrostatic potential and the electrostatic interaction energy from single-crystal X-ray diffraction data. The method was applied to experimental pyrazine data; however, owing to the relativel

  13. Laterally Overgrown Structures as Substrates for Lattice Mismatched Epitaxy

    Science.gov (United States)

    2002-06-03

    Chocho , Jpn. J. Appl. Phys. 36 (1997) Growing the layers standing free above the mask seems L1568.[3] T. Nishinaga, Cryst. Prop. Prep. 31 (1991) 92. to be...moto, M. Sano, K. Chocho , Jpn. J. Appl. Phys. 36 (1997) 5S1 (2000) W2.3, L1568. [38] I. Kidoguchi, A. Ishibashi, G. Sugahara, Y. Ban, Appl. Phys

  14. Optimization of control parameters of CdZnTe ACRT-Bridgman single crystal growth

    Institute of Scientific and Technical Information of China (English)

    2004-01-01

    [1]Kennedey, J. J., Amirtharaj, P. M., Boyd, P. R. Et al., Growth and characterization of Cd1-xZnxTe and Hg1-yZnyTe, J. Cryst. Growth, 1988, 86: 93-99.[2]Tanaka, A., Masa, Y., Seto, S. et al., Zinc and selenium co-doped CdTe substrates lattice matched to HgCdTe, J. Cryst. Growth, 1989, 94: 166-170.[3]Sen, S., Stanard, J. E., Developments in the bulk growth of Cd1-xZnxTe for substrates, Prog. Crystal Growth and Charact., 1994, 29: 253-273.[4]Azoulay, M., Rotter, S., Gafni, G. et al., Zinc segregation in CdZnTe grown under Cd/Zn partial pressure control, J. Cryst. Growth, 1992, 117: 276-280.[5]Lee, T. S., Lee, S. B., Kim, J. M. et al., Vertical Bridgman techniques to homogenize zinc composition of CdZnTe substrates, J. Electronic Materials, 1995, 24: 1057-1059.[6]Mühlberg, M., Rudolph, P., Genzel, C. Et al., Crystalline and chemical quality of CdTe and Cd1-xZnxTe grown by the Bridgman method in low temperature gradients, J. Cryst. Growth, 1990, 101: 275-280.[7]Cheuvart, P., El-Hanani, U., Schneider, D. et al., CdTe and CdZnTe crystal growth by horizontal Bridgman technique, J. Cryst. Growth, 1990, 101: 270-274.[8]Lu, Y. C., Shiau, J. J., Fiegelson, R. S. et al., Effect of vibrational stirring on the quality of Bridgman-grown CdTe, J. Cryst. Growth, 1990, 102: 807-813.[9]Butler, J. F., Doty, F. P., Apotovsky, B. Et al., γ-ray and X-ray detectors manufactured from Cd1-xZnxTe grown by a high-pressure Bridgman method, Mater. Sci. & Eng. B, 1993, 16: 291-295.[10]Capper, P., The role of accelerated crucible rotation in the growth of Hg1-xCdxTe and CdTe/CdZnTe, Prog. Crystal Growth and Charact., 1994, 28: 1-55.[11]Schulz-Dubois, E. O., Accelerated crucible rotation: hydrodynamics and stirring effect, J. Cryst. Growth, 1971, 12: 81-87.[12]Capper, P., Gosney, J. J. G., Jones, C. L. et al., Fluid flows in tall narrow containers by ACRT, Journal of Electronic Materials, 1986 15(6): 361-370.[13]Distanov, V. E., Kirdyashkin, A

  15. Doping silver nanoparticles in AOT lyotropic lamellarphases

    Institute of Scientific and Technical Information of China (English)

    CHEN; Xiao

    2001-01-01

    aerosol OT/water/oil system, J. Colloid Interface Sci., 1979, 70: 577-583.[15]Fontell, K., The structure of the lamellar liquid crystalline phase in serosol OT-water system, J. Colloid Interface Sci.,1973, 44: 318-329.[16]Kotlarchyk, M., Sheu, E. Y., Capel, M., Structural and dynamical transformations between neighboring dense microemulsion phases, Phys. Rev. A, 1992, 46: 928-939.[17]Antelmi, D. A., Kekicheff, P., Measurement of the compressibility modulus in a lyotropic lamellar phase stabilized by undulation forces, J. Phys. Chem. B, 1997, 101: 8169-8179.[18]Wang, W., Efrima, S., Regev, O., Directing silver nanoparticles into colloid-surfactant lyotropic lamellar systems, J. Phys.Chem. B, 1999, 103: 5613-5621.[19]Chidichimo, G., La Mesa, C., Ranieri, G. A. et al., NMR investigation of the lamellar mesophase occuring in the system aerosol OT-water, Mol. Cryst. Liq. Cryst., 1987, 150b: 221-236.[20]Callaghan, P. T., Soderman, O., Examination of the lamellar phase of aerosol OT/water using pulsed field gradient nuclear magnetic resonance, J. Phys. Chem., 1983, 87: 1737-744.

  16. 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.

  17. TRAITEMENT PHYSICO - CHIMIQUE ET BIOLOGIQ UE D’UN EFFLUENT LAITIER LIQ UIDE

    Directory of Open Access Journals (Sweden)

    N . ELOUTASSI

    2013-09-01

    Full Text Available Effluent dairy industries are among the most organic-rich food waste. The milk processing unit of the City Rabat / Salè rejects daily about 900 m3/d of liquid waste(including 7.5 m3/d of whey They are a source of dangerous pollution by its richness in microorganisms, lactose, protein, vitamins and minerals which is explained by the high values of DCO, total nitrogen, total phosphorus, fecal coliforms and fecal streptococci.This study focuses on the treatment of dairy effluent by two different methods. The first is a physicochemical treatment (coagulation, flocculation using aluminum sulphate and sodium alginate. The results show a decrease of about 30% of chemical oxygen demand, 49% of turbidity, 78% of suspended solids and 20% of the total phosphorus.While the second process is a biological treatment using Pseudomonas fluorescens and Bacillus spp. This process has shown a significant reduction of the studied parameters even better than the physico- chemical treatment, with fluctuations in efficacy between the strains tested.In conclusion, we have developed biotechnological processes, which are simple,economical and environmentally friendly for treating the discharges of the dairy industry and reduce polluting factors.

  18. 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.

  19. Symmetry elements in space groups and point groups. Addenda to two IUCr reports on the nomenclature of symmetry.

    Science.gov (United States)

    Flack, H D; Wondratschek, H; Hahn, T; Abrahams, S C

    2000-01-01

    The definition of 'symmetry element' given in the Report of the IUCr Ad-Hoc Committee on the Nomenclature of Symmetry by de Wolff et al. [Acta Cryst. (1989). A45, 494-499] is shown to contain an ambiguity in the case of space groups P6/m, P6/mmm, P6/mcc and point groups 6/m and 6/mmm. The ambiguity is removed by redefining the 'geometric element' as a labelled geometric item in which the label is related to the rotation angle of the rotation or rotoinversion symmetry operation. The complete set of different types of glide plane is shown to contain three more than the 15 that are illustrated in the 1992 Report by de Wolff et al. [Acta Cryst. (1992). A48, 727-732].

  20. 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].

  1. 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.

  2. Serial femtosecond crystallography datasets from G protein-coupled receptors.

    Science.gov (United States)

    White, Thomas A; Barty, Anton; Liu, Wei; Ishchenko, Andrii; Zhang, Haitao; Gati, Cornelius; Zatsepin, Nadia A; Basu, Shibom; Oberthür, Dominik; Metz, Markus; Beyerlein, Kenneth R; Yoon, Chun Hong; Yefanov, Oleksandr M; James, Daniel; Wang, Dingjie; Messerschmidt, Marc; Koglin, Jason E; Boutet, Sébastien; Weierstall, Uwe; Cherezov, Vadim

    2016-08-01

    We describe the deposition of four datasets consisting of X-ray diffraction images acquired using serial femtosecond crystallography experiments on microcrystals of human G protein-coupled receptors, grown and delivered in lipidic cubic phase, at the Linac Coherent Light Source. The receptors are: the human serotonin receptor 2B in complex with an agonist ergotamine, the human δ-opioid receptor in complex with a bi-functional peptide ligand DIPP-NH2, the human smoothened receptor in complex with an antagonist cyclopamine, and finally the human angiotensin II type 1 receptor in complex with the selective antagonist ZD7155. All four datasets have been deposited, with minimal processing, in an HDF5-based file format, which can be used directly for crystallographic processing with CrystFEL or other software. We have provided processing scripts and supporting files for recent versions of CrystFEL, which can be used to validate the data.

  3. 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.

  4. High Temperature Reactions of Uranium Dioxide with Various Metal Oxides

    Science.gov (United States)

    1956-02-20

    HfO2 , 0.02 weight percent of SiO,, and not more than 0.005 weight percent of any other impurity) is reported to be 2,710°± 100 C [19, 201. Lambertson...CaO, J. Chem. Soc., p. 1352, 1151. (151 H. D. Megaw, Ferroelectricity and crystal structure, II, Acta Cryst. 1, 187 (1954). [16] W. A. Lanbertson and

  5. Pharmacokinetics of Peramivir in an Adolescent Patient Receiving Continuous Venovenous Hemodiafiltration

    OpenAIRE

    Dillon, Ryan C.; Witcher, Robert; Cies, Jeffrey J.; Moore, Wayne S.; Chopra, Arun

    2017-01-01

    Critically ill patients requiring renal replacement therapy commonly experience pharmacokinetic alterations. This case report describes the pharmacokinetics of peramivir (Rapivab, BioCryst Pharmaceuticals, Inc, Durham, NC), the first US Food and Drug Administration?approved intravenous neuraminidase inhibitor for the treatment of influenza, in an adolescent patient receiving continuous renal replacement therapy (CRRT). A 49.5-kg, 17-year-old Caucasian female presented with fever, cough, and p...

  6. 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....

  7. Carbon Fiber Morphology. 2. Expanded Wide-Angle X-Ray Diffraction Studies of Carbon Fibers

    Science.gov (United States)

    1991-02-01

    X- Ray Diffraction," JPS. Polym. Phys. Ed., 16, 939 (1978). 17. Rosalind E. Franklin , "The Structure of Graphitic Carbons," Acta Cryst., 4, 253 (1951...18. Rosalind E. Franklin , "The Interpretation of Diffuse X-ray Diagrams of Carbon," Acta CrL, 3, 107 (1950). 19. K. Jain and A. S. Abhiraman...been generally mentioned much earlier by Franklin [17,18]. Jain and Abhiraman [19] demonstrated that these corrections can make significant differences

  8. Mission Support for the Communication/Navigation Outage Forecast System (C/NOFS) Satellite

    Science.gov (United States)

    2007-11-21

    applications. Acta Cryst., A52:561, 1996. [18] P. N. Guzdar, P. Satyanarayana , J. D. Huba, and S. L. Ossakow. Influence of velocity shear on Rayleigh...H. G. Mitchell, J. A. Fedder, P. Satyanarayana , S. T. Zalesak, and J. D. Huba. Nonlinear evolution of the Kelvin-Helmholtz instability in the high...1960. [52] E. E. Salpeter. Plasma density fluctuations in a magnetic field. Phys. Rev., 122:1663, 1961. [53] P. Satyanarayana , P. N. Guzdar, J. D. Huba

  9. Redetermination of tetra-kis(trimethyl-stann-yl)germane.

    Science.gov (United States)

    Bauer, Matthew; Groy, Thomas L; Kouvetakis, John

    2007-12-06

    Redetermination of the structure of the title compound, [Ge(SnMe(3))(4)] or [GeSn(4)(CH(3))(12)], previously refined from powder diffraction data only [Dinnebier, Bernatowicz, Helluy, Sebald, Wunschel, Fitch & van Smaalen et al. (2002 ▶). Acta Cryst. B58, 52-61], confirms that four bulky trimethyl-stannyl ligands surround the central Ge atom (site symmetry 1) in a tetra-hedral coordination.

  10. Triclinic polymorph of 4-[4-(4-formylphenoxybutoxy]benzaldehyde

    Directory of Open Access Journals (Sweden)

    Ivana Balić

    2013-01-01

    Full Text Available The title compound, C18H18O4, is a triclinic polymorph of the previously reported monoclinic polymorph [Han & Zhen (2005. Acta Cryst. E61, o4358–o4359]. In the crystal of the triclinic polymorph, molecules are linked by two pairs of C—H...O hydrogen bonds, forming a two-dimensional network parallel to (102, and enclosing loops with graph set motifs of R22(8 and R22(6.

  11. Chromium isotope fractionation during coprecipitation with calcium carbonate

    DEFF Research Database (Denmark)

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

    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...... et al., 2007, Water Air Soil Poll. 179, 381-390. [2] Sánchez-Pastor et al., 2011, Cryst. Growth Des. 11, 3081-3089....

  12. Redetermination of tetra­kis(trimethyl­stann­yl)germane

    Science.gov (United States)

    Bauer, Matthew; Groy, Thomas L.; Kouvetakis, John

    2008-01-01

    Redetermination of the structure of the title compound, [Ge(SnMe3)4] or [GeSn4(CH3)12], previously refined from powder diffraction data only [Dinnebier, Bernatowicz, Helluy, Sebald, Wunschel, Fitch & van Smaalen et al. (2002 ▶). Acta Cryst. B58, 52–61], confirms that four bulky trimethyl­stannyl ligands surround the central Ge atom (site symmetry 1) in a tetra­hedral coordination. PMID:21200620

  13. Redetermination of tetrakis(trimethylstannylgermane

    Directory of Open Access Journals (Sweden)

    Matthew Bauer

    2008-01-01

    Full Text Available Redetermination of the structure of the title compound, [Ge(SnMe34] or [GeSn4(CH312], previously refined from powder diffraction data only [Dinnebier, Bernatowicz, Helluy, Sebald, Wunschel, Fitch & van Smaalen et al. (2002. Acta Cryst. B58, 52–61], confirms that four bulky trimethylstannyl ligands surround the central Ge atom (site symmetry 1 in a tetrahedral coordination.

  14. Nested sampling for materials: the case of hard spheres

    OpenAIRE

    Partay, Livia B.; Bartok, Albert P.; Csanyi, Gabor

    2012-01-01

    The recently introduced nested sampling algorithm allows the direct and efficient calculation of the partition function of atomistic systems. We demonstrate its applicability to condensed phase systems with periodic boundary conditions by studying the three dimensional hard sphere model. Having obtained the partition function, we show how easy it is to calculate the compressibility and the free energy as functions of the packing fraction and local order, verifying that the transition to cryst...

  15. From deep TLS validation to ensembles of atomic models built from elemental motions. Addenda and corrigendum.

    Science.gov (United States)

    Urzhumtsev, Alexandre; Afonine, Pavel V; Van Benschoten, Andrew H; Fraser, James S; Adams, Paul D

    2016-09-01

    Researcher feedback has indicated that in Urzhumtsev et al. [(2015) Acta Cryst. D71, 1668-1683] clarification of key parts of the algorithm for interpretation of TLS matrices in terms of elemental atomic motions and corresponding ensembles of atomic models is required. Also, it has been brought to the attention of the authors that the incorrect PDB code was reported for one of test models. These issues are addressed in this article.

  16. Itraconazol, an Antifungal and a Hedgehog Pathway Inhibitor for Treatment of Prostate Cancer

    Science.gov (United States)

    2016-10-01

    containing MTT solution [3-(4,5-dimethylthiazol- 2-yl)-2,5-diphenyltetrazolium bromide] for 2 hours. Metabolically intact cells cleave tetrazolium salts... cell ith indicate 8 hours. Aft essed for ce s were l)-2,5- Metabolical uccinate- mazan cryst is the...growth and metastasis of human PCa cells representative of the advanced disease; the effect of the combination, on the growth and metastasis of human

  17. Incorporation Kinetics in Mixed Anion Compound Semiconductor Alloys

    Science.gov (United States)

    2013-01-01

    PROGRAM ELEMENT NUMBER 611102 6. AUTHORS Sd. PROJECT NUMBER Joanna M. Milhmchick, Evan M . Anderson, Chris Pearson, Wendy L. Samey, Stefan P. Svensson...Chris Pearson, Department of Computer Science, Engineering, and Physics, University of Michigan–Flint, Flint, MI 48502 Wendy L. Sarney and Stefan P...M.H. Francombe, and C.E.C. Wood , J Appl Phys 52, 7416 (1981). 27 B.W. Liang and C.W. Tu, J Cryst Growth 128, 538 (1993). 14 12 Table 1

  18. A Study of GaAsSb Nanowires by Molecular Beam Epitaxy for Near IR Applications

    Science.gov (United States)

    2015-09-18

    8), 1578–1580, 2003. 14. C. Thelander, H. A. Nilsson, L. E. Jensen, and L. Samuelson , Nano Lett. 5(4), 635–638, 2005. 15. Y. Huang, X. Duan, and C... Samuelson , and L.E. Wernersson, J. Cryst. Growth 310(18), 4115–4121, 2008. 28. A. F. Moses, T. B. Hoang, D. L. Dheeraj, H. L. Zhou, A. T. J. van Helvoort

  19. Redetermination of 1,4-dimethoxybenzene

    Directory of Open Access Journals (Sweden)

    David M. Grant

    2009-02-01

    Full Text Available 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.

  20. Molecular weight–gyration radius relation of globular proteins: a comparison of light scattering, small-angle X-ray scattering and structure-based data

    Science.gov (United States)

    Smilgies, Detlef-M.; Folta-Stogniew, Ewa

    2015-01-01

    The molecular weight–gyration radius relation for a number of globular proteins based on experimental light scattering data is compared with small-angle X-ray scattering data recently published by Mylonas & Svergun [J. Appl. Cryst. (2007 ▸), 40, s245–s249]. In addition, other recent experimental data and theoretical calculations are reviewed. It is found that the M W–R g relation for the globular proteins is well represented by a power law with an exponent of 0.37 (2). PMID:26500468

  1. Expansion Coefficient on Oxides and Oxide Ceramics.

    Science.gov (United States)

    1986-05-01

    Ferroelectrics )," Ph.D. thesis submitted to the Indian Institute of Science, Bangalore- 12, (1969). 29. B. Alefeld. "The Change of Lattice Parameters of...Kamenetskii. "Anomalous Thermal Expansion of ZrO2 and HfO2 Over the Range 20-1200 0 C," Soy. Phy.-Cryst., 14 (1970) pp. 696-99. 89. A. K. Sreedhar. "Thermal...D. Gac. "Axial and Linear Thermal Expansion of ZrO 2 and HfO2 ," Am. Ceram. Soc. RuZl. 60(4) (1981), pp. 504-506. 167. R. Ruh, G. W. Hollenberg, E

  2. 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.

  3. NCBI nr-aa BLAST: CBRC-TBEL-01-0595 [SEVENS

    Lifescience Database Archive (English)

    Full Text Available pdb|2I35|A Chain A, Crystal Structure Of Rhombohedral Crystal Form Of Ground- State Rhodopsin pdb|2I36|A Cha...in A, Crystal Structure Of Trigonal Crystal Form Of Ground-State Rhodopsin pdb|2I36|B Chain B, Crystal Struc...ture Of Trigonal Crystal Form Of Ground-State Rhodopsin pdb|2I36|C Chain C, Cryst...al Structure Of Trigonal Crystal Form Of Ground-State Rhodopsin pdb|2I37|A Chain A, Crystal Structure Of A P

  4. NCBI nr-aa BLAST: CBRC-BTAU-01-2416 [SEVENS

    Lifescience Database Archive (English)

    Full Text Available pdb|2I35|A Chain A, Crystal Structure Of Rhombohedral Crystal Form Of Ground- State Rhodopsin pdb|2I36|A Cha...in A, Crystal Structure Of Trigonal Crystal Form Of Ground-State Rhodopsin pdb|2I36|B Chain B, Crystal Struc...ture Of Trigonal Crystal Form Of Ground-State Rhodopsin pdb|2I36|C Chain C, Cryst...al Structure Of Trigonal Crystal Form Of Ground-State Rhodopsin pdb|2I37|A Chain A, Crystal Structure Of A P

  5. Novel Virtual Substrates for Future Generation IR Photodetectors

    Science.gov (United States)

    2014-12-23

    substrates, J. Cryst. Growth, submitted for publication. [4] X.-H. Zhao, M.J. DiNezza, S. Liu, P.A.R.D. Jayathilaka, O.C. Noriega , T.H. Myers,, and Y.- H...Pathiraja A. R. D. Jayathilaka, Odille C. Noriega , Thomas H. Myers, and Yong-Hang Zhang, "Temperature-dependent time-resolved photoluminescence study of...X.-H Zhao, M. J. DiNezza, S. Liu, E. G. LeBlanc, P. Jayathilaka, O. C. Noriega , T. H. Myers, and Y.-H. Zhang, "CdTe/MgCdTe Double Heterostructures

  6. Atomic-Scale Imaging of Surfaces and Interfaces. Materials Research Society Symposium Proceedings Held in Boston, Massachusetts on November 30-December 2, 1992. Volume 295

    Science.gov (United States)

    1992-01-01

    51 J. J. Barton, Phys. Rev. Lett. 61, 1356 (1988) [6] S. Hardcastle, Z. -L. Han, G. R. Harp, J1. Zhang, H. L. Chen, D. K. Saldin and B. P. Tonner...Quian, Phys, Rev. B (in press). [11] W. Quian, J.C.H. Spence and J.M. Zuo, Acta Cryst. (in press). [12] G.R. Harp, D.K. Saldin , and B.P. Tonner, Phys...Lett. 67, 3102 (19--). (15] J.J. Barton, Phys. Rev. Lett. 67, 3106 (1991). [16) D.K. Saldin , G.R. Harp, B.L. Chen, and B.P. Tonner, Phys. Rev. B 44

  7. RbZnFe(PO4)2: synthesis and crystal structure

    Science.gov (United States)

    Badri, Abdessalem; Ben Amara, Mongi

    2016-01-01

    A new iron phosphate, rubidium zinc iron(III) phosphate, RbZnFe(PO4)2, has been synthesized as single crystals by the flux method. This compound is isostructural to the previously reported KCoAl(PO4)2 [Chen et al. (1997 ▸). Acta Cryst. C53,1754–1756]. Its structure consists of a three-dimensional framework built up from corner-sharing PO4 and (Zn,Fe)O4 tetra­hedra. This mode of linkage forms channels parallel to the [100], [010] and [001] directions in which the Rb+ ions are located. PMID:27536385

  8. Semiconductor Laser Diode Arrays by MOCVD (Metalorganic Chemical Vapor Deposition)

    Science.gov (United States)

    1987-09-01

    Roberts. N. J1. Mason. and M. Robinson, J. Cryst. Growth 68, 422 (1984). ’M. R. Leys. C. van Opdorp. M. P. A. .’iegers, and H. J. Talen -van der Mheen...geometry effects is and superlattices has been dominated obtained by including one measured by the MOCVD growth technology . data point in the analysis...Dapkus, Gallium : Arsenide Technology , D.K. Ferry, Ed., tices i Howard W. Sams and Co., Indianapolis, hetero- 1985, p. 79. s is nec- G . 4. G. Costrini and

  9. 3-Substituted Indole Inhibitors Against Francisella tularensis FabI Identified by Structure-Based Virtual Screening

    Science.gov (United States)

    2013-07-01

    FabI, but share low sequence identity and are poorly inhibited by triclosan.25,26 S. pneumoniae and P. aeruginosa contain FabK,24 and Vibrio cholerae ,27...Massengo-Tiasse, R. P.; Cronan, J. E. Vibrio cholerae FabV defines a new class of enoyl-acyl carrier protein reductase. J. Biol. Chem. 2008, 283, 1308...of enoyl- (acyl-carrier protein) reductase, FabV, from Vibrio fischeri. Acta Crystallogr., Sect. F: Struct. Biol. Cryst. Commun. 2012, 68, 78−80. (27

  10. An introduction to the tools hosted in the Bilbao Crystallographic Server

    Directory of Open Access Journals (Sweden)

    Aroyo M.I.

    2012-03-01

    Full Text Available The programs hosted in the Bilbao Crystallographic Server (http://www.cryst.ehu.es are briefly explained along with worked examples on various cases related to different fields of applications. It is our aim to have this text acting as a primer on the various usage of the crystallographic tools in conjunction with each other due to the modular structure of the server. For this reason, diverse topics such as crystallographic groups and their subgroups, pseudosymmetry, extinction conditions, k-vectors and irreducible representations have been discussed in the context.

  11. 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.

  12. 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].

  13. 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.

  14. Two-dimensional motion of unstable steps induced by flow in solution

    OpenAIRE

    Sato, Masahide

    2011-01-01

    By carrying out Monte Carlo simulation, we study step instabilities during crystal growth from solution. In previous studies [M. Sato. J. Phys. Soc. Jpn. 79 (2010) 064606; M. Sato, J. Cryst. Growth 318 (2011) 5; M. Sato. J. Phys. Soc. Jpn. 80 (2011) 024604], we used a one-dimensional model, so that we were unable to study another type of instability, step wandering. In this research, we use a two-dimensional model to study both step wandering and step bunching. When the flow of solutes is in ...

  15. InxGa1-xSb Channel p-Metal-Oxide-Semiconductor Field Effect Transistors: Effect of Strain and Heterostructure Design

    Science.gov (United States)

    2011-07-06

    from 300 K to 80 K, ION increased up to 4 times due to the increase in the hole mobility, while IOFF decreased by a factor of 10 3, indi- cating a diode...N. A. Papanicolaou , and J. B. Boos, J. Cryst. Growth 312(1), 37 (2009). TABLE I. Surface roughness comparison with known values in silicon and...Bennett, N. A. Papanicolaou , M. G. Ancona, J. G. Cham- plain, R. Bass, and B. V. Shanabrook, Electron. Lett. 43, 834 (2007). 15A. Nainani, T. Irisawa, Z

  16. 3-(6-Bromo-4-oxo-4H-chromen-3-yl-3,4-dihydro-2H-1,2,4-benzothiadiazine-1,1-dione

    Directory of Open Access Journals (Sweden)

    Ghulam Abbas

    2010-12-01

    Full Text Available The molecular structure of the title compound, C16H11BrN2O4S, is very similar to that of the previously reported fluoro analogue [al-Rashida et al. (2010. Acta Cryst. E66, o2707]. The mean planes of the bicyclic chromone system and the benzene ring of the benzothiadiazine derivative make a dihedral angle of 58.23 (8°. An intramolecular N—H...O hydrogen bond occurs. In the crystal, molecules are linked into layers by N—H...O and C—H...O hydrogen bonds, generating an infinite two-dimensional network.

  17. Cinchonidinium chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Shi-Feng Ni

    2008-01-01

    Full Text Available In the title salt, C19H23N2O+·Cl−·H2O, the ions and the water molecule are held together by O—H...Cl, N—H...Cl, O—H...O, O—H...N and C—H...Cl hydrogen bonds, forming a three-dimensional framework. The vinyl group is disordered over two orientations with refined occupancies of 0.564 (16 and 0.436 (16. The cell parameters of the title compound have been reported previously [Griffiths (1952. Acta Cryst. 5, 290–291].

  18. Application of maximum likelihood to direct methods: the probability density function of the triple-phase sums. XI.

    Science.gov (United States)

    Rius, Jordi

    2006-09-01

    The maximum-likelihood method is applied to direct methods to derive a more general probability density function of the triple-phase sums which is capable of predicting negative values. This study also proves that maximization of the origin-free modulus sum function S yields, within the limitations imposed by the assumed approximations, the maximum-likelihood estimates of the phases. It thus represents the formal theoretical justification of the S function that was initially derived from Patterson-function arguments [Rius (1993). Acta Cryst. A49, 406-409].

  19. Patterson function and δ recycling: derivation of the phasing equations.

    Science.gov (United States)

    Rius, Jordi

    2012-05-01

    Two phasing equations based on the Fourier syntheses δ(P) = T(-1)[(E(2) - )exp(iφ)] and δ(M) = T(-1)[(E - )exp(iφ)] were recently described [Rius (2012). Acta Cryst. A 68, 77-81] (E is the quasi-normalized structure factor and is the average over all reflections). These equations were found by comparison with the direct methods origin-free modulus sum function and constitute the core of the `δ recycling' phasing procedure. The derivation of these phasing equations from the minimization of a residual (R(P)) between two differently calculated density functions (one of them including the positivity constraint) is shown.

  20. N-Methyl-N-styrylcinnamamide (lansamide from Clausena lansium in Vietnam

    Directory of Open Access Journals (Sweden)

    Peter Luger

    2009-04-01

    Full Text Available The title compound, C18H17NO, was isolated from the seeds of Clausena lansium (wampee (Rutaceae. The X-ray crystal structure analysis confirmed its chemical identity and revealed that it is solvent-free, in contrast to the previously reported monohydrate [Huang, Ou & Tang (2006. Acta Cryst. E62, o1987–o1988]. The molecular structures are practically identical but the molecules pack differently. In contrast to the monohydrate in which the water molecule generates two hydrogen bonds, no such intermolecular contacts are present in the title compound. The dihedral angle between the cinnamamide and the styryl group is 53.1 (1°.

  1. trans-Dichloridobis(triphenylphosphane-κPpalladium(II benzene hemisolvate

    Directory of Open Access Journals (Sweden)

    Frank Meyer-Wegner

    2012-04-01

    Full Text Available The title complex, [PdCl2(C18H15P2]·0.5C6H6, has the PdII ion in a square-planar coordination mode (r.m.s. deviation for Pd, P and Cl atoms = 0.024 Å with the PPh3 and Cl ligands mutually trans. The benzene solvent molecule is located about a crystallographic inversion centre. The title complex is isostructural with trans-dichloridobis(triphenylphosphanepalladium(II 1,4-dichlorobenzene sesquisolvate [Kitano et al. (1983. Acta Cryst. C39, 1015–1017].

  2. Crystal structure of hexaaquadichloridoytterbium(III chloride

    Directory of Open Access Journals (Sweden)

    Kevin M. Knopf

    2015-06-01

    Full Text Available The crystal structure of the title compound, [YbCl2(H2O6]Cl, was determined at 110 K. Samples were obtained from evaporated acetonitrile solutions containing the title compound, which consists of a [YbCl2(H2O6]+ cation and a Cl− anion. The cations in the title compound sit on a twofold axis and form O—H...Cl hydrogen bonds with the nearby Cl− anion. The coordination geometry around the metal centre forms a distorted square antiprism. The ytterbium complex is isotypic with the europium complex [Tambrornino et al. (2014. Acta Cryst. E70, i27].

  3. Crystal structure of hexa-aqua-dichlorido-ytterbium(III) chloride.

    Science.gov (United States)

    Knopf, Kevin M; Crundwell, Guy; Westcott, Barry L

    2015-06-01

    The crystal structure of the title compound, [YbCl2(H2O)6]Cl, was determined at 110 K. Samples were obtained from evaporated aceto-nitrile solutions containing the title compound, which consists of a [YbCl2(H2O)6](+) cation and a Cl(-) anion. The cations in the title compound sit on a twofold axis and form O-H⋯Cl hydrogen bonds with the nearby Cl(-) anion. The coordination geometry around the metal centre forms a distorted square anti-prism. The ytterbium complex is isotypic with the europium complex [Tambrornino et al. (2014 ▶). Acta Cryst. E70, i27].

  4. Crystal structure of benzene-1,3,5-tri-carb-oxy-lic acid-4-pyridone (1/3).

    Science.gov (United States)

    Staun, Selena L; Oliver, Allen G

    2015-11-01

    Slow co-crystallization of a solution of benzene-1,3,5-tri-carb-oxy-lic acid with a large excess of 4-hy-droxy-pyridine produces an inter-penetrating, three-dimensional, hydrogen-bonded framework consisting of three 4-pyridone and one benzene-1,3,5-tri-carb-oxy-lic acid mol-ecules, C9H6O6·3C5H5NO. This structure represents an ortho-rhom-bic polymorph of the previously reported C-centered, monoclinic structure [Campos-Gaxiola et al. (2014 ▸). Acta Cryst. E70, o453-o454].

  5. Erratum: 2-(2-Thien-yl)-4,5-dihydro-1H-imidazole. Corrigendum.

    Science.gov (United States)

    Kia, Reza; Fun, Hoong-Kun; Kargar, Hadi

    2009-05-23

    Consideration of a previous unrecognized twinning of the original investigated crystal of the title compound [Kia et al. (2009 ▶). Acta Cryst. E65, o301] led to improved reliability factors and to a slightly higher precision for all geometric parameters. The crystal under investigation was twinned by pseudo-merohedry with [100, 00, 00] as the twin matrix and a refined twin domain fraction of 0.9610 (5):0.0390 (5). The results of the new crystal structure refinement are given here.[This corrects the article DOI: 10.1107/S1600536809001068.].

  6. 2-(2-Thien­yl)-4,5-dihydro-1H-imidazole. Corrigendum

    Science.gov (United States)

    Kia, Reza; Fun, Hoong-Kun; Kargar, Hadi

    2009-01-01

    Consideration of a previous unrecognized twinning of the original investigated crystal of the title compound [Kia et al. (2009 ▶). Acta Cryst. E65, o301] led to improved reliability factors and to a slightly higher precision for all geometric parameters. The crystal under investigation was twinned by pseudo-merohedry with [100, 00, 00] as the twin matrix and a refined twin domain fraction of 0.9610 (5):0.0390 (5). The results of the new crystal structure refinement are given here. PMID:21582973

  7. 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.

  8. Synthesis and Thermal Behaviour of Lanthanide Complexes of 4′-[(Cholesterylox y)Carbonyl]-Benzo-15-Crown-5

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Lanthanide complexes of a steroid-substituted benzocrown ether were synthesised . The metal-to-ligand ratio of all the metal complexes is 1∶1. The ligand 4′ -[(cholesteryloxy)carbonyl]-benzo-15-crown-5 is a monotropic liquid cryst al, displaying a cholesteric mesophase. The lanthanide complexes with nitrate co unter-ions form a highly viscous mesophase, decomposing at the clearing point. The transition temperatures change as a function of the lanthanide ion. The corr esponding lanthanide complexes with dodecylsulphate (DOS) counter-ions do not f orm a mesophase. In both cases, the metal complexes have a much lower melting po int than the parent ligand.

  9. A revised version of the program VEC (visual computing in electron crystallography)

    Institute of Scientific and Technical Information of China (English)

    Li Xue-Ming; Li Fang-Hua; Fan Hai-Fu

    2009-01-01

    The program package VEC (Visual computing in Electron Crystallography) has been revised such that (i) a program converting one-line symbols to two-line symbols of (3+1)-dimensional superspace groups has been incorporated into VEC so that the latter can interpret both kinds of symbols; (ii) a bug in calculating structure factors of one-dimensionally incommensurate modulated crystals has been fixed. The correction has been verified by successfully matching the experimental electron microscopy image of an incommensurate crystal with a series of simulated images.The precompiled revised version of VEC and relevant materials are available on the Web at http://cryst.iphy.ac.cn.

  10. Molecular ordering of ethanol at the calcite surface

    DEFF Research Database (Denmark)

    Pasarín, I. S.; Yang, M.; Bovet, Nicolas Emile

    2012-01-01

    -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-CH2-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...

  11. 3-Phenylisoxazolin-5-one: a redetermination

    Directory of Open Access Journals (Sweden)

    Abdelhanine Essaghouani

    2017-01-01

    Full Text Available The structure of the title molecule, C9H7NO2, has been redetermined to improved precision and the H atoms located [Cannas et al. (1969. Acta Cryst. B25, 1050]. The five-membered ring is almost planar (r.m.s. deviation = 0.006 Å and subtends a dihedral angle of 2.45 (6° with the benzene ring. In the crystal, molecules form ribbons running parallel to the a-axis direction through a combination of C—H...N and C—H...O hydrogen bonds. `Stair-step' offset π–π stacking interactions are also observed.

  12. 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].

  13. iotbx.cif: a comprehensive CIF toolbox.

    Science.gov (United States)

    Gildea, Richard J; Bourhis, Luc J; Dolomanov, Oleg V; Grosse-Kunstleve, Ralf W; Puschmann, Horst; Adams, Paul D; Howard, Judith A K

    2011-12-01

    iotbx.cif is a new software module for the development of applications that make use of the CIF format. Comprehensive tools are provided for input, output and validation of CIFs, as well as for interconversion with high-level cctbx [Grosse-Kunstleve, Sauter, Moriarty & Adams (2002). J. Appl. Cryst.35, 126-136] crystallographic objects. The interface to the library is written in Python, whilst parsing is carried out using a compiled parser, combining the performance of a compiled language (C++) with the benefits of using an interpreted language.

  14. Electron Spin Polarization and Detection in InAs Quantum Dots Through p-Shell Trions

    Science.gov (United States)

    2010-01-08

    Kurtze, M. Bayer, S. Fafard, Z. Wasilewski , and A. Forchel, Phys. Rev. B 71, 235328 2005. 15M. E. Ware, E. A. Stinaff, D. Gammon, M. F. Doty, A. S...Potemski, S. Raymond, J. Lapointe, and Z. R. Wasilewski , Phys. Status Solidi C 3, 3748 2006. 17 I. V. Ignatiev, S. Y. Verbin, I. Y. Gerlovin, R. V...045305-5 20Z. R. Wasilewski , S. Fafard, and J. P. McCaffrey, J. Cryst. Growth 201-202, 1131 1999. 21A. Greilich, D. R. Yakovlev, A. Shabaev, A. L. Efros

  15. 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.

  16. The structure and refinement of apocrustacyanin C2 to 1.3 A resolution and the search for differences between this protein and the homologous apoproteins A1 and C1.

    Science.gov (United States)

    Habash, Jarjis; Helliwell, John R; Raftery, James; Cianci, Michele; Rizkallah, Pierre J; Chayen, Naomi E; Nneji, Gwen A; Zagalsky, Peter F

    2004-03-01

    The blue carotenoprotein alpha-crustacyanin of Homarus gammarus lobster carapace is comprised chemically of five 20 kDa subunits. Only two genes for the proteins have been isolated (J. B. C. Findlay, personal communication) and the five apoproteins fall into two sets of homologous proteins based on their chemical properties (CRTC, consisting of apoproteins C(1), C(2) and A(1), and CRTA, consisting of apoproteins A(2) and A(3)). The diffraction quality of apo C(2) has been improved from 2.2 to 1.3 A and its structure solved. The structure is compared with the A(1) and C(1) proteins determined at 1.4 A [Cianci et al. (2001), Acta Cryst. D57, 1219-1229] and 1.15 A, respectively [Gordon et al. (2001), Acta Cryst. D57, 1230-1237] and found to be very similar. Normalized B-factor difference plots per residue of different types were used to try to find chemically modified residues; none were found at these resolutions. It remains possible that the differences between the CRTC proteins result from differences in amidation. By comparison of a crystal grown with glycerol (studied at 1.6 A) and one grown without glycerol (studied at 1.3 A) it was seen that glycerol bound at the astaxanthin site.

  17. Crystal structure and Hirshfeld surface analysis of 1-carb­oxy-2-(3,4-di­hydroxy­phen­yl)ethan-1-aminium chloride 2-ammonio-3-(3,4-di­hydroxy­phen­yl)propano­ate: a new polymorph of l-dopa HCl and isotypic with its bromide counterpart

    Science.gov (United States)

    Kathiravan, Perumal; Balakrishnan, Thangavelu; Venkatesan, Perumal; Ramamurthi, Kandasamy; Percino, María Judith; Thamotharan, Subbiah

    2016-01-01

    The title mol­ecular salt, C9H12NO4 +·Cl−·C9H11NO4, is isotypic with that of the bromide counterpart [Kathiravan et al. (2016 ▸). Acta Cryst. E72, 1544–1548]. The title salt is a second monoclinic polymorph of the l-dopa HCl structure reported earlier in the monoclinic space group P21 [Jandacek & Earle (1971 ▸). Acta Cryst. B27, 841–845; Mostad & Rømming (1974 ▸). Acta Chemica Scand. B28, 1161–1168]. In the title compound, monoclinic space group I2, one of the dopa mol­ecules has a positive charge with a protonated α-amino group and the α-carb­oxy­lic acid group uncharged, while the second dopa mol­ecule has a neutral charge, the α-amino group is protonated and the α-carb­oxy­lic acid is deprotonated. In the previously reported form, a single dopa mol­ecule is observed in which the α-amino group is protonated and the α-carb­oxy­lic acid group is uncharged. The invariant and variations of various types of inter­molecular inter­actions present in these two forms of dopa HCl structures are discussed with the aid of two-dimensional fingerprint plots. PMID:27840723

  18. Crystal structure and Hirshfeld surface analysis of 1-carb-oxy-2-(3,4-di-hydroxy-phen-yl)ethan-1-aminium chloride 2-ammonio-3-(3,4-di-hydroxy-phen-yl)propano-ate: a new polymorph of l-dopa HCl and isotypic with its bromide counterpart.

    Science.gov (United States)

    Kathiravan, Perumal; Balakrishnan, Thangavelu; Venkatesan, Perumal; Ramamurthi, Kandasamy; Percino, María Judith; Thamotharan, Subbiah

    2016-11-01

    The title mol-ecular salt, C9H12NO4(+)·Cl(-)·C9H11NO4, is isotypic with that of the bromide counterpart [Kathiravan et al. (2016 ▸). Acta Cryst. E72, 1544-1548]. The title salt is a second monoclinic polymorph of the l-dopa HCl structure reported earlier in the monoclinic space group P21 [Jandacek & Earle (1971 ▸). Acta Cryst. B27, 841-845; Mostad & Rømming (1974 ▸). Acta Chemica Scand. B28, 1161-1168]. In the title compound, monoclinic space group I2, one of the dopa mol-ecules has a positive charge with a protonated α-amino group and the α-carb-oxy-lic acid group uncharged, while the second dopa mol-ecule has a neutral charge, the α-amino group is protonated and the α-carb-oxy-lic acid is deprotonated. In the previously reported form, a single dopa mol-ecule is observed in which the α-amino group is protonated and the α-carb-oxy-lic acid group is uncharged. The invariant and variations of various types of inter-molecular inter-actions present in these two forms of dopa HCl structures are discussed with the aid of two-dimensional fingerprint plots.

  19. On the crystal structure of Cr2N precipitates in high-nitrogen austenitic stainless steel. III. Neutron diffraction study on the ordered Cr2N superstructure.

    Science.gov (United States)

    Lee, Tae-Ho; Kim, Sung-Joon; Shin, Eunjoo; Takaki, Setsuo

    2006-12-01

    The ordered structure of Cr(2)N precipitates in high-nitrogen austenitic steel was investigated utilizing high-resolution neutron powder diffractometry (HRPD). On the basis of the Rietveld refinement of neutron diffraction patterns, the ordered Cr2N superstructure was confirmed to be trigonal (space group P31m), with lattice parameters a=4.800 (4) and c=4.472 (5) A, as suggested in previous transmission electron microscopy studies [Lee, Oh, Han, Lee, Kim & Takaki (2005). Acta Cryst. B61, 137-144; Lee, Kim & Takaki (2006). Acta Cryst. B62, 190-196]. The occupancies of the N atoms in four crystallographic sites [1(a), 1(b), 2(d) and 2(c) Wyckoff sites] were determined to be 1.00 (5), 0.0, 0.74 (9) and 0.12 (3), respectively, reflecting a partial disordering of N atoms along the c axis. The position of the metal atom was specified to be x=0.346 (8) and z=0.244 (6), corresponding to a deviation from the ideal position (x=0.333 and z=0.250). This deviation caused the ((1/3 1/3)(0))-type superlattice reflection to appear. A comparison between the ideal and measured crystal structures of Cr2N was performed using a computer simulation of selected-area diffraction patterns.

  20. 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.

  1. Crystal structure and Hirshfeld surface analysis of 1-carboxy-2-(3,4-dihydroxyphenylethan-1-aminium chloride 2-ammonio-3-(3,4-dihydroxyphenylpropanoate: a new polymorph of l-dopa HCl and isotypic with its bromide counterpart

    Directory of Open Access Journals (Sweden)

    Perumal Kathiravan

    2016-11-01

    Full Text Available The title molecular salt, C9H12NO4+·Cl−·C9H11NO4, is isotypic with that of the bromide counterpart [Kathiravan et al. (2016. Acta Cryst. E72, 1544–1548]. The title salt is a second monoclinic polymorph of the l-dopa HCl structure reported earlier in the monoclinic space group P21 [Jandacek & Earle (1971. Acta Cryst. B27, 841–845; Mostad & Rømming (1974. Acta Chemica Scand. B28, 1161–1168]. In the title compound, monoclinic space group I2, one of the dopa molecules has a positive charge with a protonated α-amino group and the α-carboxylic acid group uncharged, while the second dopa molecule has a neutral charge, the α-amino group is protonated and the α-carboxylic acid is deprotonated. In the previously reported form, a single dopa molecule is observed in which the α-amino group is protonated and the α-carboxylic acid group is uncharged. The invariant and variations of various types of intermolecular interactions present in these two forms of dopa HCl structures are discussed with the aid of two-dimensional fingerprint plots.

  2. 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.

  3. Collaborative annotation of 3D crystallographic models.

    Science.gov (United States)

    Hunter, J; Henderson, M; Khan, I

    2007-01-01

    This paper describes the AnnoCryst system-a tool that was designed to enable authenticated collaborators to share online discussions about 3D crystallographic structures through the asynchronous attachment, storage, and retrieval of annotations. Annotations are personal comments, interpretations, questions, assessments, or references that can be attached to files, data, digital objects, or Web pages. The AnnoCryst system enables annotations to be attached to 3D crystallographic models retrieved from either private local repositories (e.g., Fedora) or public online databases (e.g., Protein Data Bank or Inorganic Crystal Structure Database) via a Web browser. The system uses the Jmol plugin for viewing and manipulating the 3D crystal structures but extends Jmol by providing an additional interface through which annotations can be created, attached, stored, searched, browsed, and retrieved. The annotations are stored on a standardized Web annotation server (Annotea), which has been extended to support 3D macromolecular structures. Finally, the system is embedded within a security framework that is capable of authenticating users and restricting access only to trusted colleagues.

  4. Redetermination of Zn2Mo3O8

    Directory of Open Access Journals (Sweden)

    Jerome Cuny

    2009-07-01

    Full Text Available The crystal structure of dizinc trimolybdenum(IV octaoxide, Zn2Mo3O8, has been redetermined from single-crystal X-ray data. The structure has been reported previously based on neutron powder diffraction data [Hibble et al. (1999. Acta Cryst. B55, 683-697] and single-crystal data [McCarroll et al. (1957. J. Am. Chem. Soc. 79, 5410–5414; Ansell & Katz (1966 Acta Cryst. 21, 482–485]. The results of the current redetermination show an improvement in the precision of the structural and geometric parameters with all atoms refined with anisotropic displacement parameters. The crystal structure consists of distorted hexagonal-close-packed oxygen layers with stacking sequence abac along [001] and is held together by alternating zinc and molybdenum layers. The Zn atoms occupy both tetrahedral and octahedral interstices with a ratio of 1:1. The Mo atoms occupy octahedral sites and form strongly bonded triangular clusters involving three MoO6 octahedra that are each shared along two edges, forming a Mo3O13 unit. All atoms lie on special positions. The Zn atoms are in 2b Wyckoff positions with 3m. site symmetry, the Mo atoms are in 6c Wyckoff positions with . m. site symmetry and the O atoms are in 2a, 2b and 6c Wyckoff positions with 3m. and . m. site symmetries, respectively.

  5. Grazing-incidence small-angle X-ray scattering in a twofold rough-interface medium: a new theoretical approach using the q-eigenwave formalism.

    Science.gov (United States)

    Chukhovskii, F N; Roshchin, B S

    2015-11-01

    Based on the rigorous Green function formalism to describe the grazing-incidence small-angle X-ray scattering (GISAXS) problem, a system of two linked integral equations is derived with respect to amplitudes of the reflected and transmitted plane q-eigenwaves (eigenstate functions) propagating through two homogeneous media separated from each other by a rough surface interface. To build up the coupled solutions of these basic equations beyond the perturbation theory constraint 2kσθ0 < 1, a simple iteration procedure is proposed as opposed to the self-consistent wave approach [Chukhovskii (2011). Acta Cryst. A67, 200-209; Chukhovski (2012). Acta Cryst. A68, 505-512]. Using the first-order iteration, analytical expressions for the averaged specular and non-specular scattering intensity distributions have been obtained. These expressions are further analysed in terms of the GISAXS parameters {k, θ, θ0} and surface finish ones {σ, l, h}, where θ and θ0 are the scattering and incidence angles of the X-rays, respectively, σ is the root-mean-square roughness, l is the correlation length, h is the fractal surface model index, k = 2π/λ, and λ is the X-ray wavelength. A direct way to determine the surface finish parameters from the experimental specular and diffuse scattering indicatrix scan data is discussed for an example of GISAXS measurements from rough surfaces of α-quartz and CdTe samples.

  6. High-resolution structure of human carbonic anhydrase II complexed with acetazolamide reveals insights into inhibitor drug design.

    Science.gov (United States)

    Sippel, Katherine H; Robbins, Arthur H; Domsic, John; Genis, Caroli; Agbandje-McKenna, Mavis; McKenna, Robert

    2009-10-01

    The crystal structure of human carbonic anhydrase II (CA II) complexed with the inhibitor acetazolamide (AZM) has been determined at 1.1 A resolution and refined to an R(cryst) of 11.2% and an R(free) of 14.7%. As observed in previous CA II-inhibitor complexes, AZM binds directly to the zinc and makes several key interactions with active-site residues. The high-resolution data also showed a glycerol molecule adjacent to the AZM in the active site and two additional AZMs that are adventitiously bound on the surface of the enzyme. The co-binding of AZM and glycerol in the active site demonstrate that given an appropriate ring orientation and substituents, an isozyme-specific CA inhibitor may be developed.

  7. An alternative empirical model for the relationship between the bond valence and the thermal expansion rate of chemical bonds.

    Science.gov (United States)

    Sidey, Vasyl

    2015-08-01

    The relationship between the bond valence s and the thermal expansion rate of chemical bonds (dr/dT) has been closely approximated by using the alternative three-parameter empirical model (dr/dT) = (u + vs)(-1/w), where u, v and w are the refinable parameters. Unlike the s-(dr/dT) model developed by Brown et al. [(1997), Acta Cryst. B53, 750-761], this alternative model can be optimized for particular s-(dr/dT) datasets in the least-squares refinement procedure. For routine calculations of the thermal expansion rates of chemical bonds, the alternative model with the parameters u = -63.9, v = 2581.0 and w = 0.647 can be recommended.

  8. A monoclinic polymorph of 1,2-bis[(1-methyl-1H-tetrazol-5-ylsulfanyl]ethane (BMTTE

    Directory of Open Access Journals (Sweden)

    Saray Argibay-Otero

    2017-10-01

    Full Text Available The synthesis and crystal structure of a monoclinic (P21/c polymorph of the title compound, C6H10S2N8, are reported. The molecule has pseudo-twofold rotational symmetry, with the tetrazole rings being inclined to one another by 5.50 (6°. In the crystal, molecules are linked by C—H...N hydrogen bonds, forming chains propagating along [101] and enclosing R22(20 ring motifs. The chains are linked by offset π–π interactions involving the tetrazole rings [intercentroid distances vary from 3.3567 (7 to 3.4227 (7 Å], forming layers parallel to the ac plane. The crystal structure of the triclinic polymorph (P\\overline{1} has been described previously [Li et al. (2011. Acta Cryst. E67, o1669].

  9. 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.

  10. 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.

  11. Quench-in of different high T complexities of glassformers for leisurely study at lower temperatures

    DEFF Research Database (Denmark)

    Angell, C. A.; Yue, Yuanzheng; Wang, L. M.

    Quenching-in of different high T complexities of glassformers for leisurely study at lower temperatures We describe a series of experiments on glass-forming liquids that are motivated by a common idea. The idea is that of trapping in a high enthalpy, high entropy, and state of the system...... from that at constant volume. For glassformers that can exhibit liquid-liquid transitions, one can use the cold equilibration approach to determine the fragility of the high temperature phase, and the enthalpy of the liquid-liquid transition, see ref.2. References. 1. C. A. Angell, Yuanzheng Yue, Limin...... Wang, John R. D. Copley, Steve Borick and Stefano Mossa. J. Phys. Cond Matt 15, S1051-S1068 (2003) 2. M. C. Wilding, P. F. McMillan, Polyamorphic transitions in yttria-alumina liquids, J. Non-Cryst. Solids 293, 357 (2001)....

  12. Exact conditional distribution of a three-phase invariant in the space group P1. I. Derivation and simplification of the Fourier series.

    Science.gov (United States)

    Shmueli, U; Rabinovich, S; Weiss, G H

    1989-06-01

    An exact expression is derived for the conditional probability density function of a three-phase invariant and the general result is applied to the space group P1. The expression for the conditional density is given in terms of a sixfold Fourier series. A straightforward numerical evaluation of this series, without further analysis, is extremely time consuming. Much of the present paper is therefore devoted to an exposition of symmetries hidden in the various summations. The computational effort required for the evaluation of the above expression is thereby reduced to manageable proportions in a number of interesting cases. Results of numerical computations of the exact conditional density are given in the second paper in this series. It is also shown that the exact expression for the conditional probability reduces to that given by Cochran [Acta Cryst. (1955), 8, 473-478].

  13. Crystal structure of bis-[tetra-kis-(tri-phenyl-phosphane-κP)silver(I)] (nitrilo-tri-acetato-κ(4) N,O,O',O'')(tri-phenyl-phosphane-κP)argentate(I) with an unknown amount of methanol as solvate.

    Science.gov (United States)

    Noll, Julian; Korb, Marcus; Lang, Heinrich

    2016-03-01

    The structure of the title compound, [Ag(C18H15P)4]2[Ag(C6H6NO6)(C18H15P)], exhibits trigonal (P-3) symmetry, with a C 3 axis through all three complex ions, resulting in an asymmetric unit that contains one third of the atoms present in the formula unit. The formula unit thus contains two of the cations, one anion and disordered mol-ecules of methanol as the packing solvent. Attempts to refine the solvent model were unsuccessful, indicating uninter-pretable disorder. Thus, the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9-18] was applied, accounting for 670 electrons per unit cell, representing approximately 18 mol-ecules of methanol in the formula unit. The stated crystal data for M r, μ etc do not take these into account.

  14. RIBFIND: a web server for identifying rigid bodies in protein structures and to aid flexible fitting into cryo EM maps.

    Science.gov (United States)

    Pandurangan, Arun Prasad; Topf, Maya

    2012-09-15

    To better analyze low-resolution cryo electron microscopy maps of macromolecular assemblies, component atomic structures frequently have to be flexibly fitted into them. Reaching an optimal fit and preventing the fitting process from getting trapped in local minima can be significantly improved by identifying appropriate rigid bodies (RBs) in the fitted component. Here we present the RIBFIND server, a tool for identifying RBs in protein structures. The server identifies RBs in proteins by calculating spatial proximity between their secondary structural elements. The RIBFIND web server and its standalone program are available at http://ribfind.ismb.lon.ac.uk. a.pandurangan@mail.cryst.bbk.ac.uk Supplementary data are available at Bioinformatics online.

  15. Dimethyl 2,2′-[(4-oxo-2-phenyl-4H-chromene-5,7-diyldioxy]diacetate: a less densely packed polymorph

    Directory of Open Access Journals (Sweden)

    Nagarajan Sulochana

    2009-02-01

    Full Text Available The title molecule, C21H18O8, crystallizes in two crystal polymorphs, see also Nallasivam, Nethaji, Vembu & Jaswant [Acta Cryst. (2009, E65, o312–o313]. The main difference between the two polymorphs is in the conformation of the oxomethylacetate groups with regard to the almost planar [total puckering amplitude 0.047 (2 Å] chromene ring. In the title compound, the best planes of the oxomethylacetate groups through the non-H atoms are almost perpendicular to the chromene ring [making dihedral angles of 89.61 (6 and 80.59 (5°], while in the second polymorph the molecules are close to planar. Both crystal structures are stabilized by C—H...O.

  16. GPCRTree: online hierarchical classification of GPCR function

    Directory of Open Access Journals (Sweden)

    Timmis Jon

    2008-08-01

    Full Text Available Abstract Background G protein-coupled receptors (GPCRs play important physiological roles transducing extracellular signals into intracellular responses. Approximately 50% of all marketed drugs target a GPCR. There remains considerable interest in effectively predicting the function of a GPCR from its primary sequence. Findings Using techniques drawn from data mining and proteochemometrics, an alignment-free approach to GPCR classification has been devised. It uses a simple representation of a protein's physical properties. GPCRTree, a publicly-available internet server, implements an algorithm that classifies GPCRs at the class, sub-family and sub-subfamily level. Conclusion A selective top-down classifier was developed which assigns sequences within a GPCR hierarchy. Compared to other publicly available GPCR prediction servers, GPCRTree is considerably more accurate at every level of classification. The server has been available online since March 2008 at URL: http://igrid-ext.cryst.bbk.ac.uk/gpcrtree/.

  17. 1-(Prop-2-ynylindoline-2,3-dione

    Directory of Open Access Journals (Sweden)

    Fatima-Zahrae Qachchachi

    2014-03-01

    Full Text Available The structure of the title compound, C11H7NO2, is isotypic to that of its homologue, 1-octylindoline-2,3-dione [Qachchachi et al. (2013. Acta Cryst. E69, o1801]. The indoline ring and the two carbonyl O atoms are approximately coplanar, the largest deviation from the mean plane being 0.021 (1 Å for one of the O atoms. The mean plane through the fused ring system is nearly perpendicular to the propynyl group, as indicated by the N—C—C—C torsion angle of 77.9 (1°. In the crystal, molecules are linked by C—H...O hydrogen bonds and π–π interactions between benzene rings [intercentroid distance = 3.5630 (10 Å], forming a three-dimensional structure.

  18. A new polymorph of N-(2-{N′-[(1E-2-hydroxybenzylidene]hydrazinecarbonyl}phenylbenzamide

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    Shaaban K. Mohamed

    2014-06-01

    Full Text Available The title compound, C21H17N3O3, is a new polymorph of an already published structure [Shashidhar et al. (2006. Acta Cryst. E62, o4473–o4475]. The previously reported structure crystallizes in the monoclinic space group C2/c, whereas the structure reported here is in the tetragonal space group I41/a. The bond lengths and angles are similar in both structures. The molecule adopts an extended conformation via intramolecular N—H...O and O—H...N hydrogen bonds; the terminal phenyl ring and the hydroxylphenyl ring are twisted with respect to the central benzene ring by 44.43 (7 and 21.99 (8°, respectively. In the crystal, molecules are linked by N—H...O hydrogen bonds, weak C—H...O hydrogen bonds and weak C—H...π interactions into a three-dimensional supramolecular network.

  19. Crystal structure of bis(2-amino-5-chloropyridinium tetrachloridocobaltate(II

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    Marwa Mghandef

    2015-05-01

    Full Text Available The title salt, (C5H6ClN22[CoCl4], was synthesized by slow evaporation of an aqueous solution at room temperature. The asymmetric unit consists of two essentially planar (C5H6ClN2+ cations [maximum deviations = 0.010 (3 and 0.014 (3 Å] that are nearly perpendicular to each other [dihedral angle = 84.12 (7°]. They are bonded through N—H...Cl hydrogen bonds to distorted [CoCl4]2− tetrahedra, leading to the formation of undulating layers parallel to (100. The structure is isotypic with the Zn analogue [Kefi et. al (2011. Acta Cryst. E67, m355–m356.

  20. Redetermination of [Pr(NO33(H2O4]·2H2O

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    Roel Decadt

    2012-07-01

    Full Text Available The structure of the title compound, tetraaquatris(nitrato-κ2O,O′praseodymium(III dihydrate, was redetermined. The structure models derived from the previous determinations [Rumanova et al. (1964. Kristallografiya, 9, 642–654; Fuller & Jacobson (1976. Cryst. Struct. Commun. 5, 349–352] were confirmed, but now with all H atoms unambiguously located, revealing a complex O—H...O hydrogen-bonding network, extending throughout the whole structure. In the title compound, the coordination environment of the PrIII atom can best be described as a distorted bicapped square antiprism defined by three bidentate nitrate anions and four water molecules. Additionally, two lattice water molecules are observed in the crystal packing. The title compound is isotypic with several other lanthanide-containing nitrate analogues.

  1. 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...... 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...

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

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    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.

  3. Structure of Physarum polycephalum cytochrome b5 reductase at 1.56 A resolution.

    Science.gov (United States)

    Kim, Sangwoo; Suga, Michihiro; Ogasahara, Kyoko; Ikegami, Terumi; Minami, Yoshiko; Yubisui, Toshitsugu; Tsukihara, Tomitake

    2007-04-01

    Physarum polycephalum cytochrome b(5) reductase catalyzes the reduction of cytochrome b(5) by NADH. The structure of P. polycephalum cytochrome b(5) reductase was determined at a resolution of 1.56 A. The molecular structure was compared with that of human cytochrome b(5) reductase, which had previously been determined at 1.75 A resolution [Bando et al. (2004), Acta Cryst. D60, 1929-1934]. The high-resolution structure revealed conformational differences between the two enzymes in the adenosine moiety of the FAD, the lid region and the linker region. The structural properties of both proteins were inspected in terms of hydrogen bonding, ion pairs, accessible surface area and cavity volume. The differences in these structural properties between the two proteins were consistent with estimates of their thermostabilities obtained from differential scanning calorimetry data.

  4. Aripiprazole salts. II. Aripiprazole perchlorate.

    Science.gov (United States)

    Freire, Eleonora; Polla, Griselda; Baggio, Ricardo

    2012-06-01

    The molecular structure of aripiprazole perchlorate (systematic name: 4-(2,3-dichlorophenyl)-1-{4-[(2-oxo-1,2,3,4-tetrahydroquinolin-7-yl)oxy]butyl}piperazin-1-ium perchlorate), C(23)H(28)Cl(2)N(3)O(2)(+)·ClO(4)(-), does not differ substantially from the recently published structure of aripiprazole nitrate [Freire, Polla & Baggio (2012). Acta Cryst. C68, o170-o173]. Both compounds have almost identical bond distances, bond angles and torsion angles. The two different counter-ions occupy equivalent places in the two structures, giving rise to very similar first-order `packing motifs'. However, these elemental arrangements interact with each other in different ways in the two structures, leading to two-dimensional arrays with quite different organizations.

  5. A triclinic polymorph of (-)-(S)-N-benzyl-2-[(R)-6-fluoro-chroman-2-yl]-2-hy-droxy-ethanaminium bromide.

    Science.gov (United States)

    Rousselin, Yoann; Laureano, Hugo; Clavel, Alexandre

    2013-12-01

    The title salt, C18H21FNO2 (+)·Br(-), determined at 115 K, crystallizes in the triclinic space group P1. The previously reported polymorph occurs in the monoclinic space group P21 and has two independent mol-ecules in the asymmetric unit [Peeters et al. (1993 ▶). Acta Cryst. C49, 2157-2160]. In the title molecule, the pyran rings adopt half-chair conformations. The absolute configuration is S for the hy-droxy-bearing C atom and R for the asymmetric C atom in the di-hydro-pyran unit. In the crystal, the components are linked by N-H⋯Br and O-H⋯Br hydrogen bonds, forming chains along the c-axis direction. The crystal studied was refined as an inversion twin.

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

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

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    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].

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

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    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.

  9. 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

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    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.

  10. 2-(2-Chlorophenyl-N-cyclohexyl-2-oxoacetamide

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    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.

  11. 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

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    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.

  12. 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

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    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].

  13. 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].

  14. Simulations of Kikuchi patterns due to thermal diffuse scattering on MgO crystals.

    Science.gov (United States)

    Omoto, Kazuya; Tsuda, Kenji; Tanaka, Michiyoshi

    2002-01-01

    Inelastic scattering of fast transmission electrons from a perfect crystal is investigated using the Bloch wave theory. A comprehensive expression for the scattering of electrons is given, which includes both elastic and inelastic multiple scatterings. This expression is an extended form of Fujimoto's expression for elastic scattering (J. Phys. Soc. Japan 14:1558 (1959)). For the approximation of single inelastic scattering, the expression becomes equivalent to the formula of Rez et al. (Phil. Mag. 35: 81 (1977)). When thermal diffuse scattering (TDS) is considered using the Einstein model or the scattering factor for TDS given by Hall and Hirsch (Proc. R. Soc. A 286: 158 (1965)), Rossouw and Bursill's expression (Acta Cryst. A 41: 320 (1985)) is derived. This expression has been used in computer simulations of TDS intensity distribution (Kikuchi pattern). It is shown that the simulations for magnesium oxide (MgO) using 357 beams agree quite well with the experimental ones.

  15. A New, More Stable Polymorphic Form of Otilonium Bromide: Solubility, Crystal Structure, and Phase Transformation.

    Science.gov (United States)

    Vega, Daniel R; Halac, Emilia; Segovia, Luciano; Baggio, Ricardo

    2016-10-01

    A new polymorphic form of otilonium bromide is presented (Form I), and a thorough analysis of its crystal and molecular structure is performed. The compound suffers a temperature-driven first-order phase transition at about 396 K, which transforms it into the polymorph reported by Dapporto P and Sega A (Acta Cryst. 1986;C42:474-478) (Form II). Through thermal analysis and solubility experiments the relative stability of both crystal modifications were determined, confirming that at room temperature this new Form I is the more stable one, Form II existing just in a metastable state. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  16. Triclinic modification of N-[(1,1-dimethylethoxycarbonyl]-3-[(R-prop-2-en-1-ylsulfinyl]-(R-alanine ethyl ester at 120 (1 K

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    Suneel P. Singh

    2009-06-01

    Full Text Available There are two independent molecules in the asymmetric unit of the title compound, C13H23NO5S. In the crystal structure, intermolecular N—H...O hydrogen bonds link molecules into two independent one-dimensional chains along [100]. The crystal studied was found to be a non-merohedral twin with a ratio of 0.615 (6:0.385 (1 for the refined components. At 200 (1 K [Singh et al. (2009. Acta Cryst. E65, o1385–o1386] the crystal structure of the title compound contains one disordered molecule in the asymmetric unit of a monoclinic unit cell.

  17. SPEDEN: Reconstructing single particles from their diffraction patterns

    CERN Document Server

    Hau-Riege, S P; Chapman, H N; Szoke, A; Marchesini, S; Noy, A; He, H; Howells, M R; Weierstall, U; Spence, J C H

    2004-01-01

    Speden is a computer program that reconstructs the electron density of single particles from their x-ray diffraction patterns, using a single-particle adaptation of the Holographic Method in crystallography. (Szoke, A., Szoke, H., and Somoza, J.R., 1997. Acta Cryst. A53, 291-313.) The method, like its parent, is unique that it does not rely on ``back'' transformation from the diffraction pattern into real space and on interpolation within measured data. It is designed to deal successfully with sparse, irregular, incomplete and noisy data. It is also designed to use prior information for ensuring sensible results and for reliable convergence. This article describes the theoretical basis for the reconstruction algorithm, its implementation and quantitative results of tests on synthetic and experimentally obtained data. The program could be used for determining the structure of radiation tolerant samples and, eventually, of large biological molecular structures without the need for crystallization.

  18. Extending the S-FFT direct-methods algorithm to density functions with positive and negative peaks. XIV.

    Science.gov (United States)

    Rius, Jordi; Frontera, Carles

    2008-11-01

    Some years ago the direct-methods origin-free modulus sum function (S) was adapted to the processing of intensity data from density functions with positive and negative peaks [Rius, Miravitlles & Allmann (1996). Acta Cryst. A52, 634-639]. That implementation used phase relationships explicitly. Although successfully applied to different situations where the number of reflections was small, its generalization to larger problems required avoiding the time-consuming manipulation of quartet terms. To circumvent this limitation, a modification of the recently introduced S-FFT algorithm (that maximizes S with only Fourier transforms) is presented here. The resulting S2-FFT algorithm is highly effective for crystal structures with at least one moderate scatterer in the unit cell. Test calculations have been performed on conventional single-crystal X-ray diffraction data, on neutron diffraction data of compounds with negative scatterers and on intensities of superstructure reflections to solve difference structures.

  19. Improving the direct-methods sign-unconstrained S-FFT algorithm. XV.

    Science.gov (United States)

    Rius, Jordi; Frontera, Carles

    2009-11-01

    In order to extend the application field of the direct-methods S-FFT phase-refinement algorithm to density functions with positive and negative peaks, the equal-sign constraint was removed from its definition by combining rho(2) with an appropriate density function mask [Rius & Frontera (2008). Acta Cryst. A64, 670-674]. This generalized algorithm (S(2)-FFT) was shown to be highly effective for crystal structures with at least one moderate scatterer in the unit cell but less effective when applied to structures with only light scatterers. To increase the success rate in this second case, the mask has been improved and the convergence rate of S(2)-FFT has been investigated. Finally, a closely related but simpler phase-refinement function (S(m)) combining rho (instead of rho(2)) with a new mask is introduced. For simple cases at least this can also treat density peaks in the absence of the equal-sign constraint.

  20. A direct phasing method based on the origin-free modulus sum function and the FFT algorithm. XII.

    Science.gov (United States)

    Rius, Jordi; Crespi, Anna; Torrelles, Xavier

    2007-03-01

    An alternative way of refining phases with the origin-free modulus sum function S is shown that, instead of applying the tangent formula in sequential mode [Rius (1993). Acta Cryst. A49, 406-409], applies it in parallel mode with the help of the fast Fourier transform (FFT) algorithm. The test calculations performed on intensity data of small crystal structures at atomic resolution prove the convergence and hence the viability of the procedure. This new procedure called S-FFT is valid for all space groups and especially competitive for low-symmetry ones. It works well when the charge-density peaks in the crystal structure have the same sign, i.e. either positive or negative.

  1. Acanthamoeba polyphaga mimivirus NDK: preliminary crystallographic analysis of the first viral nucleoside diphosphate kinase.

    Science.gov (United States)

    Jeudy, Sandra; Coutard, Bruno; Lebrun, Régine; Abergel, Chantal

    2005-06-01

    The complete sequence of the largest known double-stranded DNA virus, Acanthamoeba polyphaga mimivirus, has recently been determined [Raoult et al. (2004), Science, 306, 1344-1350] and revealed numerous genes not expected to be found in a virus. A comprehensive structural and functional study of these gene products was initiated [Abergel et al. (2005), Acta Cryst. F61, 212-215] both to better understand their role in the virus physiology and to obtain some clues to the origin of DNA viruses. Here, the preliminary crystallographic analysis of the viral nucleoside diphosphate kinase protein is reported. The crystal belongs to the cubic space group P2(1)3, with unit-cell parameter 99.425 A. The self-rotation function confirms that there are two monomers per asymmetric unit related by a twofold non-crystallographic axis and that the unit cell thus contains four biological entities.

  2. Redetermination of 5α-androstane-3,17-dione

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    Jerry P. Jasinski

    2010-06-01

    Full Text Available The structure of the title compound, C19H28O2, has been redermined at 295 (2 K, with much improved precision. The structure and molecular packing of the title compound was first reported by Coiro et al. [Acta Cryst. (1973. B29, 1404–1409] by means of potential-energy calculations. The cell parameters in this study differ considerably in space group C2. It is a derivative of testosterone and consists of a cyclopentanone ring (A fused to to successive cyclohexane (B and C and cyclohexanone (D rings. The three cyclohexanone rings are in slightly distorted boat configurations and the cyclopentanone ring is a distorted half-chair. The crystal packing is stabilized by weak intermolecular C—H...O interactions involving O atoms from each of the cyclohexanone and cyclopentanone rings and H atoms from each of their respective rings.

  3. A monoclinic polymorph of (R,R-4,4′-dibromo-2,2′-[cyclohexane-1,2-diylbis(nitrilomethanylylidene]diphenol

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    Kwang Ha

    2012-05-01

    Full Text Available The title compound, C20H20Br2N2O2, a tetradentate Schiff base, is the enantiomerically pure R,R-diastereomer of four possible stereoisomers. The molecular structure reveals two strong intramolecular O—H...N hydrogen bonds between the hydroxy O atom and the imino N atom, which each generate S(6 rings. In the crystal, molecules are stacked in columns along the a axis; when viewed down the b axis, successive columns are stacked in the opposite direction. The structure reported herein is the monoclinic polymorph of the previously reported orthorhombic form [Yi & Hu (2009. Acta Cryst. E65, o2643], in which the complete molecule is generated by a crystallographic twofold axis.

  4. Tris{2-methoxy-6-[(4-methylphenyliminiomethyl]phenolate-κ2O,O′}tris(thiocyanato-κNeuropium(III

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    Guo-Liang Zhao

    2009-12-01

    Full Text Available The metal center in the structure of the title compound, [Eu(NCS3(C15H15NO23], is coordinated by three Schiff base 2-methoxy-6-[(4-methylphenyliminiomethyl]phenolate (L ligands and three independent thiocyanate ions. In the crystal structure, the acidic H atom is located on the Schiff base N atom and hydrogen bonded to the phenolate O atom. The coordination environment of the EuIII ion is nine-coordinate by three chelating methoxyphenolate pairs of O atoms and three N-atom terminals of the thiocyanate ions. The compound is isostructural with the CeIII analogue [Liu et al. (2009. Acta Cryst. E65, m650].

  5. Refinement of macromolecular structures against neutron data with SHELXL2013.

    Science.gov (United States)

    Gruene, Tim; Hahn, Hinrich W; Luebben, Anna V; Meilleur, Flora; Sheldrick, George M

    2014-02-01

    Some of the improvements in SHELX2013 make SHELXL convenient to use for refinement of macromolecular structures against neutron data without the support of X-ray data. The new NEUT instruction adjusts the behaviour of the SFAC instruction as well as the default bond lengths of the AFIX instructions. This work presents a protocol on how to use SHELXL for refinement of protein structures against neutron data. It includes restraints extending the Engh & Huber [Acta Cryst. (1991), A47, 392-400] restraints to H atoms and discusses several of the features of SHELXL that make the program particularly useful for the investigation of H atoms with neutron diffraction. SHELXL2013 is already adequate for the refinement of small molecules against neutron data, but there is still room for improvement, like the introduction of chain IDs for the refinement of macromolecular structures.

  6. Redetermination of AgPO(3).

    Science.gov (United States)

    Terebilenko, Katherina V; Zatovsky, Igor V; Ogorodnyk, Ivan V; Baumer, Vyacheslav N; Slobodyanik, Nikolay S

    2011-02-09

    Single crystals of silver(I) polyphosphate(V), AgPO(3), were prepared via a phospho-ric acid melt method using a solution of Ag(3)PO(4) in H(3)PO(4). In comparison with the previous study based on single-crystal Weissenberg photographs [Jost (1961 ▶). Acta Cryst. 14, 779-784], the results were mainly confirmed, but with much higher precision and with all displacement parameters refined anisotropically. The structure is built up from two types of distorted edge- and corner-sharing [AgO(5)] polyhedra, giving rise to multidirectional ribbons, and from two types of PO(4) tetra-hedra linked into meandering chains (PO(3))(n) spreading parallel to the b axis with a repeat unit of four tetra-hedra. The calculated bond-valence sum value of one of the two Ag(I) ions indicates a significant strain of the structure.

  7. Redetermination of AgPO3

    Science.gov (United States)

    Terebilenko, Katherina V.; Zatovsky, Igor V.; Ogorodnyk, Ivan V.; Baumer, Vyacheslav N.; Slobodyanik, Nikolay S.

    2011-01-01

    Single crystals of silver(I) polyphosphate(V), AgPO3, were prepared via a phospho­ric acid melt method using a solution of Ag3PO4 in H3PO4. In comparison with the previous study based on single-crystal Weissenberg photographs [Jost (1961 ▶). Acta Cryst. 14, 779–784], the results were mainly confirmed, but with much higher precision and with all displacement parameters refined anisotropically. The structure is built up from two types of distorted edge- and corner-sharing [AgO5] polyhedra, giving rise to multidirectional ribbons, and from two types of PO4 tetra­hedra linked into meandering chains (PO3)n spreading parallel to the b axis with a repeat unit of four tetra­hedra. The calculated bond-valence sum value of one of the two AgI ions indicates a significant strain of the structure. PMID:21522230

  8. Triclinic modification of diaqua-bis-(5-carb-oxy-1H-imidazole-4-carboxyl-ato-κ(2)N(3),O(4))iron(II).

    Science.gov (United States)

    Ohshima, Eriko; Yoshida, Kazuki; Sugiyama, Kazumasa; Uekusa, Hidehiro

    2012-08-01

    The title compound, [Fe(C(5)H(3)N(2)O(4))(2)(H(2)O)(2)], is a triclinic modification of a monoclinic form recently reported by Du et al. [Acta Cryst. (2011) ▶, E67, m997]. The Fe(II) ion lies at an inversion center and is coordinated by two N and two O atoms from two 5-carb-oxy-1H-imidazole-4-carboxyl-ate ligands in trans positions, together with two water mol-ecules, completing a slightly distorted octahedral coordination. Inter-molecular N-H⋯O hydrogen bonding between the N-H group of the imidazole ring and the deprotonated carboxyl-ate group builds a chain of 5-carb-oxy-1H-imidazole-4-carboxyl-ate anions along the [101] direction. The water molecules form intermolecular hydrogen bonds to O-C and O=C sites of the carboxylate group in adjacent layers.

  9. Redetermined crystal structure of N-(β-carb-oxy-eth-yl)-α-isoleucine.

    Science.gov (United States)

    Chandrarekha, M; Srinivasan, N; Krishnakumar, R V

    2015-09-01

    Redetermination of the crystal structure of N-(β-carb-oxy-eth-yl)-α-isoleucine, C9H18N2O3, reported earlier by Nehls et al. [Acta Cryst. (2013), E69, o172-o173], was undertaken in which the ionization state assigned to the mol-ecule as unionized has been modified as zwitterionic in the present work. Single-crystal X-ray intensity data obtained from freshly grown crystals and freely refining the amino H atoms provide enhanced refinement and structural parameters, particularly the hydrogen-bonding scheme. N-H⋯O hydrogen bonds dominate the inter-molecular inter-actions along with a C-H⋯O hydrogen bond. The inter-molecular inter-action pattern is a three-dimensional network. The structure was refined as a two-component perfect inversion twin.

  10. A third polymorph of 1,4-bis(1H-benzimidazol-2-ylbenzene

    Directory of Open Access Journals (Sweden)

    Wei-Wei Fu

    2014-06-01

    Full Text Available The title compound, C20H14N4, is a new polymorph of the previously reported structures, which were orthorhombic, space group Pbca [Bei et al. (2000. Acta Cryst. C56, 718–719] and monoclinic, space group P21/c [Dudd et al. (2003. Green Chem. 5, 187–192]. The asymmetric unit consists of two independent molecules in which the dihedral angels between the central benzene ring and the outer benzimidazole ring systems are 16.81 (10 and 14.23 (10° in one molecule and 26.09 (10 and 37.29 (10° in the other. In the crystal, molecules are linked by N—H...N and C—H...N hydrogen bonds into a tape running along the c-axis direction.

  11. 5-Methylspiro[indoline-3,7′-[6H,7H,8H]pyrano[3,2-c:5,6-c′]di[1]benzopyran]-2,6′,8′-trione chloroform hemisolvate

    Directory of Open Access Journals (Sweden)

    Abdulrahman I. Almansour

    2012-04-01

    Full Text Available In the title compound, C27H15NO6·0.5CHCl3, the central pyran ring and both the benzopyran systems are planar, with the dihedral angle between the outer rings being 3.24 (6°. The indolin-2-one system is in a perpendicular configuration with respect to the pyran ring [dihedral angle = 87.58 (2°]. Supramolecular layers in the ac plane are formed in the crystal structure whereby inversion-related molecules are connected by N—H...O hydrogen bonds. These are further linked by C—H...O interactions, forming a supramolecular layer in the ac plane. Disordered CHCl3 solvent in the structure was modelled with the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  12. 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...

  13. 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...

  14. (R-2-[(Dimethylaminomethyl]-1,1′-bis(diphenylphosphinothioylferrocene dichloromethane monsolvate

    Directory of Open Access Journals (Sweden)

    Elisabeth Philippe

    2012-06-01

    Full Text Available In the title compound, [Fe(C20H21NPS(C17H14PS]·CH2Cl2, both cyclopentadienyl (Cp rings constituting the ferrocene unit are substituted by a sulfur-protected diphenylphosphine. One of the Cp ligands is additionally substituted by a dimethylaminomethyl group causing the chirality of the molecule. Surprisingly, although the synthetic procedure yielded the title compound as a racemic mixture, the reported crystal is enantiomerically pure with the R absolute configuration. The dimethylamino group is exo with respect to the Cp ring. Both diphenylthiophosphine groups are trans with respect to the centroid–Fe–centroid direction. Weak intramolecular C—H...S and C—H...π interactions between symmetry-related molecules are observed. The contribution of the disordered solvent was removed from the refinement using SQUEEZE in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  15. Bis{2-[(Triphenylmethylamino]phenyl} diselenide acetonitrile monosolvate

    Directory of Open Access Journals (Sweden)

    Adam Neuba

    2014-05-01

    Full Text Available The molecular structure of the title compound, C50H40N2Se2·C2H3N, shows a syn conformation of the benzene rings bound to the Se atoms, with an Se—Se bond length of 2.3529 (6 Å and a C—Se—Se—C torsion angle of 93.53 (14°. The two Se-bonded aromatic ring planes make a dihedral angle of 18.42 (16°. Intramolecular N—H...Se hydrogen bonds are noted. Intermolecular C—H...Se interactions give rise to supramolecular chains extended along [100]. One severely disordered acetonitrile solvent molecule per asymmetric unit was treated with SQUEEZE in PLATON [Spek (2009. Acta Cryst. D65, 148–155]; the crystal data take the presence of this molecule into account.

  16. Na4.25Mo15S19: a novel ternary reduced molybdenum sulfide containing Mo6 and Mo9 clusters

    Directory of Open Access Journals (Sweden)

    D. Salloum

    2014-06-01

    Full Text Available The structure of tetrasodium pentadecamolybdenum nonadecasulfide, Na4.25Mo15S19, is isotypic with Na3.9Mo15Se19 [Salloum et al. (2013. Acta Cryst. E69, i67–i68]. It is characterized by Mo6Si8Sa6 and Mo9Si11Sa6 (where i represents inner and a apical atoms cluster units that are present in a 1:1 ratio. The cluster units are centered at Wyckoff positions 2b and 2c, and have point-group symmetry -3 and -6, respectively. The clusters are interconnected through additional Mo—S bonds. The Na+ cations occupy interunit voids formed by six or seven S atoms. One Mo, one S and one Na site [occupancy 0.751 (12] are situated on mirror planes, and two other S atoms and one Na site (full occupancy are situated on threefold rotation axes.

  17. Reinvestigation of the crystal structure of lautite, CuAsS

    Directory of Open Access Journals (Sweden)

    Paola Bonazzi

    2008-03-01

    Full Text Available The crystal structure of the mineral lautite (copper arsenic sulfide, CuAsS, previously described as either centrosymmetric [Pnma; Marumo & Nowacki (1964. Schweiz. Miner. Petro. Mitt. 44, 439–454] or noncentrosymmetric [Pna21; Craig & Stephenson (1965. Acta Cryst. 19, 543–547], was reinvestigated by means of single-crystal X-ray diffraction. The centrosymmetric structural model reported previously was confirmed, although with improved precision for the atomic coordinates and interatomic distances. Lautite shows a sphalerite-derivative structure with a linking of Cu[AsS3], As[CuAs2S] and S[Cu3As] tetrahedra. All atoms lie on special positions (Wyckoff position 4c, site symmetry m.

  18. Tl2Mo9Se11

    Directory of Open Access Journals (Sweden)

    Patrick Gougeon

    2010-08-01

    Full Text Available The structure of Tl2Mo9Se11, dithallium nonamolybdenum undecaselenide, is isotypic with Tl2Mo9S11 [Potel et al. (1980. Acta Cryst. B36, 1319–1322]. The structural set-up is characterized by a mixture of Mo6Sei8Sea6 and Mo12Sei14Sea6 cluster units in a 1:1 ratio. Both components are interconnected through interunit Mo—Se bonds. The cluster units are centered at Wyckoff positions 3a and 3b (point-group symmetry overline{3}.. The two TlI atoms are situated in the voids of the three-dimensional arrangement. Two of the five independent Se atoms and the Tl atoms lie on sites with 3. symmetry (Wyckoff site 6c.

  19. X-ray structure of Salmonella typhimurium uridine phosphorylase complexed with 5-fluorouracil and molecular modelling of the complex of 5-fluorouracil with uridine phosphorylase from Vibrio cholerae.

    Science.gov (United States)

    Lashkov, Alexander A; Sotnichenko, Sergey E; Prokofiev, Igor I; Gabdulkhakov, Azat G; Agapov, Igor I; Shtil, Alexander A; Betzel, Christian; Mironov, Alexander S; Mikhailov, Al'bert M

    2012-08-01

    Uridine phosphorylase (UPh), which is a key enzyme in the reutilization pathway of pyrimidine nucleoside metabolism, is a validated target for the treatment of infectious diseases and cancer. A detailed analysis of the interactions of UPh with the therapeutic ligand 5-fluorouracil (5-FUra) is important for the rational design of pharmacological inhibitors of these enzymes in prokaryotes and eukaryotes. Expanding on the preliminary analysis of the spatial organization of the active centre of UPh from the pathogenic bacterium Salmonella typhimurium (StUPh) in complex with 5-FUra [Lashkov et al. (2009), Acta Cryst. F65, 601-603], the X-ray structure of the StUPh-5-FUra complex was analysed at atomic resolution and an in silico model of the complex formed by the drug with UPh from Vibrio cholerae (VchUPh) was generated. These results should be considered in the design of selective inhibitors of UPhs from various species.

  20. Crystal structures of two ytterbium(III complexes comprising alkynylamidinate ligands

    Directory of Open Access Journals (Sweden)

    Sida Wang

    2016-09-01

    Full Text Available Two ytterbium(III complexes comprising alkynylamidinate ligands, namely bis(η5-cyclopentadienyl(3-cyclopropyl-N,N′-diisopropylpropynamidinato-κ2N,N′ytterbium(III, [Yb(C5H52(C12H19N2] or Cp2Yb[(iPr2N2C—C[triple-bond]C—c-C3H5] (1 and tris(3-phenyl-N,N′-dicyclohexylpropynamidinato-κ2N,N′ytterbium(III, [Yb(C21H27N23] or Yb[(CyN2C—C[triple-bond]C—Ph]3 (Cy = cyclohexyl (2 have been synthesized and structurally characterized. Both complexes are monomers; for complex 2, the contribution to the scattering from highly disordered toluene solvent molecules in these voids 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.

  1. Crystal structure of bis­[tetra­kis­(tri­phenyl­phosphane-κP)silver(I)] (nitrilo­tri­acetato-κ4 N,O,O′,O′′)(tri­phenyl­phosphane-κP)argentate(I) with an unknown amount of methanol as solvate

    Science.gov (United States)

    Noll, Julian; Korb, Marcus; Lang, Heinrich

    2016-01-01

    The structure of the title compound, [Ag(C18H15P)4]2[Ag(C6H6NO6)(C18H15P)], exhibits trigonal (P-3) symmetry, with a C 3 axis through all three complex ions, resulting in an asymmetric unit that contains one third of the atoms present in the formula unit. The formula unit thus contains two of the cations, one anion and disordered mol­ecules of methanol as the packing solvent. Attempts to refine the solvent model were unsuccessful, indicating uninter­pretable disorder. Thus, the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18] was applied, accounting for 670 electrons per unit cell, representing approximately 18 mol­ecules of methanol in the formula unit. The stated crystal data for M r, μ etc do not take these into account. PMID:27006796

  2. 1,3,5-Tri-p-tolyl­pentane-1,5-diol

    Science.gov (United States)

    Thiruvalluvar, A.; Chithiravel, R.; Muthusubramanian, S.; Butcher, R. J.

    2014-01-01

    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)]. PMID:24764851

  3. 2-(5-Iodo-2-oxoindolin-3-yl­idene)hydrazinecarbo­thio­amide including an unknown solvate

    Science.gov (United States)

    Conceição Duarte de Bittencourt, Viviane; Carratu Gervini, Vanessa; Rosa de Menezes Vicenti, Juliano; Maciel Velasques, Jecika; Jussiane Zambiazi, Priscilla

    2014-01-01

    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. PMID:24940248

  4. The effect of intermolecular forces on diffusion in polymers

    CERN Document Server

    Chatten, R

    2002-01-01

    is proposed that since correlation function integral equation theories capture polymer-penetrant coupling effects the overall diffusion equation requires the simultaneous solution of a correlation function based polymer diffusion equation with only a random motion equation for the penetrant. It is demonstrated that a correlation function based theory is able to incorporate the mechanistic essence of both molecular models and free-volume theories whilst providing the possibility of interpretation of phenomenology at a more detailed level. The permeation of small molecules through polymer materials has been investigated both experimentally and theoretically. Experimentally the permeation of species from a Br sub 2 containing electrolyte through HDPE, LLDPE and PVDF has been examined using novel permeation cells. The effect of polymer and penetrant properties and environmental variables are discussed in conjunction with analyses of observed structural and dynamic features. Penetrant-induced changes such as cryst...

  5. Affinity and its derivatives in the glass transition process

    Science.gov (United States)

    Garden, J.-L.; Guillou, H.; Richard, J.; Wondraczek, L.

    2012-07-01

    The thermodynamic treatment of the glass transition remains an issue of intense debate. When associated with the formalism of non-equilibrium thermodynamics, the lattice-hole theory of liquids can provide new insight in this direction, as has been shown by Schmelzer and Gutzow [J. Chem. Phys. 125, 184511 (2006)], 10.1063/1.2374894, by Möller et al. [J. Chem. Phys. 125, 094505 (2006)], 10.1063/1.2346673, and more recently by Tropin et al. [J. Non-Cryst. Solids 357, 1291 (2011), 10.1016/j.jnoncrysol.2010.11.111; Tropin et al., J. Non-Cryst. Solids 357, 1303 (2011)], 10.1016/j.jnoncrysol.2010.12.005. Here, we employ a similar approach. We include pressure as an additional variable, in order to account for the freezing-in of structural degrees of freedom upon pressure increase. Second, we demonstrate that important terms concerning first order derivatives of the affinity-driving-force with respect to temperature and pressure have been previously neglected. We show that these are of crucial importance in the approach. Macroscopic non-equilibrium thermodynamics is used to enlighten these contributions in the derivation of Cp,κT, and αp. The coefficients are calculated as a function of pressure and temperature following different theoretical protocols, revealing classical aspects of vitrification and structural recovery processes. Finally, we demonstrate that a simple minimalist model such as the lattice-hole theory of liquids, when being associated with rigorous use of macroscopic non-equilibrium thermodynamics, is able to account for the primary features of the glass transition phenomenology. Notwithstanding its simplicity and its limits, this approach can be used as a very pedagogical tool to provide a physical understanding on the underlying thermodynamics which governs the glass transition process.

  6. An approximation of the Cioslowski-Mixon bond order indexes using the AlteQ approach

    Science.gov (United States)

    Salmina, Elena; Grishina, Maria A.; Potemkin, Vladimir A.

    2013-09-01

    Fast and reliable prediction of bond orders in organic systems based upon experimentally measured quantities can be performed using electron density features at bond critical points (J Am Chem Soc 105:5061-5068, 1983; J Phys Org Chem 16:133-141, 2003; Acta Cryst B 61:418-428, 2005; Acta Cryst B 63:142-150, 2007). These features are outcomes of low-temperature high-resolution X-ray diffraction experiments. However, a time-consuming procedure of gaining these quantities makes the prediction limited. In the present work we have employed an empirical approach AlteQ (J Comput Aided Mol Des 22:489-505, 2008) for evaluation of electron density properties. This approach uses a simple exponential function derived from comparison of electron density, gained from high-resolution X-ray crystallography, and distance to atomic nucleus what allows calculating density distribution in time-saving manner and gives results which are very close to experimental ones. As input data AlteQ accepts atomic coordinates of isolated molecules or molecular ensembles (for instance, protein-protein complexes or complexes of small molecules with proteins, etc.). Using AlteQ characteristics we have developed regression models predicting Cioslowski-Mixon bond order (CMBO) indexes (J Am Chem Soc 113(42):4142-4145, 1991). The models are characterized by high correlation coefficients lying in the range from 0.844 to 0.988 dependently on the type of covalent bond, thereby providing a bonding quantification that is in reasonable agreement with that obtained by orbital theory. Comparative analysis of CMBOs approximated using topological properties of AlteQ and experimental electron densities has shown that the models can be used for fast determination of bond orders directly from X-ray crystallography data and confirmed that AlteQ characteristics can replace experimental ones with satisfactory extent of accuracy.

  7. 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.

  8. The Study of Wipe off Magnesium in Phosphoric Acid Solution by Means of Liq-uid Membrane Technique%液膜分离技术净化湿法磷酸中的镁离子

    Institute of Scientific and Technical Information of China (English)

    高枫; 王帮贺; 汤德元

    2004-01-01

    镁离子是湿法磷酸中有害杂质之一,采用正交实验的方法,对湿法磷酸中除镁的液膜物质进行筛选,通过对实验数据处理和分析,得到了除去湿法磷酸中镁离子的最佳工艺条件:表面活性剂:L113A,膜试剂:环己烷,萃取剂:P204,反萃取剂:HCl3 mol/L,增稠剂:石蜡量0.5 mL,萃取剂量:0.5 mL.

  9. X-Ray Data on Extraterrestrial CA Dialuminate (CaAl4O7)

    Science.gov (United States)

    Weber, D.; Ross, C. R., II; Bischoff, A.

    1993-07-01

    volume, are slightly higher in Ca-dialuminate from Acfer 182 than from synthetic CaAl4O7. This may be due to the incorporation of traces of refractory elements (REE) with large ionic radii, which were analyzed within inclusion 022/9 [10]. With the determination of the cell constants of natural Ca-dialuminate combined with data on synthetic CaAl4O7, sufficient X-ray data should be available required to nominate this mineral. References: [1] Christophe Michel-Levy M. et al. (1982) EPSL, 61, 13-22. [2] Kimura M. et al. (1993) GCA, in press. [3] Weber D. and Bischoff A. (1992) Meteoritics, 27, 304-305. [4] Weber D. and Bischoff A. (1993) GCA, submitted. [5] Boyko E. R. and Wisnyi L. G. (1958) Acta Cryst., 11, 444-445. [6] Goodwin D. W. and Lindop A. J. (1970) Acta Cryst., B26, 1230-1235. [7] Baldock P. J. et al. (1970) J. Appl. Cryst., 3, 188-191. [8] Geiger C. A. et al. (1988) GCA, 52, 1729-1736. [9] Gross S. (1977) Geol. Surv. Israel Bull. 70, 1-80. [10] Bischoff A. et al. (1992) Meteoritics, 27, 204. Table 1, which appears in the hard copy, shows unit-cell constants of Ca- dialuminate (monocline; space group C2/c) and X-ray powder diffraction data (CrK-alpha (Ni-beta), 45 kV, 30 mA) on extraterrestrial CaAl4O7 in comparison to JCPDS data [7]. Numbers in parentheses are uncertainties in last significant figures.

  10. 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

  11. Effect of phase transformations on microstructures in deep mantle materials

    Science.gov (United States)

    Merkel, Sébastien; Langrand, Christopher; Rosa, Angelika; Hilairet, Nadège

    2017-04-01

    árik, Vaughan, Merkel, Reliability of Multigrain Indexing for Orthorhombic Polycrystals above 1 Mbar: Application to MgSiO3-Post-Perovskite, J Appl Cryst 50, in press (2017) Rosa, Hilairet, Ghosh, Garbarino, Jacobs, Perrillat, Vaughan, Merkel, In situ monitoring of phase transformation microstructures at Earth's mantle pressure and temperature using multi-grain XRD, J Appl Cryst 48, 1346-1354 (2015) Rosa, Hilairet, Ghosh, Perrillat, Garbarino, Merkel, Evolution of grain sizes and orientations during phase transitions in hydrous Mg2SiO4, J Geophys Res 121, 7161-7176 (2016)

  12. Chloro(L-glutamato-kappa 2N,O)(1,10-phenanthroline-kappa 2,N')copper(II) monohydrate.

    Science.gov (United States)

    Lu, Li-Ping; Zhu, Miao-Li; Yang, Pin

    2004-01-01

    The crystal structure of the title compound, [CuCl(C(5)H(8)NO(4))(C(12)H(8)N(2))].H(2)O or [CuCl(L-Glu)(phen)].H(2)O (where phen is 1,10-phenanthroline and L-Glu is L-glutamate), shows that the ternary complex consists of two neutral molecules, in which the Cu(II) ions each have a distorted square-pyramidal coordination geometry comprised of one bidentate phenanthroline ligand, one O,N-bidentate L-glutamate anion and an apical Cl(-) anion. The angles between the planes of the Cu-phenanthroline and the Cu-aminocarboxylate chelate rings are 6.1 (5) and 11.8 (5) degrees in the two molecules. The Cu-Cl bond lengths are 2.608 (3) and 2.590 (3) A in the two molecules, slightly longer than the value of 2.546 A observed for the Cu-Cl bond in the analogous chloro(L-glycinato)(1,10-phenanthroline)copper complex [Solans, Ruiz-Ramírez, Martinez, Gasque & Briansó (1983). Acta Cryst. C44, 628-631]. Additionally, the Cu ion is weakly coordinated at a sixth position by an alpha-carboxyl O atom from a neighbouring complex. A number of intra- and intermolecular hydrogen bonds stabilize the crystal structure.

  13. 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.

  14. Structure and dynamics of iron doped and undoped silicate glasses

    Science.gov (United States)

    Santos, Cristiane N.; Meneses, Domingos D. S.; Echegut, Patrick; Lecomte, Emmanuel

    2010-03-01

    The optical properties of common silicate glass compositions are well known at room temperature. However, their radiative properties and structural evolution of these glasses with temperature are still largely unexplored. In this work we have measured the emissivity of a set of iron doped and undoped silicate and borosilicate glasses over an unprecedented temperature (up to 1700 K) and spectral range (40 -- 20000 cm-1). This was achieved by means of a home-made apparatus composed of a CO2 laser as the heat source, a black-body reference and two spectrometers. The optical functions were assessed using a dielectric function model [1], and the structure and dynamics of the glassy network, as well the absorption of iron species in different redox states were evidenced. We believe that these new data will help to understand the heat transfer in molten silicates. [4pt] [1] D. D. S. Meneses, G. Gruener, M. Malki, and P. Echegut, J. Non-Cryst. Solids 351, 124 (2005)

  15. 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.

  16. 2,4-Bis(4-ethoxyphenyl-7-methyl-3-azabicyclo[3.3.1]nonan-9-one

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    V. Ramkumar

    2012-03-01

    Full Text Available The molecule of the title compound, C25H31NO3, exists in a twin-chair conformation with an equatorial orientation of the 4-ethoxyphenyl groups, as observed for its ortho isomer [Parthiban, Ramkumar, Park & Jeong (2011b, Acta Cryst. E67, o1475–o1476]. The methyl and 4-ethoxyphenyl groups are also equatorially oriented on the bicycle, as in the ortho analogue. In particular, although the cyclohexanone ring deviates from an ideal chair, the piperidone ring is closer to an ideal chair, whereas in the ortho isomer both rings are significantly puckered and deviate from ideal chairs. The 4-ethoxyphenyl groups on both sides of the secondary amine group are oriented at an angle of 26.11 (3° with respect to each other, but the 2-ethoxyphenyl groups in the ortho isomer are oriented by less than half this [12.41 (4°]. In contrast to the absence of any significant interactions in the crystal packing of the ortho isomer, the title compound features N—H...O interactions, linking the molecules along the b axis.

  17. Bis[2-(hy-droxy-imino-meth-yl)phenolato]nickel(II): a second monoclinic polymorph.

    Science.gov (United States)

    Rusanova, Julia A; Buvaylo, Elena A; Rusanov, Eduard B

    2011-01-15

    The title compound, [Ni(C(7)H(6)NO(2))(2)], (I), is a second monoclinic polymorph of the compound, (II), reported by Srivastava et al. [Acta Cryst. (1967), 22, 922] and Mereiter [Private communication (2002) CCDC refcode NISALO01]. The bond lengths and angles are similar in both structures. The mol-ecule in both structures lies on a crystallographic inversion center and both have an inter-nal hydrogen bond. The title compound crystallizes in the space group P2(1)/c (Z = 2), whereas compound (II) is in the space group P2(1)/n (Z = 2) with a similar cell volume but different cell parameters. In both polymorphs, mol-ecules are arranged in the layers but in contrast to the previously published compound (II) where the dihedral angle between the layers is 86.3°, in the title polymorph the same dihedral angle is 29.4°. The structure of (I) is stabilized by strong intra-molecular O-H⋯O hydrogen bonding between the O-H group and the phenolate O atom.

  18. Bis[2-(hydroxyiminomethylphenolato]nickel(II: a second monoclinic polymorph

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    Julia A. Rusanova

    2011-02-01

    Full Text Available The title compound, [Ni(C7H6NO22], (I, is a second monoclinic polymorph of the compound, (II, reported by Srivastava et al. [Acta Cryst. (1967, 22, 922] and Mereiter [Private communication (2002 CCDC refcode NISALO01]. The bond lengths and angles are similar in both structures. The molecule in both structures lies on a crystallographic inversion center and both have an internal hydrogen bond. The title compound crystallizes in the space group P21/c (Z = 2, whereas compound (II is in the space group P21/n (Z = 2 with a similar cell volume but different cell parameters. In both polymorphs, molecules are arranged in the layers but in contrast to the previously published compound (II where the dihedral angle between the layers is 86.3°, in the title polymorph the same dihedral angle is 29.4°. The structure of (I is stabilized by strong intramolecular O—H...O hydrogen bonding between the O—H group and the phenolate O atom.

  19. Does mathematical crystallography still have a role in the XXI century?

    Science.gov (United States)

    Nespolo, Massimo

    2008-01-01

    Mathematical crystallography is the branch of crystallography dealing specifically with the fundamental properties of symmetry and periodicity of crystals, topological properties of crystal structures, twins, modular and modulated structures, polytypes and OD structures, as well as the symmetry aspects of phase transitions and physical properties of crystals. Mathematical crystallography has had its most evident success with the development of the theory of space groups at the end of the XIX century; since then, it has greatly enlarged its applications, but crystallographers are not always familiar with the developments that followed, partly because the applications sometimes require some additional background that the structural crystallographer does not always possess (as is the case, for example, in graph theory). The knowledge offered by mathematical crystallography is at present only partly mirrored in International Tables for Crystallography and is sometimes still enshrined in more specialist texts and publications. To cover this communication gap is one of the tasks of the IUCr Commission on Mathematical and Theoretical Crystallography (MaThCryst).

  20. Nomenclature of magnetic, incommensurate, composition-changed morphotropic, polytype, transient-structural and quasicrystalline phases undergoing phase transitions. II. Report of an IUCr Working Group on Phase Transition Nomenclature.

    Science.gov (United States)

    Tolédano, J C; Berry, R S; Brown, P J; Glazer, A M; Metselaar, R; Pandey, D; Perez-Mato, J M; Roth, R S; Abrahams, S C

    2001-09-01

    A general nomenclature applicable to the phases that form in any sequence of transitions in the solid state has been recommended by an IUCr Working Group [Acta Cryst. (1998). A54, 1028-1033]. The six-field notation of the first Report, hereafter I, was applied to the case of structural phase transitions, i.e. to transformations resulting from temperature and/or pressure changes between two crystalline (strictly periodic) phases involving modifications to the atomic arrangement. Extensive examples that illustrate the recommendations were provided. This second Report considers, within the framework of a similar six-field notation, the more complex nomenclature of transitions involving magnetic phases, incommensurate phases and transitions that occur as a function of composition change. Extension of the nomenclature to the case of phases with less clearly established relevance to standard schemes of transition in equilibrium systems, namely polytype phases, radiation-induced and other transient phases, quasicrystalline phases and their transitions is recommended more tentatively. A uniform notation for the translational periodicity, propagation vector or wavevector for magnetic and/or incommensurate substances is specified. The notation adopted for incommensurate phases, relying partly on the existence of an average structure, is also consistent with that for commensurate phases in a sequence. The sixth field of the nomenclature is used to emphasize the special features of polytypes and transient phases. As in I, illustrative examples are provided for each category of phase sequence.

  1. Crystal families and systems in higher dimensions, and geometrical symbols of their point groups. I. Crystal families in five-dimensional space with two-, three-, four- and sixfold symmetries.

    Science.gov (United States)

    Veysseyre, R; Weigel, D; Phan, Th

    2008-11-01

    The aim of this paper and of the following one [Weigel, Phan & Veysseyre (2008). Acta Cryst. A64, 687-697] is to complete the list of the Weigel-Phan-Veysseyre (WPV) symbols of the point groups of space E5 that was started in previous papers and in two reports of an IUCr Subcommittee on the Nomenclature of n-Dimensional Crystallography. In this paper, some crystal families of space E5 are studied. The cells of these are right hyperprisms with as a basis either two squares, or two hexagons, or a square and a hexagon. If the basis is made up of two squares, the two families are the (monoclinic di squares)-al family (No. XVI) and the (di squares)-al family (No. XIX). If the basis is made up of two hexagons, the two families are the (monoclinic di hexagons)-al family (No. XVII) and the (di hexagons)-al family (No. XXI). If the basis is made up of one square and one hexagon, the family is the (square hexagon)-al family (No. XX). In order to link space E5 to spaces E2, E3 and E4, some results published in previous papers are recalled. In fact, most of the symbols of the point groups of space E5 can be deduced from the symbols of the four, six and 23 crystal families of spaces E2, E3 and E4, respectively.

  2. 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.

  3. Rappertk: a versatile engine for discrete restraint-based conformational sampling of macromolecules

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    Karmali Anjum M

    2007-03-01

    Full Text Available Abstract Background Macromolecular structures are modeled by conformational optimization within experimental and knowledge-based restraints. Discrete restraint-based sampling generates high-quality structures within these restraints and facilitates further refinement in a continuous all-atom energy landscape. This approach has been used successfully for protein loop modeling, comparative modeling and electron density fitting in X-ray crystallography. Results Here we present a software toolkit (Rappertk which generalizes discrete restraint-based sampling for use in structural biology. Modular design and multi-layered architecture enables Rappertk to sample conformations of any macromolecule at many levels of detail and within a variety of experimental restraints. Performance against a Cα-tracing benchmark shows that the efficiency has not suffered despite the overhead required by this flexibility. We demonstrate the toolkit's capabilities by building high-quality β-sheets and by introducing restraint-driven sampling. RNA sampling is demonstrated by rebuilding a protein-RNA interface. Ability to construct arbitrary ligands is used in sampling protein-ligand interfaces within electron density. Finally, secondary structure and shape information derived from EM are combined to generate multiple conformations of a protein consistent with the observed density. Conclusion Through its modular design and ease of use, Rappertk enables exploration of a wide variety of interesting avenues in structural biology. This toolkit, with illustrative examples, is freely available to academic users from http://www-cryst.bioc.cam.ac.uk/~swanand/mysite/rtk/index.html.

  4. 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.

  5. Crystal structure of lead(II tartrate: a redetermination

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    Matthias Weil

    2015-01-01

    Full Text Available Single crystals of poly[μ4-tartrato-κ6O1,O3:O1′:O2,O4:O4′-lead], [Pb(C4H4O6]n, were grown in a gel medium. In comparison with the previous structure determination of this compound from laboratory powder X-ray diffraction data [De Ridder et al. (2002. Acta Cryst. C58, m596–m598], the redetermination on the basis of single-crystal data reveals the absolute structure, all atoms with anisotropic displacement parameters and a much higher accuracy in terms of bond lengths and angles. It could be shown that a different space group or incorporation of water as reported for similarly gel-grown lead tartrate crystals is incorrect. In the structure, each Pb2+ cation is bonded to eight O atoms of five tartrate anions, while each tartrate anion links four Pb2+ cations. The resulting three-dimensional framework is stabilized by O—H...O hydrogen bonds between the OH groups of one tartrate anion and the carboxylate O atoms of adjacent anions.

  6. Probability density functions of the average and difference intensities of Friedel opposites.

    Science.gov (United States)

    Shmueli, U; Flack, H D

    2010-11-01

    Trigonometric series for the average (A) and difference (D) intensities of Friedel opposites were carefully rederived and were normalized to minimize their dependence on sin(theta)/lambda. Probability density functions (hereafter p.d.f.s) of these series were then derived by the Fourier method [Shmueli, Weiss, Kiefer & Wilson (1984). Acta Cryst. A40, 651-660] and their expressions, which admit any chemical composition of the unit-cell contents, were obtained for the space group P1. Histograms of A and D were then calculated for an assumed random-structure model and for 3135 Friedel pairs of a published solved crystal structure, and were compared with the p.d.f.s after the latter were scaled up to the histograms. Good agreement was obtained for the random-structure model and a qualitative one for the published solved structure. The results indicate that the residual discrepancy is mainly due to the presumed statistical independence of the p.d.f.'s characteristic function on the contributions of the interatomic vectors.

  7. Pharmacokinetics of Peramivir in an Adolescent Patient Receiving Continuous Venovenous Hemodiafiltration.

    Science.gov (United States)

    Dillon, Ryan C; Witcher, Robert; Cies, Jeffrey J; Moore, Wayne S; Chopra, Arun

    2017-01-01

    Critically ill patients requiring renal replacement therapy commonly experience pharmacokinetic alterations. This case report describes the pharmacokinetics of peramivir (Rapivab, BioCryst Pharmaceuticals, Inc, Durham, NC), the first US Food and Drug Administration-approved intravenous neuraminidase inhibitor for the treatment of influenza, in an adolescent patient receiving continuous renal replacement therapy (CRRT). A 49.5-kg, 17-year-old Caucasian female presented with fever, cough, and persistent hypoxia. She quickly progressed to acute respiratory and renal failure in the setting of viral septic shock as a result of a severe influenza H1N1 infection. On hospital day 3, therapy was switched from oseltamivir (Tamiflu, Roche Laboratories Inc, Nutley, NJ) to peramivir owing to the concern for inadequate enteral absorption. On the third day of peramivir treatment, at a dose of 200 mg daily, peramivir serum concentrations revealed a smaller peak concentration, larger volumes of distribution, similar 24-hour area under the curve, and a shorter half-life as compared to adult patients with normal renal function. This illustrated the significant differences in pharmacokinetics when administered in the setting of CRRT. The patient had resolution of viral infection as evidenced by negative respiratory viral panel polymerase chain reaction at hospital day 14 and was eventually discharged at her baseline.

  8. Crystal structure of tri-aqua-(2,6-di-methyl-pyrazine-κN (4))bis-(thio-cyanato-κN)manganese(II) 2,5-di-methyl-pyrazine disolvate.

    Science.gov (United States)

    Suckert, Stefan; Wöhlert, Susanne; Jess, Inke; Näther, Christian

    2015-12-01

    In the crystal structure of the title complex, [Mn(NCS)2(C6H8N2)(H2O)3]·2C6H8N2, the Mn(II) cation is coordinated by two terminally N-bonded thio-cyanate anions, three water mol-ecules and one 2,6-di-methyl-pyrazine ligand within a slightly distorted N3O3 octa-hedral geometry; the entire complex mol-ecule is generated by the application of a twofold rotation axis. The asymmetric unit also contains an uncoordinating 2,5-di-methyl-pyrazine ligand in a general position. Obviously, the coordination to the 2,6-di-methyl-pyrazine ligand is preferred because coordination to the 2,5-di-methyl-pyrazine 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-di-methyl-pyzazine/2,5-di-methyl-pyza-zine) hydrogen bonding, forming a three-dimensional network. In the crystal, mol-ecules 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.

  9. (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].

  10. Crystal structure of 4-methyl-N-{(E-methyl[(3aR,8aS-2-oxo-3,3a,8,8a-tetrahydro-2H-indeno[1,2-d][1,3]oxazol-3-yl]-λ4-sulfanylidene}benzenesulfonamide

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    Patrícia A. Pereira

    2015-12-01

    Full Text Available The formulation that the title compound, C18H18N2O4S2, adopts is a zwitterionic core with the charge separated to the sulfilimine S and N atoms and is supported by the two different S—N bond distances about the sulfinimine N atom [1.594 (2 and 1.631 (2 Å, respectively] that are typical for such bonds. The notably unusual bond is S—N(oxazolidinone [1.692 (2 Å] that is longer than a typical S—N bond [1.603 (18 Å, Mogul analysis; Macrae et al. (2008. J. Appl. Cryst. 41, 466–470]. The bond-angle sum about sulfilimine sulfur (308.35° reflects the trigonal–pyramidal geometry of this atom. Two of the angles are less than 100°. Despite the pyramidalization of this sulfur, there are no significant intermolecular interactions, beyond usual van der Waals contacts, in the crystal packing.

  11. 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].

  12. An ortho-rhom-bic polymorph of N (1),N (4)-diphenyl-3,6-bis-(phenyl-imino)-cyclo-hexa-1,4-diene-1,4-di-amine.

    Science.gov (United States)

    Ohno, Keiji; Fujihara, Takashi; Nagasawa, Akira

    2014-04-01

    A new ortho-rhom-bic polymorph of the title compound, C30H24N4, with a density of 1.315 Mg m(-3), has been obtained. The mol-ecule is centrosymmetric with the centroid of the cyclo-hexa-1,4-diene ring located on an inversion center. The two unique benzene rings are almost perpendicular to each other [dihedral angle = 86.70 (6)°] and are oriented at dihedral angles of 30.79 (5) and 68.07 (5)° with respect to the central cyclo-hexa-diene ring. In the crystal, π-π stacking is observed between the central cyclo-hexa-1,4-diene-1,4-di-amine unit and a phenyl ring of a neighboring mol-ecule [centroid-centroid distance = 3.7043 (7) Å]. The crystal structure of the triclinic polymorph [Ohno et al. (2014 ▶). Acta Cryst. E70, o303-o304] showed chains running along the b-axis direction through weak C-H⋯π inter-actions.

  13. Efficient Exciton Transfer from In0.35Ga0.65As Template into InAs Quantum Dots Grown on GaAs (311)B Substrates

    Institute of Scientific and Technical Information of China (English)

    WANG Fang-Zhen; CHEN Zhang-Hai; GONG Qian; R. N(o)tzel; BAI Li-Hui; SHEN Xue-Chu

    2006-01-01

    @@ Atomic force microscopy (AFM) and power-dependent micro-photoluminescence (μ-PL) spectroscopy are used to study the structure and exciton energy states in InAs quantum dots (QDs) grown on an In0.35 Ga0.65As template on GaAs (311)B. The In0.35Ga0.65As template, consisting of a two-dimensionally modulated layer of closely packed connected cells, has a remarkable effect on the optical properties of the InAs QDs. By comparing the emission spectra of the samples without and with InAs QDs and the work carried out by Gong et al. [J. Cryst.Growth 251 (2003) 150; Appl. Phys. Lett. 81 (2002) 3254] we conclude that the existence of the In0.35Ga0.65As template enhances the photo-absorption and therefore the exciton emission from the QDs due to efficient exciton transfer from the template into the QDs. Furthermore, the PL emission from the QDs clearly reveals four discrete energy levels, S, P, D, and F with increasing excitation power.

  14. Crystal structure of ethyl 3-amino-6-methyl-2-[(4-methylphenylcarbamoyl]-4-[(E-2-phenylethenyl]thieno[2,3-b]pyridine-5-carboxylate monohydrate

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    Joel T. Mague

    2016-03-01

    Full Text Available In the title molecule, C27H25N3O3S·H2O, the dihedral angle between the planes of the thienyl ring and the pendant p-tolyl group is 39.25 (6°, while that between the pyridine ring and the pendant phenyl ring is 44.37 (6°. In addition, there is a slight twist in the bicyclic core, with a dihedral angle of 2.39 (4° between the thienyl and pyridine rings. The conformation of the carbamoyl moiety is partially determined by an intramolecular N—H...O hydrogen bond. In the crystal, complementary N—H...O hydrogen bonds form dimers which are then associated into chains parallel to the c axis through O—H...N hydrogen bonds involving the water molecule of crystallization. Electron density associated with an additional solvent molecule of partial occupancy and disordered about a twofold axis was removed with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s.

  15. Facilitating model reconstruction for single-particle scattering using small-angle X-ray scattering methods.

    Science.gov (United States)

    Ma, Shufen; Liu, Haiguang

    2016-04-01

    X-ray free-electron lasers generate intense femtosecond X-ray pulses, so that high-resolution structure determination becomes feasible from noncrystalline samples, such as single particles or single molecules. At the moment, the orientation of sample particles cannot be precisely controlled, and consequently the unknown orientation needs to be recovered using computational algorithms. This delays the model reconstruction until all the scattering patterns have been re-oriented, which often entails a long elapse of time and until the completion of the experiment. The scattering patterns from single particles or multiple particles can be summed to form a virtual powder diffraction pattern, and the low-resolution region, corresponding to the small-angle X-ray scattering (SAXS) regime, can be analysed using existing SAXS methods. This work presents a pipeline that converts single-particle data sets into SAXS data, from which real-time model reconstruction is achieved using the model retrieval approach implemented in the software package SASTBX [Liu, Hexemer & Zwart (2012). J. Appl. Cryst.45, 587-593]. To illustrate the applications, two case studies are presented with real experimental data sets collected at the Linac Coherent Light Source.

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

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    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.

  17. Etude structurale et vibrationnelle d'un nouveau composé complexe de cobalt: [Co(imidazole4Cl]Cl

    Directory of Open Access Journals (Sweden)

    Amira Derbel

    2015-10-01

    Full Text Available In the title complex, chloridotetrakis(1H-imidazole-κN3cobalt(II chloride, [CoCl(C3H4N24]Cl, the CoII 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(Im4Cl]Cl [Morzyk-Ociepa et al. (2012. J. Mol. Struct. 1028, 49–56] and [Cu(Im4Br]Br [Hossaini Sadr et al. (2004. Acta Cryst. E60, m1324–m1326]. In the crystal, the [CoCl(C3H4N24]+ 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] interactions, 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 orthorhombic 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.

  18. A log-likelihood-gain intensity target for crystallographic phasing that accounts for experimental error.

    Science.gov (United States)

    Read, Randy J; McCoy, Airlie J

    2016-03-01

    The crystallographic diffraction experiment measures Bragg intensities; crystallographic electron-density maps and other crystallographic calculations in phasing require structure-factor amplitudes. If data were measured with no errors, the structure-factor amplitudes would be trivially proportional to the square roots of the intensities. When the experimental errors are large, and especially when random errors yield negative net intensities, the conversion of intensities and their error estimates into amplitudes and associated error estimates becomes nontrivial. Although this problem has been addressed intermittently in the history of crystallographic phasing, current approaches to accounting for experimental errors in macromolecular crystallography have numerous significant defects. These have been addressed with the formulation of LLGI, a log-likelihood-gain function in terms of the Bragg intensities and their associated experimental error estimates. LLGI has the correct asymptotic behaviour for data with large experimental error, appropriately downweighting these reflections without introducing bias. LLGI abrogates the need for the conversion of intensity data to amplitudes, which is usually performed with the French and Wilson method [French & Wilson (1978), Acta Cryst. A35, 517-525], wherever likelihood target functions are required. It has general applicability for a wide variety of algorithms in macromolecular crystallography, including scaling, characterizing anisotropy and translational noncrystallographic symmetry, detecting outliers, experimental phasing, molecular replacement and refinement. Because it is impossible to reliably recover the original intensity data from amplitudes, it is suggested that crystallographers should always deposit the intensity data in the Protein Data Bank.

  19. Crystal structure of di-chlorido-(2,2':6',2''-terpyridine-κ(3) N,N',N'')zinc: a redeter-min-ation.

    Science.gov (United States)

    Kong, Cheng-Cheng; Zhou, Jia-Zheng; Yu, Jian-Hua; Li, Sheng-Li

    2014-11-01

    The crystal structure of the title compound, [ZnCl2(C15H11N3)], was redetermined based on modern CCD data. In comparison with the previous determination from photographic film data [Corbridge & Cox (1956 ▶). J. Chem. Soc. 159, 594-603; Einstein & Penfold (1966 ▶). Acta Cryst. 20, 924-926], all non-H atoms were refined with anisotropic displacement parameters, leading to a much higher precision in terms of bond lengths and angles [e.g. Zn-Cl = 2.2684 (8) and 2.2883 (11) compared to 2.25 (1) and 2.27 (1) Å]. In the title mol-ecule, the Zn(II) atom is five-coordinated in a distorted square-pyramidal mode by two Cl atoms and by the three N atoms from the 2,2':6',2''-terpyridine ligand. The latter is not planar and shows dihedral angles between the least-squares planes of the central pyridine ring and the terminal rings of 3.18 (8) and 6.36 (9)°. The mol-ecules in the crystal structure pack with π-π inter-actions [centroid-centroid distance = 3.655 (2) Å] between pyridine rings of neighbouring terpyridine moieties. These, together with inter-molecular C-H⋯Cl inter-actions, stablize the three-dimensional structure.

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

    Science.gov (United States)

    Li, Xiaozhou; Bond, Andrew D; Johansson, Kristoffer E; Van de Streek, Jacco

    2014-08-01

    The crystal structure of the title compound, C11H13N3O2S2, has been determined previously on the basis of refinement against laboratory powder X-ray diffraction (PXRD) data, supported by comparison of measured and calculated (13)C solid-state NMR spectra [Hangan et al. (2010). Acta Cryst. B66, 615-621]. The molecule is tautomeric, and was reported as an amine tautomer [systematic name: N-(5-ethyl-1,3,4-thiadiazol-2-yl)-p-toluenesulfonamide], rather than the correct imine tautomer. The protonation site on the molecule's 1,3,4-thiadiazole ring is indicated by the intermolecular 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 intermolecular interactions. 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 quantitative 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 (13)C SS-NMR spectrum based on the correct imine tautomer also provides considerably better agreement with the measured (13)C SS-NMR spectrum.

  1. Interfacial instabilities in directional solidification of dilute binary alloys: The Kuramoto-Sivashinsky equation

    Science.gov (United States)

    Novick-Cohen, A.

    1987-05-01

    Directional solidification processes in the presence of an impurity are studied in the limit in which the dimensionless parameter overlineW = {GD}/{VC}0( g + ⨍ c) is small. Here G is the imposed temperature gradient, D is the diffusion coefficient of the impurity, V is the imposed transport velocity, g is equal to minus the slope of the liquidus line, C0 is the impurity concentration at the liquid side of a planar interface, and ⨍ c is a coefficient reflecting deviations from local thermal equilibrium. The dynamics of interfacial kinetics becomes important in this limit and the phenomenological model of Coriell and Sekerka [J. Cryst. Growth 61 (1983) 499-508] is used to model these processes. In this limit, the Kuramoto-Sivashinsky equation is shown to be an asymptotically valid description of the interfacial dynamics. The Kuramoto-Sivashinsky equation is known to exhibit intermittancy superimposed on a relatively stable array of cusps or wrinkles [Michelson and Sivashinsky, Acta Astronautica 4 (1977) 1207-1221] and thus may give a reasonable limiting description of the solidification interface just before coherency is lost. These cusps may also be important in the initiation of dendritic growth by serving as defect points [Schaefer and Glicksman, Met. Trans. 1 (1970) 1973-1978].

  2. Structure of Physarum polycephalum cytochrome b{sub 5} reductase at 1.56 Å resolution

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Sangwoo; Suga, Michihiro; Ogasahara, Kyoko [Institute for Protein Research, Osaka University, 3-2 Yamada-oka, Suita, Osaka (Japan); Ikegami, Terumi; Minami, Yoshiko; Yubisui, Toshitsugu [Department of Biochemistry, Okayama University of Science, 1-1 Ridai-cho, Okayama 700-0005 (Japan); Tsukihara, Tomitake, E-mail: tsuki@protein.osaka-u.ac.jp [Institute for Protein Research, Osaka University, 3-2 Yamada-oka, Suita, Osaka (Japan)

    2007-04-01

    The structure of P. polycephalum cytochrome b{sub 5} reductase, an enzyme which catalyzes the reduction of cytochrome b{sub 5} by NADH, was determined at a resolution of 1.56 Å. Physarum polycephalum cytochrome b{sub 5} reductase catalyzes the reduction of cytochrome b{sub 5} by NADH. The structure of P. polycephalum cytochrome b{sub 5} reductase was determined at a resolution of 1.56 Å. The molecular structure was compared with that of human cytochrome b{sub 5} reductase, which had previously been determined at 1.75 Å resolution [Bando et al. (2004 ▶), Acta Cryst. D60, 1929–1934]. The high-resolution structure revealed conformational differences between the two enzymes in the adenosine moiety of the FAD, the lid region and the linker region. The structural properties of both proteins were inspected in terms of hydrogen bonding, ion pairs, accessible surface area and cavity volume. The differences in these structural properties between the two proteins were consistent with estimates of their thermostabilities obtained from differential scanning calorimetry data.

  3. Acanthamoeba polyphaga mimivirus NDK: preliminary crystallographic analysis of the first viral nucleoside diphosphate kinase

    Energy Technology Data Exchange (ETDEWEB)

    Jeudy, Sandra [Information Génomique et Structurale, CNRS UPR 2589, 31 Chemin Joseph Aiguier, 13402 Marseille CEDEX 20 (France); Coutard, Bruno [Architecture et Fonction des Macromolecules Biologiques, CNRS UMR 6098, 31 Chemin Joseph Aiguier, 13402 Marseille CEDEX 20 (France); Lebrun, Régine [IBSM, 31 Chemin Joseph Aiguier, 13402 Marseille CEDEX 20 (France); Abergel, Chantal, E-mail: chantal.abergel@igs.cnrs-mrs.fr [Information Génomique et Structurale, CNRS UPR 2589, 31 Chemin Joseph Aiguier, 13402 Marseille CEDEX 20 (France)

    2005-06-01

    A. polyphaga mimivirus, the largest known double-stranded DNA virus, is the first virus to exhibit a nucleoside diphosphate kinase gene. The expression and crystallization of the viral NDK are reported. The complete sequence of the largest known double-stranded DNA virus, Acanthamoeba polyphaga mimivirus, has recently been determined [Raoult et al. (2004 ▶), Science, 306, 1344–1350] and revealed numerous genes not expected to be found in a virus. A comprehensive structural and functional study of these gene products was initiated [Abergel et al. (2005 ▶), Acta Cryst. F61, 212–215] both to better understand their role in the virus physiology and to obtain some clues to the origin of DNA viruses. Here, the preliminary crystallographic analysis of the viral nucleoside diphosphate kinase protein is reported. The crystal belongs to the cubic space group P2{sub 1}3, with unit-cell parameter 99.425 Å. The self-rotation function confirms that there are two monomers per asymmetric unit related by a twofold non-crystallographic axis and that the unit cell thus contains four biological entities.

  4. 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.

  5. 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.

  6. A second monoclinic polymorph of 2-(diformylmethylidene-3,3-dimethyl-2,3-dihydro-1H-indole

    Directory of Open Access Journals (Sweden)

    Hamid Khaledi

    2009-10-01

    Full Text Available The crystal structure of the title compound, C13H13NO2, is a polymorph of the structure first reported by Helliwell et al. [Acta Cryst. (2006, E62, o737-o738]. It is also monoclinic (space group P21/c, but with completely different cell constants. The molecular conformations of these polymorphs differ by a 180° rotation of one formyl group. The present molecule is planar [maximum deviation 0.089 (2 Å] with the exception of the two methyl groups which lie on either side of the plane. There are strong intra- and intermolecular N—H...O hydrogen bonds. The latter link pairs of molecules across crystallographic centers of symmetry. Two aldehyde O atoms are brought close together [2.896 (4 Å in this arrangement but are not hydrogen bonded. In the earlier polymorph, one formyl group is rotated by 180° to yield intermolecular hydrogen bonding and an infinite polymeric chain. The other formyl group is involved in the same intramolecular hydrogen bonding as has been found here.

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

  9. 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.

  10. 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].

  11. (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

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    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.].

  12. 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.

  13. 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.

  14. (E-1-Phenylethanone semicarbazone

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    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.

  15. Crystal structure of 2-[(3S,4S-4-(anthracen-9-yl-1-(4-methoxyphenyl-2-oxoazetidin-3-yl]-2-aza-2H-phenalene-1,3-dione unknown solvate

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    Ísmail Çelik

    2015-03-01

    Full Text Available The central β-lactam ring of the title compound, C36H24N2O4, is almost planar (r.m.s. deviation = 0.003 Å and makes dihedral angles of 17.17 (19, 89.76 (17 and 78.44 (17° with the benzene ring, the anthracene ring (r.m.s. deviation = 0.003 Å and the 1H-benzo[de]isoquinoline-1,3(2H-dione moiety, which is nearly planar [maximum deviation = 0.098 (2 Å], respectively. The molecular structure is stabilized by an intramolecular C—H...N hydrogen bond. In the crystal, molecules are linked via C—H...π and π–π stacking interactions [centroid–centroid distances = 3.5270 (19 and 3.779 (2 Å], forming a three-dimensional structure. A region of disordered electron density, probably disordered solvent molecules, was treated with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18], which indicated a solvent cavity of 322 Å3 containing approximately 91 electrons. Their formula mass and unit-cell characteristics were not taken into account during the refinement.

  16. catena-Poly[[[iodidocopper(I]-{μ-N-[(pyridin-2-yl-κNmethylidene]pyridin-3-amine-κ2N3:N1}] acetonitrile hemisolvate

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    Ali Mahmoudi

    2012-10-01

    Full Text Available In the asymmetric unit of the title polymeric complex, {[CuI(C11H9N3]·0.5CH3CN}n, there are two CuI atoms, two N-[(pyridin-2-yl-κNmethylidene]pyridin-3-amine (PyPy ligands and two I atoms. Both CuI atoms have a distorted tetrahedral geometry, each being coordinated by one I atom, two N atoms of one PyPy ligand and one N atom from an adjacent PyPy ligand. In the crystal, infinite helical chains of [Cu2(PyPy2]n are formed propagating along the b axis. These chains are linked via weak C—H...I hydrogen bonds and π–π stacking interactions [shortest centroid–centroid distance = 3.2727 (14 Å]. During the refinement, electron-density peaks were located that were believed to be highly disordered solvent molecules (possibly acetonitrile. The SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155] indicated there were solvent cavities with a total volume of 196 Å3 containing approximately 60 electrons per unit cell, which equated to one molecule of acetonitrile per asymmetric unit.

  17. 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

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    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.

  18. Poly[dimethylammonium [(μ2-benzene-1,2-dicarboxylato-κ2O1:O3[μ2-3-(pyridin-4-yl-1H-pyrazol-1-ido-κ2N1:N3]cuprate(II

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    Liu Na

    2013-07-01

    Full Text Available In the title complex, {(C2H8N[Cu(C8H4O4(C8H6N3]}n, there are two CuII cations (each located on a centre of inversion, one benzene-1,2-dicarboxylate dianion, one 3-(pyridin-4-yl-1H-pyrazol-1-ide anion and one dimethylammonium cation in the asymmetric unit. The dimethylammonium cation was highly disordered and was treated with the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]; the crystallographic data takes into account the presence of the cation. Each CuII cation exhibits a square-planar coordination geometry. A benzene-1,2-dicarboxylate dianion bridges two CuII cations, building a linear chain along [001]. The chains are connected by 3-(pyridin-4-yl-1H-pyrazol-1-ide anions, constructing a layer parallel to (101. The layers are assembled into a three-dimensional supramolecular network through C—H...π interactions.

  19. (RS-Efonidipine acetone hemisolvate

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    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. 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.

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

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    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].

  2. 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

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    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].

  3. 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.

  4. (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.

  5. Bromidocarbonyl{(1S,2S-N-[2-(dicyclohexylphosphanylethylidenyl]-N′-[2-(diphenylphosphanylethyl]-1,2-diphenylethane-1,2-diamine}iron(II tetraphenylborate

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    Samantha A. M. Smith

    2017-03-01

    Full Text Available In the title compound, trans-(S,S-[FeBr(CO(PPh2CH2CH2NHCHPhCHPhNCHCH2PCy2]BPh4, the FeII ion is in a distorted octahedral complex geometry with a cis-β ligand geometry in which two diastereomers co-crystallized in the asymmetric unit. These diastereomers differ by the orientation of the N—H moieties on the ligand; one is in the S conformation (A, and the other R (B. Diasteromer A has a P—Fe—P angle of 104.36 (6° and B has a P—Fe—P angle of 102.70 (6°. During the refinement of the structure, electron density peaks were located that were believed to be highly disordered solvent molecules (possibly diethyl ether. Attempts made to model the solvent molecule were not successful. The SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] option in PLATON indicated there was a large solvent cavity of 363 Å3. In the final cycles of refinement, this contribution of 117 electrons to the electron density was removed from the observed data. The density, the F(000 value, the molecular weight and the formula are given without taking into account the results obtained with SQUEEZE.

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

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    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.

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

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    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.

  8. 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.

  9. (E-4-[4-(Dimethylaminostyryl]-1-methylpyridin-1-ium tetrakis[(Z-4,4,4-trifluoro-3-oxo-1-(thiophen-2-ylbut-1-en-1-olato]gadolinate(III with an unknown amount of water as solvate

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    Da-Jun Wu

    2016-11-01

    Full Text Available In the complex anion of the title salt, (C16H19N2[Gd(C8H4F3S4], the GaIII cation is O,O′-chelated by four anionic 4,4,4-trifluoro-3-oxo-1-(thiophen-2-ylbut-1-en-1-olate ligands in a distorted square-antiprismatic geometry; the 4-[4-(dimethylaminostyryl]-1-methylpyridin-1-ium cation is nearly planar, with a dihedral angle of 9.6 (5° between the planes of the pyridine and benzene rings. In the crystal, the cations are linked with the complex anions via weak C—H...F and C—H...π interactions. Two of the four independent thiophene rings are disordered over two sites; occupancies were refined to 0.662 (10:0.338 (10. The solvent water molecules are highly disordered in a solvent-accessible void of 54 (3 Å3; the diffuse electron densities were removed from the data set using SQUEEZE [Spek (2015. Acta Cryst. C71, 9–16]. These solvent molecules are not considered in the given chemical formula and other crystal data.

  10. 1,1′-(Diselanediylbis{[P,P-diphenyl-N-(trimethylsilylphosphorimidoyl]methanylylidene}bis[1,1-diphenyl-N-(trimethylsilyl-λ5-phosphanamine] pentane disolvate

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    Ramalingam Thirumoorthi

    2014-01-01

    Full Text Available The title compound, C62H78N4P4Se2Si4·2C5H12, is made up of two [SeC(PPh2NSiMe3(PPh2NHSiMe3] units related by an inversion center situated at the mid-point of the diselenide bond. It crystallized with two disordered molecules of pentane used as solvent of crystallization. It is a rare example of an antiperiplanar diselenide and exhibits a long Se—Se bond of 2.4717 (8 Å. The Se—C bond length of 1.876 (5 Å is short in comparison with the range of values found for other diselenides (1.91–1.97 Å. The molecule exhibits two intramolecular N—H...N hydrogen bonds. In the crystal, there are no significant intermolecular interactions present. One of the Me3Si– groups is disordered over two positions with a refined occupancy ratio of 0.708 (8:0.292 (8. The contribution of the disordered solvent to the scattering was removed with the SQUEEZE option of PLATON [Spek (2009. Acta Cryst. D65, 148–155]. The solvent contribution has been included in the reported molecular weight and density.

  11. 1,1′-(Diselanediylbis{[P,P-diphenyl-N-(tri­methyl­sil­yl)phospho­rimido­yl]methanylyl­idene})bis­[1,1-diphenyl-N-(tri­methyl­sil­yl)-λ5-phosphanamine] pentane disolvate

    Science.gov (United States)

    Thirumoorthi, Ramalingam; Chivers, Tristram; Laitinen, Risto S.

    2014-01-01

    The title compound, C62H78N4P4Se2Si4·2C5H12, is made up of two [SeC(PPh2NSiMe3)(PPh2NHSiMe3)] units related by an inversion center situated at the mid-point of the diselenide bond. It crystallized with two disordered mol­ecules of pentane used as solvent of crystallization. It is a rare example of an anti­periplanar diselenide and exhibits a long Se—Se bond of 2.4717 (8) Å. The Se—C bond length of 1.876 (5) Å is short in comparison with the range of values found for other diselenides (1.91–1.97 Å). The mol­ecule exhibits two intra­molecular N—H⋯N hydrogen bonds. In the crystal, there are no significant inter­molecular inter­actions present. One of the Me3Si– groups is disordered over two positions with a refined occupancy ratio of 0.708 (8):0.292 (8). The contribution of the disordered solvent to the scattering was removed with the SQUEEZE option of PLATON [Spek (2009 ▶). Acta Cryst. D65, 148–155]. The solvent contribution has been included in the reported mol­ecular weight and density. PMID:24526971

  12. 1,1'-(Diselanediylbis{[P,P-diphenyl-N-(tri-methyl-sil-yl)phospho-rimido-yl]methanylyl-idene})bis-[1,1-diphenyl-N-(tri-methyl-sil-yl)-λ(5)-phosphanamine] pentane disolvate.

    Science.gov (United States)

    Thirumoorthi, Ramalingam; Chivers, Tristram; Laitinen, Risto S

    2014-01-01

    The title compound, C62H78N4P4Se2Si4·2C5H12, is made up of two [SeC(PPh2NSiMe3)(PPh2NHSiMe3)] units related by an inversion center situated at the mid-point of the diselenide bond. It crystallized with two disordered mol-ecules of pentane used as solvent of crystallization. It is a rare example of an anti-periplanar diselenide and exhibits a long Se-Se bond of 2.4717 (8) Å. The Se-C bond length of 1.876 (5) Å is short in comparison with the range of values found for other diselenides (1.91-1.97 Å). The mol-ecule exhibits two intra-molecular N-H⋯N hydrogen bonds. In the crystal, there are no significant inter-molecular inter-actions present. One of the Me3Si- groups is disordered over two positions with a refined occupancy ratio of 0.708 (8):0.292 (8). The contribution of the disordered solvent to the scattering was removed with the SQUEEZE option of PLATON [Spek (2009 ▶). Acta Cryst. D65, 148-155]. The solvent contribution has been included in the reported mol-ecular weight and density.

  13. A new interpretation and practical aspects of the direct-methods modulus sum function. VIII.

    Science.gov (United States)

    Rius, Jordi; Torrelles, Xavier; Miravitlles, Carles; Amigó, J M; Reventós, M M

    2002-01-01

    Since the first publication of the direct-methods modulus sum function [Rius (1993). Acta Cryst. A49, 406-409], the application of this function to a variety of situations has been shown in a series of seven subsequent papers. In this way, much experience about this function and its practical use has been gained. It is thought by the authors that it is now the right moment to publish a more complete study of this function which also considers most of this practical knowledge. The first part of the study relates, thanks to a new interpretation, this function to other existing phase-refinement functions, while the second shows, with the help of test calculations on a selection of crystal structures, the behaviour of the function for two different control parameters. In this study, the principal interest is focused on the function itself and not on the optimization procedure which is based on a conventional sequential tangent formula refinement. The results obtained are quite satisfactory and seem to indicate that, when combined with more sophisticated optimization algorithms, the application field of this function could be extended to larger structures than those used for the test calculations.

  14. Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes.

    Science.gov (United States)

    Rius, Jordi; Mugnaioli, Enrico; Vallcorba, Oriol; Kolb, Ute

    2013-07-01

    δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now available for structure determination by direct methods. To check the tolerance of δ recycling to missing data-collection corrections and to deviations from kinematical behaviour of ADT intensities, δ recycling has been applied to differently shaped nanocrystals of various inorganic materials. The results confirm that it can phase ADT data very efficiently. In some cases even more complete structure models than those derived from conventional direct methods and least-squares refinement have been found. During this study it has been demonstrated that the Wilson-plot scaling procedure is largely insensitive to sample thickness variations and missing absorption corrections affecting electron ADT intensities.

  15. Direct phasing from Patterson syntheses by δ recycling.

    Science.gov (United States)

    Rius, Jordi

    2012-01-01

    The direct methods origin-free modulus sum function [Rius (1993). Acta Cryst. A49, 406-409] includes in its definition the structure factor G(Φ) of the squared crystal structure expressed in terms of Φ, the set of φ phases of the normalized structure factors E's of the crystal structure of unit-cell volume V. Here the simpler sum function variant S'(P) = ∑(H)E(-H)∫(V)δ(P,Δ)(Φ)exp(i2πHr)dV extended over all H reflections is introduced which involves no G's and in which the δ(P,Δ) function corresponds to δ(P) = FT(-1){(E(2)(H) - )exp[iφ(H)(Φ)]} (where FT = Fourier transform) with all values smaller than Δ = 2.5σ(P) equated to zero (σ(2)(P) is the variance of δ(P) calculable from the experimental intensities). The new phase estimates are obtained by Fourier transforming δ(P,Δ). This iterative phasing method (δ recycling) only requires calculation of Fourier transforms at two stages. Since δ(M) ≃ δ(P)/2, similar arguments are valid for δ(M) = FT(-1)[(E(H) - )exp(iφ(H))] from which the corresponding S'(M) phasing function follows.

  16. Crystal structures of spinel-type Na2MoO4 and Na2WO4 revisited using neutron powder diffraction

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    A. Dominic Fortes

    2015-06-01

    Full Text Available Time-of-flight neutron powder diffraction data have been collected from Na2MoO4 and Na2WO4 to a resolution of sin (θ/λ = 1.25 Å−1, which is substantially better than the previous analyses using Mo Kα X-rays, providing roughly triple the number of measured reflections with respect to the previous studies [Okada et al. (1974. Acta Cryst. B30, 1872–1873; Bramnik & Ehrenberg (2004. Z. Anorg. Allg. Chem. 630, 1336–1341]. The unit-cell parameters are in excellent agreement with literature data [Swanson et al. (1962. NBS Monograph No. 25, sect. 1, pp. 46–47] and the structural parameters for the molybdate agree very well with those of Bramnik & Ehrenberg (2004. However, the tungstate structure refinement of Okada et al. (1974 stands apart as being conspicuously inaccurate, giving significantly longer W—O distances, 1.819 (8 Å, and shorter Na—O distances, 2.378 (8 Å, than are reported here or in other simple tungstates. As such, this work represents an order-of-magnitude improvement in precision for sodium molybdate and an equally substantial improvement in both accuracy and precision for sodium tungstate. Both compounds adopt the spinel structure type. The Na+ ions have site symmetry .-3m and are in octahedral coordination while the transition metal atoms have site symmetry -43m and are in tetrahedral coordination.

  17. Cannabidiol revisited

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    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.

  18. A monoclinic polymorph of [(Z-N-(3-chlorophenyl-O-methylthiocarbamato-κS](triphenylphosphane-κPgold(I: crystal structure and Hirshfeld surface analysis

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    Chien Ing Yeo

    2016-08-01

    Full Text Available The title compound, [Au(C8H7ClNOS(C18H15P], is a monoclinic (P21/n, Z′ = 1; form β polymorph of the previously reported triclinic form (P-1, Z′ = 1; form α [Tadbuppa & Tiekink (2010. Acta Cryst. E66, m664]. The molecular structures of both forms feature an almost linear gold(I coordination geometry [P—Au—S = 175.62 (5° in the title polymorph], being coordinated by thiolate S and phosphane P atoms, a Z conformation about the C=N bond and an intramolecular Au...O contact. The major conformational difference relates to the relative orientations of the residues about the Au—S bond: the P—Au—S—C torsion angles are −8.4 (7 and 106.2 (7° in forms α and β, respectively. The molecular packing of form β features centrosymmetric aggregates sustained by aryl-C—H...O interactions, which are connected into a three-dimensional network by aryl-C—H...π contacts. The Hirshfeld analysis of forms α and β shows many similarities with the notable exception of the influence of C—H...O interactions in form β.

  19. Oscillatory thermocapillary convection in liquid bridges with highly deformed free surfaces: Experiments and energy-stability analysis

    Science.gov (United States)

    Sumner, L. B. S.; Neitzel, G. P.; Fontaine, J.-P.; Dell'Aversana, P.

    2001-01-01

    Laboratory experimentation, numerical simulation, and energy-stability theory are used to examine the effect of interface deformation on the onset of oscillatory thermocapillary convection in half zones. Experiments are performed to map the stability boundaries marking the onset of oscillatory flow, modifying the free-surface deformation by adjusting the volume of liquid in the bridge. The stability results presented here along with those of other researchers [Monti et al., Proceedings of the 43rd Cong. Int. Artro. Fed. (1992); Hu et al., J. Cryst. Growth 142, 379 (1994)] show that free-surface curvature can have a pronounced influence on flow stability. Steady, axisymmetric flow simulations are computed using the commercial code FIDAP to model the conditions of the experiments, and reveal that flow structure near the stability boundary is sensitive to several parameters. Energy theory is applied to these simulations to determine sufficient conditions for stability. Comparisons between the theoretical and experimental results show nonconservative energy limits falling above the experimentally determined stability boundaries for bridges of various liquid volumes. While the trend of the experimental data is predicted for zones of large volume ratio (bulging zones), the same cannot be said for those with small volume ratio (necked-down zones). In addition, energy-stability limits for some undeformed-free-surface cases were determined which are above the linear-stability limits determined by other researchers, in clear contradiction of the roles of the respective theories.

  20. Ring-strain release in neutral and dicationic 7,8,17,18-tetrabromo-5,10,15,20-tetraphenylporphyrin: crystal structures of C44H26Br4N4 and C44H28Br4N42+·2ClO4−·3CH2Cl2

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    W. Robert Scheidt

    2016-06-01

    Full Text Available Two porphyrin complexes were studied to determine the effects of protonation on ring deformation within the porphyrin. The porphyrin 7,8,17,18-tetrabromo-5,10,15,20-tetraphenylporphyrin, C44H26Br4N4, was selected because the neutral species is readily doubly protonated to yield a dication, which was crystallized here with perchlorate counter-ions as a dichloromethane trisolvate, C44H28Br4N42+·2ClO4−·3CH2Cl2. The centrosymmetric neutral species is observed to have a mild `ruffling' of the pyrrole rings and is essentially planar throughout; intramolecular N—H...N hydrogen bonds occur. In contrast, the dication exhibits considerable deformation, with the pyrrole rings oriented well out of the plane of the porphyrin, resulting in a `saddle' conformation of the ring. The charged species forms N—H...O hydrogen bonds to the perchlorate anions, which lie above and below the plane of the porphyrin ring. Distortions to the planarity of the pyrrole rings in both cases are very minor. The characterization of the neutral species represents a low-temperature redetermination of the previous room-temperature analyses [Zou et al. (1995. Acta Cryst. C51, 760–761; Rayati et al. (2008. Polyhedron, pp. 2285–2290], which showed disorder and physically unrealistic displacement parameters.

  1. Mol-ecular and crystal structure of gossypol tetra-methyl ether with an unknown solvate.

    Science.gov (United States)

    Honkeldieva, Muhabbat; Talipov, Samat; Mardanov, Rustam; Ibragimov, Bakhtiyar

    2015-02-01

    The title compound, C34H38O8 (systematic name: 5,5'-diisopropyl-2,2',3,3'-tetra-meth-oxy-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 mol-ecule is situated on a twofold rotation axis, so the asymmetric unit contains one half-mol-ecule. In the mol-ecule, the hy-droxy groups are involved in intra-molecular 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 inter-actions 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 mol-ecules, 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].

  2. Crystal structure of cis-bis-{4-phenyl-1-[(3R)-1,7,7-tri-methyl-2-oxobi-cyclo-[2.2.1]heptan-3-ylidene]thio-semicarbazidato-κ(3) O,N (1),S}cadmium(II) with an unknown solvent mol-ecule.

    Science.gov (United States)

    Nogueira, Vanessa Senna; Bresolin, Leandro; Näther, Christian; Jess, Inke; de Oliveira, Adriano Bof

    2015-12-01

    The reaction between the racemic mixture of the camphor-4-phenyl-thio-semicarbazone derivative and cadmium acetate dihydrate yielded the title compound, [Cd(C17H20N3OS)2]. The Cd(II) ion is six-coordinated in a distorted octa-hedral environment by two deprotonated thio-semicarbazone ligands acting as an O,N,S-donor in a tridentate chelating mode, forming five-membered chelate rings. In the crystal, the mol-ecules are connected via pairs of N-H⋯S and C-H⋯S inter-actions, building centrosymmetric dimers. One of the ligands is disordered in the campher unit over two sets of sites with site-occupancy factors of 0.7 and 0.3. The structure contains additional solvent mol-ecules, which are disordered and for which no reasonable split model was found. Therefore, the data were corrected for disordered solvent using the SQUEEZE routine [Spek (2015 ▸). Acta Cryst. C71, 9-18] in PLATON. Since the disordered solvents were removed by data processing, and the number of solvent entities was a suggestion only, they were not considered in the chemical formula and subsequent chemical or crystal information.

  3. Crystal structure of 5-amino-5'-chloro-6-(4-chloro-benzo-yl)-8-nitro-2,3-di-hydro-1H-spiro-[imidazo[1,2-a]pyridine-7,3'-indolin]-2'-one including an unknown solvent mol-ecule.

    Science.gov (United States)

    Nagalakshmi, R A; Suresh, J; Sivakumar, S; Kumar, R Ranjith; Lakshman, P L Nilantha

    2014-09-01

    The asymmetric unit of the title compound, C21H15Cl2N5O4, contains two independent mol-ecules (A and B) having similar conformations. The amine (NH2) group forms an intra-molecular hydrogen bond with the benzoyl group, giving an S(6) ring motif in both mol-ecules. The central six-membered rings adopt sofa conformations and the imidazole rings are planar (r.m.s deviations = 0.0150 and 0.0166 Å). The pyridine and imidazole rings are inclined to one another by 3.54 (1) and 3.03 (1)° in mol-ecules A and B, respectively. In the crystal, mol-ecules are linked by N-H⋯O hydrogen bonds, forming chains along the a axis which enclose R 2 (2)(16) ring motifs. The rings are linked by weak N-H⋯O and C-H⋯O hydrogen bonds and C-H⋯π inter-actions forming sheets lying parallel to (001). A region of disordered electron density, most probably disordered solvent mol-ecules, occupying voids of ca 753 Å(3) for an electron count of 260, 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.

  4. Experimental and theoretical study of diffraction properties of various crystals for the realization of a soft gamma-ray Laue lens

    CERN Document Server

    Barriere, Nicolas; von Ballmoos, Peter; Abrosimov, Nikolai V; Courtois, Pierre; Bastie, Pierre; Camus, Thierry; Jentschel, Michael; Kurlov, Vladimir N; Natalucci, Lorenzo; Roudil, Gilles; Brejnholt, Nicolai Frisch; Serre, Denis

    2009-01-01

    Crystals are the elementary constituents of Laue lenses, an emerging technology which could allow the realization of a space borne telescope 10 to 100 times more sensitive than existing ones in the 100 keV - 1.5 MeV energy range. This study addresses the current endeavor to the development of efficient crystals for the realization of a Laue lens. In the theoretical part 35 candidate-crystals both pure and two-components are considered. Their peak reflectivity at 100 keV, 500 keV and 1 MeV is calculated assuming they are mosaic crystals. It results that a careful selection of crystals can allow a reflectivity above 30% over the whole energy range, and even reaching 40% in its lower part. Experimentally, we concentrated on three different materials (Si_{1-x}Ge_x with gradient of composition, mosaic Cu and Au) that have been measured both at ESRF and ILL using highly-monochromatic beams ranging from 300 keV up to 816 keV. The aim was to check their homogeneity, quality and angular spread (mosaicity). These cryst...

  5. A Hidden Markov model web application for analysing bacterial genomotyping DNA microarray experiments.

    Science.gov (United States)

    Newton, Richard; Hinds, Jason; Wernisch, Lorenz

    2006-01-01

    Whole genome DNA microarray genomotyping experiments compare the gene content of different species or strains of bacteria. A statistical approach to analysing the results of these experiments was developed, based on a Hidden Markov model (HMM), which takes adjacency of genes along the genome into account when calling genes present or absent. The model was implemented in the statistical language R and applied to three datasets. The method is numerically stable with good convergence properties. Error rates are reduced compared with approaches that ignore spatial information. Moreover, the HMM circumvents a problem encountered in a conventional analysis: determining the cut-off value to use to classify a gene as absent. An Apache Struts web interface for the R script was created for the benefit of users unfamiliar with R. The application may be found at http://hmmgd.cryst.bbk.ac.uk/hmmgd. The source code illustrating how to run R scripts from an Apache Struts-based web application is available from the corresponding author on request. The application is also available for local installation if required.

  6. Redetermination of diaqua[N,N′-bis(3-methoxy-2-oxidobenzylideneethylenediamine-κ4O,N,N′,O′]manganese(III perchlorate at 100 K

    Directory of Open Access Journals (Sweden)

    Shabana Noor

    2016-11-01

    Full Text Available The crystal structure of the organic–inorganic title salt, [Mn(C18H18N2O4(H2O2]ClO4, has been redetermined at 100 K. In contrast to the crystal structure determinations at room temperature [Akitsu et al. (2005. Acta Cryst. C61, m324–m328; Bermejo et al. (2007. Eur. J. Inorg. Chem. pp. 3789–3797], positional disorder of the ethylene bridge in the Schiff base ligand and the perchlorate anion is not observed at 100 K. The MnIII ion is six-coordinated with the tetradentate Schiff base chelate ligand N,N′-bis(3-methoxy-2-oxybenzylideneethylenediamine occupying coordination sites in the equatorial plane and the aqua ligands residing in the two axial positions. The octahedral coordination sphere of the MnIII ion exhibits an axial elongation due to the Jahn–Teller effect, which is characteristic of a d4 high-spin electronic configuration.

  7. Azimuthal anchoring of a nematic liquid crystal on a grooved interface with anisotropic polar anchoring

    Institute of Scientific and Technical Information of China (English)

    Zhou Xuan; Zhang Zhi-Dong; Ye Wen-Jiang; Xuan Li

    2012-01-01

    Zhang Y Jet al.[Zhang Y J,Zhang Z D,Zhu L Z and Xuan L 2011 Liquid Cryst.38 355] investigated the effects of finite polar anchoring on the azimuthal anchoring energy at a grooved interface,in which polar anchoring was isotropic in the local tangent plane of the surface.In this paper,we investigate the effects of both isotropic and anisotropic polar anchoring on the surface anchoring energy in the frame of Fukuda et al.'s theory.The results show that anisotropic polar anchoring strengthens the azimuthal anchoring of grooved surfaces.In the one-elastic-constant approximation (K11 =K22 =K33 =K),the surface-groove-induced azimuthal anchoring energy is entirely consistent with the result of Faetti,and it reduces to the original result of Berreman with an increase in polar anchoring.Moreover,the contribution of the surface-like elastic term to the Rapini-Papoular anchoring energy is zero.

  8. Crystal structure of lead(II) tartrate: a redetermination.

    Science.gov (United States)

    Weil, Matthias

    2015-01-01

    Single crystals of poly[μ4-tartrato-κ(6) O (1),O (3):O (1'):O (2),O (4):O (4')-lead], [Pb(C4H4O6)] n , were grown in a gel medium. In comparison with the previous structure determination of this compound from laboratory powder X-ray diffraction data [De Ridder et al. (2002 ▶). Acta Cryst. C58, m596-m598], the redetermination on the basis of single-crystal data reveals the absolute structure, all atoms with anisotropic displacement parameters and a much higher accuracy in terms of bond lengths and angles. It could be shown that a different space group or incorporation of water as reported for similarly gel-grown lead tartrate crystals is incorrect. In the structure, each Pb(2+) cation is bonded to eight O atoms of five tartrate anions, while each tartrate anion links four Pb(2+) cations. The resulting three-dimensional framework is stabilized by O-H⋯O hydrogen bonds between the OH groups of one tartrate anion and the carboxyl-ate O atoms of adjacent anions.

  9. Inferring planar disorder in close-packed structures via ε-machine spectral reconstruction theory: examples from simulated diffraction patterns.

    Science.gov (United States)

    Varn, D P; Canright, G S; Crutchfield, J P

    2013-07-01

    A previous paper detailed a novel algorithm, ε-machine spectral reconstruction theory (εMSR), that infers pattern and disorder in planar-faulted, close-packed structures directly from X-ray diffraction patterns [Varn et al. (2013). Acta Cryst. A69, 197-206]. Here εMSR is applied to simulated diffraction patterns from four close-packed crystals. It is found that, for stacking structures with a memory length of three or less, εMSR reproduces the statistics of the stacking structure; the result being in the form of a directed graph called an ε-machine. For stacking structures with a memory length larger than three, εMSR returns a model that captures many important features of the original stacking structure. These include multiple stacking faults and multiple crystal structures. Further, it is found that εMSR is able to discover stacking structure in even highly disordered crystals. In order to address issues concerning the long-range order observed in many classes of layered materials, several length parameters are defined, calculable from the ε-machine, and their relevance is discussed.

  10. 2,3-Dibromo-3-phenylpropanoic acid: a monoclinic polymorph

    Directory of Open Access Journals (Sweden)

    Trent R. Howard

    2016-11-01

    Full Text Available Bromination of trans-cinnamic acid resulted in the formation of 2,3-dibromo-3-phenylpropanoic acid, C9H8Br2O2. Crystallization from ethanol–water (1:1 gave crystals of different shapes. One is in the form of rods, that crystallized as the orthorhombic polymorph (Pnma, and whose structure has been described [Thong et al. (2008. Acta Cryst. E64, o1946]. The other are thin plate-like crystals which are the monoclinic polymorph (P21/n. The structure of this monoclinic polymorph is similar to that of the orthorhombic polymorph; here the aliphatic C atoms are disordered over three sets of sites (occupancy ratio 0.5:0.25:0.25. In the crystal, molecules are linked by pairs of O—H...O hydrogen bonds, forming inversion dimers with an R22(8 ring motif. The dimers are linked by weak C—H...Br hydrogen bonds, forming chains propagating along the a-axis direction.

  11. A polymorph structure of copper(II hydrogenphosphite dihydrate

    Directory of Open Access Journals (Sweden)

    Lei Yang

    2009-04-01

    Full Text Available The title compound, poly[[diaquacopper(II]-μ3-hydrogenphosphito], [Cu(HPO3(H2O2]n, (I, has been prepared by hydrothermal synthesis at 393 K. Its non-centrosymmetric polymorph structure, (II, was known previously and has been redetermined at 193 (2 K [El Bali & Massa (2002. Acta Cryst. E58, i29–i31]. The Cu atoms in (I and (II are square-pyramidal coordinated. A distorted octahedral geometry around the Cu atoms is considered by including the strongly elongated apical distances of 2.8716 (15 Å in (I and 3.000 (1 Å in (II. The Cu...Cu separation of the dimeric unit is 3.1074 (3 Å. The secondary building units (SBU (the Cu2O2 dimer and two HPO3 units in (I are inversion related and form a two-dimensional layered structure, with sheets parallel to the bc plane, whereas in the structure of (II, the chain elements are connected via screw-axis symmetry to form a three-dimensional microporous framework. In both polymorph structures, strong O—H...O hydrogen bonds are observed.

  12. Di-n-butylammonium 2-[(3,5-di-tert-butyl-4-hydroxybenzylsulfanyl]benzoate

    Directory of Open Access Journals (Sweden)

    Abeer A. Alhadi

    2010-09-01

    Full Text Available The title salt, C8H20N+·C22H27O3S−, is a proton-transfer compound derived from the recently reported parent carboxylic acid [Alhadi et al. (2010. Acta Cryst. E66, o1787] by the addition of a second equivalent of di-n-butylamine, yielding the di-n-butylammonium carboxylate salt. The structure of the carboxylate anion resembles that of the parent carboxylic acid. The main difference lies in the position of the H atom in the 4-hydroxy group. In the anion the O—H bond is perpendicular, rather than parallel, to the benzyl ring. This position appears to facilitate hydrogen bonding to an O atom of the carboxylate group of a symmetry-related anion. In addition, there are three N—H...O hydrogen bonds. In contrast, the neutral species hydrogen bonds via a carboxylic acid dimer. The dihedral angle between the benzene rings in the anion is 79.19 (7°.

  13. 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.

  14. 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.

  15. Crystal structure of ethyl 3-amino-6-methyl-2-[(4-methyl­phen­yl)carbamo­yl]-4-[(E)-2-phenyl­ethen­yl]thieno[2,3-b]pyridine-5-carboxyl­ate monohydrate

    Science.gov (United States)

    Mague, Joel T.; Akkurt, Mehmet; Mohamed, Shaaban K.; Bakhite, Etify A.; Albayati, Mustafa R.

    2016-01-01

    In the title mol­ecule, C27H25N3O3S·H2O, the dihedral angle between the planes of the thienyl ring and the pendant p-tolyl group is 39.25 (6)°, while that between the pyridine ring and the pendant phenyl ring is 44.37 (6)°. In addition, there is a slight twist in the bicyclic core, with a dihedral angle of 2.39 (4)° between the thienyl and pyridine rings. The conformation of the carbamoyl moiety is partially determined by an intra­molecular N—H⋯O hydrogen bond. In the crystal, complementary N—H⋯O hydrogen bonds form dimers which are then associated into chains parallel to the c axis through O—H⋯N hydrogen bonds involving the water mol­ecule of crystallization. Electron density associated with an additional solvent mol­ecule of partial occupancy and disordered about a twofold axis was removed with the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s). PMID:27006791

  16. A Fourier transform method for powder diffraction based on the Debye scattering equation.

    Science.gov (United States)

    Thomas, Noel William

    2011-11-01

    A fast Fourier transform algorithm is introduced into the method recently defined for calculating powder diffraction patterns by means of the Debye scattering equation (DSE) [Thomas (2010). Acta Cryst. A66, 64-77]. For this purpose, conventionally used histograms of interatomic distances are replaced by compound transmittance functions. These may be Fourier transformed to partial diffraction patterns, which sum to give the complete diffraction pattern. They also lead to an alternative analytical expression for the DSE sum, which reveals its convergence behaviour. A means of embedding the DSE approach within the reciprocal-lattice-structure-factor method is indicated, with interpolation methods for deriving the peak profiles of nanocrystalline materials outlined. Efficient calculation of transmittance functions for larger crystallites requires the Patterson group symmetry of the crystals to be taken into account, as shown for α- and β-quartz. The capability of the transmittance functions to accommodate stacking disorder is demonstrated by reference to kaolinite, with a fully analytical treatment of disorder described. Areas of future work brought about by these developments are discussed, specifically the handling of anisotropic atomic displacement parameters, inverse Fourier transformation and the incorporation of instrumental (diffractometer) parameters.

  17. 4-De­oxy-4-fluoro-β-d-gluco­pyranose

    Science.gov (United States)

    Zhang, Wenhui; Oliver, Allen G.; Serianni, Anthony S.

    2010-01-01

    4-De­oxy-4-fluoro-β-d-glucopyran­ose, C6H11FO5, (I), crystallizes from water at room temperature in a slightly distorted 4 C 1 chair con­formation. The observed chair distortion differs from that observed in β-d-glucopyran­ose [Kouwijzer, van Eijck, Kooijman & Kroon (1995 ▶). Acta Cryst. B51, 209–220], (II), with the former skewed toward a B C3,O5 (boat) conformer and the latter toward an O5 TB C2 (twist–boat) conformer, based on Cremer–Pople analysis. The exocyclic hy­droxy­methyl group conformations in (I) and (II) are similar; in both cases, the O—C—C—O torsion angle is ∼−60° (gg con­former). Inter­molecular hydrogen bonding in the crystal structures of (I) and (II) is conserved in that identical patterns of donors and acceptors are observed for the exocyclic substituents and the ring O atom of each monosaccharide. Inspection of the crystal packing structures of (I) and (II) reveals an essentially identical packing configuration. PMID:20921614

  18. 4-Deoxy-4-fluoro-β-D-glucopyranose.

    Science.gov (United States)

    Zhang, Wenhui; Oliver, Allen G; Serianni, Anthony S

    2010-10-01

    4-Deoxy-4-fluoro-β-D-glucopyranose, C(6)H(11)FO(5), (I), crystallizes from water at room temperature in a slightly distorted (4)C(1) chair conformation. The observed chair distortion differs from that observed in β-D-glucopyranose [Kouwijzer, van Eijck, Kooijman & Kroon (1995). Acta Cryst. B51, 209-220], (II), with the former skewed toward a B(C3,O5) (boat) conformer and the latter toward an (O5)TB(C2) (twist-boat) conformer, based on Cremer-Pople analysis. The exocyclic hydroxymethyl group conformations in (I) and (II) are similar; in both cases, the O-C-C-O torsion angle is ∼-60° (gg conformer). Intermolecular hydrogen bonding in the crystal structures of (I) and (II) is conserved in that identical patterns of donors and acceptors are observed for the exocyclic substituents and the ring O atom of each monosaccharide. Inspection of the crystal packing structures of (I) and (II) reveals an essentially identical packing configuration.

  19. 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.

  20. 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.

  1. Crystal structures of two ytterbium(III) complexes comprising alkynylamidinate ligands.

    Science.gov (United States)

    Wang, Sida; Sroor, Farid M; Liebing, Phil; Lorenz, Volker; Hilfert, Liane; Edelmann, Frank T

    2016-09-01

    Two ytterbium(III) complexes comprising alkynylamidinate ligands, namely bis-(η(5)-cyclo-penta-dien-yl)(3-cyclo-propyl-N,N'-diiso-propyl-propynamidinato-κ(2)N,N')ytterbium(III), [Yb(C5H5)2(C12H19N2)] or Cp2Yb[( (i) Pr2N)2C-C≡C-c-C3H5] (1) and tris-(3-phenyl-N,N'-di-cyclo-hexyl-propynamidinato-κ(2)N,N')ytterbium(III), [Yb(C21H27N2)3] or Yb[(CyN)2C-C≡C-Ph]3 (Cy = cyclo-hex-yl) (2) have been synthesized and structurally characterized. Both complexes are monomers; for complex 2, the contribution to the scattering from highly disordered toluene solvent molecules in these voids 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.

  2. Crystal structure of Sc1.91In1.39Mo15Se19, containing Mo6 and Mo9 clusters

    Directory of Open Access Journals (Sweden)

    Patrick Gougeon

    2015-07-01

    Full Text Available The structure of scandium indium pentadecamolybdenum nonadecaselenide, Sc1.91In1.39Mo15Se19, 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 -3 and -6, respectively. The clusters are interconnected through additional Mo—Se bonds. Sc—Se and In—Se bonds complete the structural set-up. In the title compound, the Sc3+ cations replace the trivalent indium atoms present in In2.9Mo15Se19, and a deficiency is observed at the monovalent indium site. One Mo, one Se and the Sc atom are situated on mirror planes, whereas two other Se atoms and the In atom are situated on threefold rotation axes.

  3. Na3.88Mo15Se19: a novel ternary reduced molybdenum selenide containing Mo6 and Mo9 clusters

    Directory of Open Access Journals (Sweden)

    Diala Salloum

    2013-10-01

    Full Text Available The structure of tetrasodium pentadecamolybdenum nonadecaselenide, Na3.88Mo15Se19, is isotypic with the In3+xMo15Se19 compounds [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 -3 and -6, respectively. The clusters are interconnected through additional Mo—Se bonds. In the title compound, the Na+ cations replace the trivalent as well as the monovalent indium atoms present in In3.9Mo15Se19. One Mo, one Se and one Na atom are situated on mirror planes, and two other Se atoms and one Na atom [occupancy 0.628 (14] are situated on threefold rotation axes. The crystal studied was twinned by merohedry with refined components of 0.4216 (12 and 0.5784 (12.

  4. Protein energy landscapes determined by five-dimensional crystallography.

    Science.gov (United States)

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

    2013-12-01

    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.

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

    Science.gov (United States)

    Coquelle, Nicolas; Brewster, Aaron S; Kapp, Ulrike; Shilova, Anastasya; Weinhausen, Britta; Burghammer, Manfred; Colletier, Jacques Philippe

    2015-05-01

    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.

  6. 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.

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

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    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].

  8. Crystal structure of 2-bromobenzoic acid at 120 K: a redetermination

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    Kornelia Kowalska

    2014-10-01

    Full Text Available The crystal structure of the title compound, C7H5BrO2, was originally studied using photographic data at room temperature with Cu Kα radiation [Ferguson & Sim (1962. Acta Cryst. 15, 346–350]. The present study was undertaken at 120 K with a CCD diffractometer using Cu Kα radiation, and resulted in improved geometrical parameters. In the molecule, the carboxy group is inclined to the benzene ring by 18.7 (2° and there is a close intramolecular Br...O contact of 3.009 (3 Å. In the crystal, molecules are linked by pairs of O—H...O hydrogen bonds, forming inversion dimers with the classical R22(8 ring motif for carboxylic acids. Neighbouring dimers are linked by weak C—H...O hydrogen bonds, forming tapes propagating in [1-10]. Adjacent tapes interact by slipped parallel π–π interactions [inter-centroid distance = 3.991 (2, interplanar distance = 3.509 (2 Å, slippage = 1.900 Å] to form columns approximately along the b-axis direction. Neighbouring columns interact dispersively, forming a three-dimensional framework structure.

  9. 2,2′-(Piperazine-1,4-diyldiethanaminium dibenzoate

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    Ignacy Cukrowski

    2012-08-01

    Full Text Available The asymmetric unit of the title salt C8H22N42+·2C7H5O2−, comprises two independent pairs of half a 2,2′-(piperazine-1,4-diyldiethanaminium dication plus a benzoate anion. The dications are symmetrical and lie across crystallographic centres of inversion. The crystal structure was refined as a two-component pseudo-merohedral twin using the twin law 001 0-10 100 [he domain fractions are 0.8645 (8 and 0.1355 (8]. The anions and cations are linked by N—H...O hydrogen bonds and weak N—H...O intermolecular interactions to form infinite two-dimensional networks parallel to [101]. The conformation adopted by the cation in the crystal structure is very similar to that adopted by the same cation in the structures of the 2-hydroxybenzoate [Cukrowski et al. (2012. Acta Cryst, E68, o2387], the nitrate and the tetrahydrogen pentaborate salts.

  10. (R C,S Fe)-1-[3,5-Bis(trifluoro­meth­yl)phen­yl]-3-{1-[2-(diphenyl­phosphan­yl)ferro­cen­yl]eth­yl}thio­urea (unknown solvate)

    Science.gov (United States)

    Ma, Peng-Fei; Zhang, Xiao-Rui; Ma, Jiang-Wei; Chen, Hui; Jiang, Ru

    2013-01-01

    In the molecule of the the title compound, [Fe(C5H5)(C28H22F6N2PS)], the absolute configuration is R C ,SFe. The dihedral angle between the trifluoro­methyl-substituted phenyl ring and the thio­urea plane is 41.8 (9)°. The iron atom is bound to the cyclo­penta­dienyl rings in the typical η5-manner in a close to eclipsed conformation. The crystal structure features N—H⋯S hydrogen bonds, with the S atom as an acceptor for both N—H groups, forming a layered arrangement parallel to (1-10). The two –CF3 groups are each disordered over two positions with refined occupancy rates for the major components of 0.66 (7) and 0.55 (5). The crystal was grown from mixed solvents (n-hexane and ethyl acetate). These solvents are disordered in the crystal and the resulting electron density was found to be uninterpretable. The solvent contribution to the structure factors was taken into account by back-Fourier transformation of all density found in the disordered solvent area using the SQUEEZE routine in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148–155]. The formula mass and density do not take account of the solvent. PMID:23723760

  11. trans-Dichloridobis{dicyclo­hex­yl[4-(dimethyl­amino)­phen­yl]phosphane-κP}platinum(II) dichloro­methane disolvate

    Science.gov (United States)

    Davis, Wade L.; Meijboom, Reinout

    2012-01-01

    In the title complex, trans-[PtCl2{P(C6H11)2(4-Me2NC6H4)}2]·2CH2Cl2, the PtII atom is located on an inversion centre, resulting in a trans-square-planar geometry. Important geometric parameters are the Pt—P and Pt—Cl bond lengths of 2.3258 (6) and 2.3106 (6) Å, respectively, and the P—Pt—Cl angles of 89.64 (2) and 90.36 (2)°. The effective cone angle for the dicyclo­hex­yl[4-(dimethyl­amino)­phen­yl]phosphane unit was calculated to be 164°. The compound crystallizes with two dichloro­methane solvent mol­ecules; one of which is severely disordered and was treated using the SQUEEZE routine in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148–155]. PMID:23468763

  12. Crystal structure of ethyl 3-amino-6-methyl-2-[(4-methyl-phen-yl)carbamo-yl]-4-[(E)-2-phenyl-ethen-yl]thieno[2,3-b]pyridine-5-carboxyl-ate monohydrate.

    Science.gov (United States)

    Mague, Joel T; Akkurt, Mehmet; Mohamed, Shaaban K; Bakhite, Etify A; Albayati, Mustafa R

    2016-03-01

    In the title mol-ecule, C27H25N3O3S·H2O, the dihedral angle between the planes of the thienyl ring and the pendant p-tolyl group is 39.25 (6)°, while that between the pyridine ring and the pendant phenyl ring is 44.37 (6)°. In addition, there is a slight twist in the bicyclic core, with a dihedral angle of 2.39 (4)° between the thienyl and pyridine rings. The conformation of the carbamoyl moiety is partially determined by an intra-molecular N-H⋯O hydrogen bond. In the crystal, complementary N-H⋯O hydrogen bonds form dimers which are then associated into chains parallel to the c axis through O-H⋯N hydrogen bonds involving the water mol-ecule of crystallization. Electron density associated with an additional solvent mol-ecule of partial occupancy and disordered about a twofold axis was removed with the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9-18]. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s).

  13. Crystal structure of an unknown tetra­hydro­furan solvate of tetra­kis­(μ 3-cyanato-κ3 N:N:N)tetra­kis­[(triphenyl­phosphane-κP)­silver(I)

    Science.gov (United States)

    Frenzel, Peter; Schaarschmidt, Dieter; Jakob, Alexander; Lang, Heinrich

    2015-01-01

    In the title compound, [{[(C6H5)3P]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 μ 3-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 (d 10⋯d 10) 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. PMID:26594421

  14. Crystal structure of 2-[(3S,4S)-4-(anthracen-9-yl)-1-(4-meth­oxy­phen­yl)-2-oxoazetidin-3-yl]-2-aza-2H-phenalene-1,3-dione unknown solvate

    Science.gov (United States)

    Çelik, Ísmail; Akkurt, Mehmet; Jarrahpour, Aliasghar; Rad, Javad Ameri; Çelik, Ömer

    2015-01-01

    The central β-lactam ring of the title compound, C36H24N2O4, is almost planar (r.m.s. deviation = 0.003 Å) and makes dihedral angles of 17.17 (19), 89.76 (17) and 78.44 (17)° with the benzene ring, the anthracene ring (r.m.s. deviation = 0.003 Å) and the 1H-benzo[de]iso­quinoline-1,3(2H)-dione moiety, which is nearly planar [maximum deviation = 0.098 (2) Å], respectively. The mol­ecular structure is stabilized by an intra­molecular C—H⋯N hydrogen bond. In the crystal, mol­ecules are linked via C—H⋯π and π–π stacking inter­actions [centroid–centroid distances = 3.5270 (19) and 3.779 (2) Å], forming a three-dimensional structure. A region of disordered electron density, probably disordered solvent mol­ecules, was treated with the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18], which indicated a solvent cavity of 322 Å3 containing approximately 91 electrons. Their formula mass and unit-cell characteristics were not taken into account during the refinement. PMID:25844239

  15. Crystal structure of an unknown solvate of bis­(tetra-n-butyl­ammonium) [N,N′-(4-tri­fluoro­methyl-1,2-phenyl­ene)bis­(oxamato)-κ4 O,N,N′,O′]nickelate(II)

    Science.gov (United States)

    Eya’ane Meva, François; Schaarschmidt, Dieter; Rüffer, Tobias

    2015-01-01

    In the title compound, [N(C4H9)4]2[Ni(C11H3F3N2O6)] or [N(n-Bu)4]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. PMID:26090126

  16. (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.

  17. CREDO: a protein-ligand interaction database for drug discovery.

    Science.gov (United States)

    Schreyer, Adrian; Blundell, Tom

    2009-02-01

    Harnessing data from the growing number of protein-ligand complexes in the Protein Data Bank is an important task in drug discovery. In order to benefit from the abundance of three-dimensional structures, structural data must be integrated with sequence as well as chemical data and the protein-small molecule interactions characterized structurally at the inter-atomic level. In this study, we present CREDO, a new publicly available database of protein-ligand interactions, which represents contacts as structural interaction fingerprints, implements novel features and is completely scriptable through its application programming interface. Features of CREDO include implementation of molecular shape descriptors with ultrafast shape recognition, fragmentation of ligands in the Protein Data Bank, sequence-to-structure mapping and the identification of approved drugs. Selected analyses of these key features are presented to highlight a range of potential applications of CREDO. The CREDO dataset has been released into the public domain together with the application programming interface under a Creative Commons license at http://www-cryst.bioc.cam.ac.uk/credo. We believe that the free availability and numerous features of CREDO database will be useful not only for commercial but also for academia-driven drug discovery programmes.

  18. An orthorhombic polymorph of N1,N4-diphenyl-3,6-bis(phenyliminocyclohexa-1,4-diene-1,4-diamine

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    Keiji Ohno

    2014-04-01

    Full Text Available A new orthorhombic polymorph of the title compound, C30H24N4, with a density of 1.315 Mg m−3, has been obtained. The molecule is centrosymmetric with the centroid of the cyclohexa-1,4-diene ring located on an inversion center. The two unique benzene rings are almost perpendicular to each other [dihedral angle = 86.70 (6°] and are oriented at dihedral angles of 30.79 (5 and 68.07 (5° with respect to the central cyclohexadiene ring. In the crystal, π–π stacking is observed between the central cyclohexa-1,4-diene-1,4-diamine unit and a phenyl ring of a neighboring molecule [centroid–centroid distance = 3.7043 (7 Å]. The crystal structure of the triclinic polymorph [Ohno et al. (2014. Acta Cryst. E70, o303–o304] showed chains running along the b-axis direction through weak C—H...π interactions.

  19. catena-Poly[[diaquabis(4-formylbenzoato-κO1nickel(II]-μ-pyrazine-κ2N:N′

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    Fatih Çelik

    2014-02-01

    Full Text Available In the title polymeric compound, [Ni(C8H5O32(C4H4N2(H2O2]n, the NiII atom is located on a twofold rotation axis and has a slightly distorted octahedral coordination sphere. In the equatorial plane, it is coordinated by two carboxylate O atoms of two symmetry-related monodentate formylbenzoate anions and by two N atoms of the bridging pyrazine ligand, which is bisected by the twofold rotation axis. The axial positions are occupied by two O atoms of the coordinating water molecules. In the formylbenzoate anion, the carboxylate group is twisted away from the attached benzene ring by 7.0 (6°, while the benzene and pyrazine rings are oriented at a dihedral angle of 66.2 (3°. The pyrazine ligands bridge the NiII cations, forming polymeric chains running along the b-axis direction. Intramolecular O—H...O hydrogen bonds link the water ligands to the carboxylate O atoms. In the crystal, water–water O—H...O hydrogen bonds link adjacent chains into layers parallel to the bc plane. Pyrazine–formyl C—H...O hydrogen bonds link the layers, forming a three-dimensional network. There are also weak C—H...π interactions present. The title compound is isotypic with the copper(II complex [Çelik et al. (2014a. Acta Cryst. E70, m4–m5].

  20. A P212121 polymorph of (+-clusianone

    Directory of Open Access Journals (Sweden)

    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.

  1. Growth and morphology of a 4PtO 6 crystals

    Science.gov (United States)

    Ohsato, H.; Sugimura, T.; Kageyama, K.

    1981-01-01

    Single crystals of Ca 4PtO 6 were precipitated from molten CaCl 2 in a wet atmosphere at 800-1000°C. Above 900°C, CaO single crystals coexisted. The Ca 4PtO 6 crystals obtained were transparent with pale brown or pale yellow colour, and were mostly granular, about 1 mm in size. The crystal habit was a combination of the {112¯0}, {101¯0}, {101¯2}, {011¯1} and {202¯1} cryst al faces. Some prismatic crystals were found, 2 mm long and 0.1 mm wide. They were found to be twinned with the (10-0) plane. The crystal has a trigonal unit cell with a = 9.332 Å, c = 11.26 Å; and with six formula units of which the space group is R—c. It is uniaxial positive with refractive indices 1.85 hydrochloric acid. The growth mechanism of Ca 4PtO 6 crystals was also discussed.

  2. FROM WATER BY NANOFILTRATION

    Directory of Open Access Journals (Sweden)

    A. Torabian, G.R.Nabi Bihdendi, P. Zanganeh Ranjbar, N. Razmkhah

    2007-07-01

    Full Text Available Nanofiltration, widely developed over the past decade, is a promising technology for the treatment of organic and inorganic pollutants in surface and groundwater resources. The aim of the present research was to study the efficiency of textile dyes removal by a commercial nanofilter NF90 (Dow-Film Tec. Dye rejection was studied using basic dye (Basic Chrysoidine Cryst Yellow Gold 0.4% with its relevant additive. Experiments were continued until the fouling time of the membrane. Each experiment was repeated after washing to evaluate the efficiency of the washing process. Results showed that the values of color removal were 97.98 % for the simulated textile wastewater containing basic dye. The membrane was sensitive to fouling since most of dyes were used for polyamide textile dyeing. Washing the membrane with a solution including NaOH (pH=12 and HCl (pH=2 showed its efficiency to solve the fouling problem. The filtration process was efficient and promising for reusing wastewater in this industry.

  3. 高效液相色谱法测定秸秆浸提液或腐解液中12种酚酸%Determination of 12 phenolic acids in straw extract or straw decomposed liquid through high performance liq-uid chromatography

    Institute of Scientific and Technical Information of China (English)

    于建光; 常志州; 王宁; 石祖梁; 卢信; 张传辉

    2016-01-01

    A method of reversed phase high performance liquid chromatography was established, which could be used to determine the con-tents of 12 phenolic acids(gallic acid, protocatechuic acid, gentisic acid, p-hydroxybenzoic acid, chlorogenic acid, vanilla acid, coffee acid, syringic acid, p-coumaric acid, ferulic acid, sinapic acid, salicylic acid)simultaneously in straw extract or decomposed liquid. Waters HLB (500 mg, 60μm, 6 mL)solid-phase extraction cartridges were used to concentrate phenolic acids in aqueous solution. The gradient elution was carried out using acetonitrile solution containing 0.5%acetic acid and 0.5%acetic acid solution as the mobile phase. The diode array detector was used for detection, and the determination of 12 kinds of phenolic acids could be completed simultaneously in 30 minutes. All of phenolic acids could reach the baseline separation. The recovery rate of 12 phenolic acids were between 79.41%~101.92%, and the RSD of retention time and peak area of 12 phenolic acids were between 0.02%~0.1%and 0.25%~2.26%, respectively. This method is rapid, sensi-tive and accurate, suitable for the simultaneous determination of 12 phenolic acids existed in straw extract, straw decomposed liquid, soil so-lution and aqueous solution.%建立了同时测定秸秆浸提液或腐解液中12种酚酸物质(没食子酸、原儿茶酸、龙胆酸、对羟基苯甲酸、绿原酸、香草酸、咖啡酸、丁香酸、对香豆酸、阿魏酸、芥子酸、水杨酸)的反相高效液相色谱测定方法。采用Waters HLB(500 mg、60μm、6 mL)固相萃取小柱对水溶液中的酚酸物质进行浓缩,以含0.5%乙酸的乙腈和0.5%乙酸的水溶液为流动相进行梯度洗脱,选用二极管阵列检测器,30 min内可对12种酚酸物质同时检测,各种酚酸均可达到基线分离。加标回收试验表明,样品中12种酚酸类化合物的加标回收率为79.41%~101.92%,12种酚酸保留时间和峰面积的RSD分别在0.02%~0.1%和0.25%~2.26%之间。该方法快速、灵敏、准确,适用于同时测定秸秆浸提液、腐解液、土壤溶液及水溶液中12种酚酸物质含量。

  4. Study of ion implanted Al0.25Ga0.75As/GaAs by Raman spectroscopy

    Institute of Scientific and Technical Information of China (English)

    LIU; Pijun

    2001-01-01

    [1]Ramam, A., Chua, S. J., Luminescence anomaly in band gap tailored In0.35(GaxAl1-x)0.47As quaternary alloy growth by molecular beam epitaxy, J. Cryst. Growth, 1997, 175: 1294.[2]Xu, X. G., Huang, B. B., Ren, H. W. et al., Study on the stability of GaAs/AlGaAs superlattice structure, Acta Physica Sinica (Overseas Edition), 1995, 4: 47.[3]Yoon, S. F., Miao, Y. B., Radhakrishnan, K., Some characteristic of silicon-doped In0.52Al0.48As grown lattice-matched on InP substrates by molecular beam epitaxy, Thin. Solid Films, 1996, 287: 284.[4]Nakamura, K., Fuyuki, T., Matsunami, H., Strain in GaP films heteroepitaxially grown in Si by Metalorganic Chemical Vapor Deposition, Jan. J. Appl. Phys., 1998, 37: 4231.[5]Sadao Adachi, GaAs, AlAs, and AlxGa1-xAs: Material parameters for use in research and device applications, J. Appl. Phys., 1985, 58: R1.[6]Attolini, G., Francesio, L., Franzosi, P. et al., Raman scattering study of residual strain in GaAs/InP heterostructures, J. Appl. Phys., 1994, 75: 4156.[7]Helmy, A. S., Bryce, A. C., Ironside, C. N. et al., Raman spectroscopy for characterizing compositional intermixing in GaAs/AlGaAs heterostructures, Appl. Phys. Lett., 1999, 74: 3978.[8]Jencic, I., Bench, M. W., Robertson, I. M. et al., A comparison of the amorphization induced in AlxGa1-xAs and GaAs by heavy-ion irradiation, J. Appl. Phys., 1991, 69: 1287.[9]Wickboldt, P., Anastassakis, E., Sauer, R. et al., Raman phonon piezospectroscopy in GaAs: Infrared measurements, Phys. Rev. B, 1987, 35: 1362.[10]Leng, J., Qian, Y., Chen, P. et al., Disorder activated optical modes and the phonon dispersion of AlxGa1-xAs lattice vibration, Solid State Commun., 1989, 69: 311.[11]Wagner, A., Koidl, P., Newman, P. G., Resonance effects in Raman scattering by dopant-induced local vibrational modes in III-V semiconductors, Appl. Phys. Lett., 1991, 59: 1729.[12]Masayuki Sugiura, Masato Kishi, Takashi Katoda, In situ observation of the strain

  5. Determining the melting curves of NiSi using the laser-heated diamond anvil cell and the multi-anvil press

    Science.gov (United States)

    Wann, E.; Lord, O. T.; Dobson, D. P.; Hunt, S. A.; Wood, I. G.; Vocadlo, L.; Ahmed, J.; Walker, A. M.; Santangeli, J. R.; Walter, M. J.

    2012-12-01

    . Physics of the Earth and Planetary Interiors 1994, 85, 319. (3) Gessmann, C. K.; Wood, B. J.; Rubie, D. C.; Kilburn, M. R. Earth and Planetary Science Letters 2001, 184, 367. (4) Lord, O. T.; Voccadlo, L.; Wood, I. G.; Dobson, D. P.; Clark, S. M.; Walter, M. J. J. Appl. Cryst. 2012, 45, 726 (5) Vočadlo, L.; Wood, I. G.; Dobson, D. J Appl Cryst. 2012, 45, 186. (6) Lord, O. T., Walter, M. J., Dobson, D. P., Armstrong, L., Clark, S. M., Kleppe, A. J. Geophys. Res., 2010, 115, B06208.

  6. Dielectric and Optical Properties of CdS-Polymer Nanocomposites Prepared by the Successive Ionic Layer Adsorption and Reaction (SILAR) Method

    Science.gov (United States)

    Azizian-Kalandaragh, Yashar; Aydemir, Umut; Altindal, Şemsettin

    2014-04-01

    The successive ionic layer adsorption and reaction (SILAR) method has been used to grow epitaxial CdS-polymer nanostructures as thin films with different surface morphology and particle size. The main purpose of the study was to investigate the dielectric properties and a.c. electrical conductivity ( σ a.c.), by a.c. impedance spectroscopy between 1 kHz and 1 MHz, at room temperature, of CdS-polymer nanocomposites produced by use of 2, 6, and 10 cycles of SILAR. The surface morphology and optical absorption of the samples were characterized by scanning electron microscopy (SEM) and UV-visible spectroscopy, respectively. Determination of the energy gaps of CdS-polymer nanocomposites prepared by use of different numbers of cycles of SILAR reveals that the band gap decreases with increasing number of cycles (J. Cryst. Growth 305, 175-180, 2007). This behavior is because of the growth of nanoparticles in the matrix materials, and can be explained by changes in the amount of confinement as a consequence of particle size variation. SEM images also confirm that different numbers of cycles lead to different morphology. Frequency-dependent dielectric properties and a.c. electrical conductivity of the samples prepared by use of different numbers of cycles of SILAR were investigated, and comparative studies on some electrophysical properties of the samples are reported. Experimental results show that values of the dielectric constant ( ɛ'), dielectric loss ( ɛ″), dielectric loss tangent (tan δ), the real ( M') and imaginary ( M″) parts of electric modulus, and σ a.c. are highly dependent on the frequency and the number of cycles. It can be concluded that changing the frequency and the number of cycles substantially alters both the dielectric properties and a.c. electrical conductivity of the samples.

  7. Three phenanthroline–metal complexes with topologically similar but geometrically different conformations

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    Miguel Angel Harvey

    2016-11-01

    Full Text Available The structures of three related complexes of general formula M(pds(nab2 [pds is the peroxodisulfate anion and nab is an nitrogen-containing aromatic base], viz. bis(2,9-dimethyl-1,10-phenanthroline-κ2N,N′(peroxodisulfato-κ2O,O′cadmium, [Cd(S2O8(C14H12N22], (V, bis(3,4,7,8-tetramethy-1,10-phenanthroline-κ2N,N′(peroxodisulfato-κ2O,O′zinc, [Zn(S2O8(C16H16N22], (VI, and bis(3,4,7,8-tetramethy-1,10-phenanthroline-κ2N,N′(peroxodisulfato-κ2O,O′cadmium, [Cd(S2O8(C16H16N22], (VII, present the same topological coordination, with three chelating ligands in an MN4O2 polyhedron. The main difference resides in the fact that the first two complexes are bisected by a crystallographic twofold axis, thus providing a symmetrical environment to the cation, while in the third one this symmetry is disrupted into a clearly unsymmetrical disposition, probably by way of an unusually strong intramolecular C—H...O hydrogen bond. The situation is compared with similar interactions in the literature. The structure of (V is based on a redetermination in the correct space group C2/c of the structure originally described in the Cc space group [Harvey et al. (2001. Aust. J. Chem. 54, 307–311; Marsh (2004. Acta Cryst. B60, 252–253].

  8. Sulfur Solubility In Silicate Melts: A Thermochemical Model

    Science.gov (United States)

    Moretti, R.; Ottonello, G.

    A termochemical model for calculating sulfur solubility of simple and complex silicate melts has been developed in the framework of the Toop-Samis polymeric approach combined with a Flood - Grjotheim theoretical treatment of silicate slags [1,2]. The model allows one to compute sulfide and sulfate content of silicate melts whenever fugacity of gaseous sulphur is provided. "Electrically equivalent ion fractions" are needed to weigh the contribution of the various disproportion reactions of the type: MOmelt + 1/2S2 ,gas MSmelt+1/2O2 ,gas (1) MOmelt + 1/2S2 ,gas + 3/2O2 ,gas MSO4 ,melt (2) Eqs. 1 and 2 account for the oxide-sulfide and the oxide-sulfate disproportiona- tion in silicate melt. Electrically equivalent ion fractions are computed, in a fused salt Temkin notation, over the appropriate matrixes (anionic and cationic). The extension of such matrixes is calculated in the framework of a polymeric model previously developed [1,2,3] and based on a parameterization of acid-base properties of melts. No adjustable parameters are used and model activities follow the raoultian behavior implicit in the ion matrix solution of the Temkin notation. The model is based on a huge amount of data available in literature and displays a high heuristic capability with virtually no compositional limits, as long as the structural role assigned to each oxide holds. REFERENCES: [1] Ottonello G., Moretti R., Marini L. and Vetuschi Zuccolini M. (2001), Chem. Geol., 174, 157-179. [2] Moretti R. (2002) PhD Thesis, University of Pisa. [3] Ottonello G. (2001) J. Non-Cryst. Solids, 282, 72-85.

  9. Crystal structures of 2-(4-nitrophenyl-3-phenyl-2,3-dihydro-4H-1,3-benzothiazin-4-one and 2-(2-nitrophenyl-3-phenyl-2,3-dihydro-4H-1,3-benzothiazin-4-one

    Directory of Open Access Journals (Sweden)

    Hemant Yennawar

    2015-04-01

    Full Text Available The crystal structures are reported of the isomeric compounds 2-(4-nitrophenyl-3-phenyl-2,3-dihydro-4H-1,3-benzothiazin-4-one, (I, and 2-(2-nitrophenyl-3-phenyl-2,3-dihydro-4H-1,3-benzothiazin-4-one, (II, both C20H14N2O3S, being the para-nitro and ortho-nitro forms, respectively, the meta-form of which is known [Yennawar et al. (2013. Acta Cryst. E69, o1679]. The six-membered thiazone ring fused with a benzene ring displays a screw-boat conformation with a total puckering amplitude of 0.627 (1 Å in (I, and a near screw-boat conformation with a total puckering amplitude of 0.600 (1 Å in (II. The dihedral angles between the planes of the substituent nitrophenyl and phenyl and rings with the benzene ring of the parent benzothiazone moiety are 75.93 (5 and 82.61 (5° [in (I], and 76.79 (6 and 71.66 (6° [in (II]. Weak intermolecular C—H...O hydrogen-bonding interactions between aromatic H-atom donors and both a nitro-O atom and a thiazone O-atom acceptor in (I and a thiazone O atom in (II are present, forming in (I a centrosymmetric 22-membered cyclic dimer which is extended through a similar inversion-related 14-membered cyclic hydrogen-bonding association into a zigzag chain structure extending along c. In (II, a single intermolecular C—H...O hydrogen bond gives a chain structure extending along b. In addition, weak C—H...π interactions are present in both structures [minimum C...ring-centroid separations = 3.630 (2 and 3.581 (2 Å, respectively].

  10. Electron densities by the maximum entropy method (MEM) for various types of prior densities: a case study on three amino acids and a tripeptide.

    Science.gov (United States)

    Prathapa, Siriyara Jagannatha; Mondal, Swastik; van Smaalen, Sander

    2013-04-01

    Dynamic model densities according to Mondal et al. [(2012), Acta Cryst. A68, 568-581] are presented for independent atom models (IAM), IAMs after high-order refinements (IAM-HO), invariom (INV) models and multipole (MP) models of α-glycine, DL-serine, L-alanine and Ala-Tyr-Ala at T ≃ 20 K. Each dynamic model density is used as prior in the calculation of electron density according to the maximum entropy method (MEM). We show that at the bond-critical points (BCPs) of covalent C-C and C-N bonds the IAM-HO and INV priors produce reliable MEM density maps, including reliable values for the density and its Laplacian. The agreement between these MEM density maps and dynamic MP density maps is less good for polar C-O bonds, which is explained by the large spread of values of topological descriptors of C-O bonds in static MP densities. The density and Laplacian at BCPs of hydrogen bonds have similar values in MEM density maps obtained with all four kinds of prior densities. This feature is related to the smaller spatial variation of the densities in these regions, as expressed by small magnitudes of the Laplacians and the densities. It is concluded that the use of the IAM-HO prior instead of the IAM prior leads to improved MEM density maps. This observation shows interesting parallels to MP refinements, where the use of the IAM-HO as an initial model is the accepted procedure for solving MP parameters. A deconvolution of thermal motion and static density that is better than the deconvolution of the IAM appears to be necessary in order to arrive at the best MP models as well as at the best MEM densities.

  11. 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.

  12. Structure of iron saturated C-lobe of bovine lactoferrin at pH 6.8 indicates a weakening of iron coordination.

    Science.gov (United States)

    Rastogi, Nilisha; Singh, Avinash; Singh, Prashant K; Tyagi, Tapesh K; Pandey, Sada; Shin, Kouichirou; Kaur, Punit; Sharma, Sujata; Singh, Tej P

    2016-05-01

    The bilobal lactoferrin is an approximately 76 kDa glycoprotein. It sequesters two Fe(3+) ions together with two CO(3)(2-) ions. The C-terminal half (residues, Tyr342-Arg689, C-lobe) of bovine lactoferrin (BLF) (residues Ala1-Arg689) was prepared by limited proteolysis using trypsin. Both C-lobe and intact BLF were saturated to 100%. Both of them retained up to nearly 85% of iron at pH 6.5. At pH 5.0, C-lobe retained 75% of iron whereas intact protein could retain only slightly more than 60%. At pH 4.0 both contained 25% iron and at pH 2.0 they were left with iron concentration of only 10%. The structure of iron saturated C-lobe was determined at 2.79 Å resolution and refined to R(cryst) and R(free) factors of 0.205 and 0.273, respectively. The structure contains two crystallographically independent molecules, A and B. They were found to have identical structures with an r.m.s. shift of 0.5 Å for their C(α) atoms. A high solvent content of 66% was observed in the crystals. The average value of an overall B-factor was 68.0 Å(2). The distance of 2.9 Å observed for the coordination bond between Fe(3+) ion and N(e2) of His595 appeared to be considerably longer than the normally observed values of 1.9-2.2 Å. This indicated that the coordination bond involving His595 may be absent. Other coordination distances were observed in the range of 2.1-2.3 Å. Based on the present structure of iron saturated C-lobe, it may be stated that His595 is the first residue to dissociate from ferric ion when the pH is lowered.

  13. Crystal structure of tetra-kis-[μ2-2-(di-methyl-amino)-ethano-lato-κ(3) N,O:O]di-μ3-hydroxido-di-thio-cyanato-κ(2) N-dichromium(III)dilead(II) di-thio-cyanate aceto-nitrile monosolvate.

    Science.gov (United States)

    Rusanova, Julia A; Semenaka, Valentyna V; Omelchenko, Irina V

    2016-04-01

    The tetra-nuclear complex cation of the title compound, [Cr2Pb2(NCS)2(OH)2(C4H10NO)4](SCN)2·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 Cr(III) ion is coordinated in a distorted octa-hedron, which involves two N atoms of one bidentate ligand and one thio-cyanate anion, two μ2-O atoms of 2-(di-methyl-amino)-ethano-late ligands and two μ3-O atoms of hydroxide ions. The coordination geometry of the Pb(II) ion is a distorted disphenoid, which involves one N atom, two μ2-O atoms and one μ3-O atom. In addition, weak Pb⋯S inter-actions involving the coordinating and non-coordinating thio-cyanate anions are observed. In the crystal, the complex cations are linked through the thio-cyanate anions via the Pb⋯S inter-actions 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 aceto-nitrile mol-ecule was removed with the SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9-18] procedure in PLATON. The solvent is included in the reported mol-ecular formula, weight and density.

  14. On the theoretical determination of the Prigogine-Defay ratio in glass transition

    Science.gov (United States)

    Tropin, Timur V.; Schmelzer, Jürn W. P.; Gutzow, Ivan; Schick, Christoph

    2012-03-01

    In a recent analysis [J. W. P. Schmelzer and I. Gutzow, J. Chem. Phys. 125, 184511 (2006), 10.1063/1.2374894] it was shown for the first time that - in contrast to earlier belief arising from the works of Prigogine and Defay [Chemical Thermodynamics (Longman, London, 1954), Chap. 19; The first French edition of this book was published in 1950] and Davies and Jones [Adv. Phys. 2, 370 (1953), 10.1080/00018735300101252; Davies and Jones Proc. R. Soc. London, Ser. A 217, 26 (1953), 10.1098/rspa.1953.0044] - a satisfactory theoretical interpretation of the experimentally observed values of the so-called Prigogine-Defay ratio Π, being a combination of jumps of thermodynamic coefficients at glass transition, can be given employing only one structural order parameter. According to this analysis, this ratio has to be, in full agreement with experimental findings, larger than one (Π > 1). Its particular value depends both on the thermodynamic properties of the system under consideration and on cooling and heating rates. Based on above-mentioned analysis, latter dependence on cooling rates has been studied in detail in another own preceding paper [T. V. Tropin, J. W. P. Schmelzer, and C. Schick, J. Non-Cryst. Solids 357, 1303 (2011), 10.1016/j.jnoncrysol.2010.12.005]. In the present analysis, an alternative general method of determination of the Prigogine-Defay ratio is outlined, allowing one to determine this ratio having at ones disposal the generalized equation of state of the glass-forming melts under consideration and, in particular, the knowledge of the equilibrium properties of the melts in the glass transformation range. Employing, as an illustration of the method, a particular model for the description of glass-forming melts, theoretical estimates are given for this ratio being, again, in good agreement with experimental data.

  15. Effect of Different pH Hydrogen Peroxide Bleaching on Human Dentin Color and Transparency%不同pH值过氧化氢漂白影响人牙本质颜色及透明度的对比及机制初探

    Institute of Scientific and Technical Information of China (English)

    王苏豫; 李冬霞

    2015-01-01

    目的:探讨不同pH值过氧化氢溶液对牙本质颜色和透明度的影响.方法:将30颗刚拔除的人前磨牙随机分为两组,每组15例,沿牙长轴剖开、去髓,使用pH=4.5和pH=7.0的两种过氧化氢溶液分别进行漂白,用Crystaleye电脑比色仪观察牙本质颜色和透明度的变化,以及与时间的关系,初步分析其机制.结果:pH=7.0过氧化氢溶液漂白1周后牙本质颜色变黄,透明度下降,基质金属蛋白酶活性下降.pH=4.5过氧化氢溶液漂白1周后牙本质颜色变黄,透明度下降,3周后部分牙本质颜色恢复,同时基质金属蛋白酶活性升高,两组差异有统计学意义(P<0.05).结论::pH=7.0的过氧化氢溶液氧化性较强,对牙本质的破坏较大,pH=4.5过氧化氢溶液对牙本质破坏性略低.其机制与牙源性基质金属蛋白酶活性有关.

  16. 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.

  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. 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.

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

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    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.

  20. Redetermined structure of gossypol (P3 polymorph

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    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.

  1. μ-XRF analysis of glasses: a non-destructive utility for Cultural Heritage applications.

    Science.gov (United States)

    Vaggelli, G; Cossio, R

    2012-02-07

    This paper presents a μ-XRF analytical approach for a non-destructive study of Cultural Heritage glass finds. This technique can be used for quantitative analysis of small volumes of solid samples, with a sensitivity that is superior to the electron microprobe but inferior to an ICP-MS system. An experimental set-up with natural and synthetic glass standards is proposed here for the quantitative analyses of major and trace elements on glass objects which cannot be sampled such as small archaeological or historical artefacts from Cultural Heritage. The described method, performed by means of the commercial μ-XRF Eagle III-XPL, was applied to Islamic glass specimens of Sasanian production (III-VII century A.D.) previously analyzed by ICP-MS and SEM-EDS techniques (P. Mirti, M. Pace, M. Negro Ponzi and M. Aceto, Archaeometry, 2008, 50(3), 429-450; P. Mirti, M. Pace, M. Malandrino and M. Negro Ponzi, J. Archaeol. Sci., 36, 1061-1069; and M. Gulmini, M. Pace, G. Ivaldi, M. Negro Ponzi and P. Mirti, J. Non-Cryst. Solids, 2009, 355, 1613-1621) and coming from the archaeological site of Veh Ardasir in modern Iraq. Major elements (Na, Mg, Al, Si, K, Ca, Fe) of glass specimens show an accuracy better than 5%. Trace elements (Cr, Mn, Sr and Zr) display an accuracy better than 5% when the checked elements have a concentration >100 ppm by weight, whereas it is around 10% with a concentration <100 ppm by weight. μ-XRF is, therefore, a suitable elemental analysis technique for the non-destructive study of small glass finds due to its relatively good accuracy, reproducibility and low detection limits (∼tens ppm).

  2. The influence of the stereochemistry of alanine residue on the solid state conformation and crystal packing of opioid peptides containing D-Ala or L-Ala in message domain--XRD and NMR study.

    Science.gov (United States)

    Trzeciak-Karlikowska, Katarzyna; Bujacz, Anna; Ciesielski, Włodzimierz; Bujacz, Grzegorz D; Potrzebowski, Marek J

    2011-08-18

    In this work, an X-ray diffraction (XRD) and solid state NMR study of two tetrapeptides with different stereochemistry of alanine residue is presented using Tyr-(D-Ala)-Phe-Gly (1), an N-terminal sequence of opioid peptide dermorphin, and its biologically inactive analog Tyr-(L-Ala)-Phe-Gly (2). Single-crystal XRD proved that 1 crystallized under different conditions from exclusively one structure: a monoclinic crystal with P2(1) space group. In contrast, 2 very easily formed at least three crystallographic modifications, 2a (monoclinic P2(1)), 2b (orthorhombic P2(1)2(1)2) and 2c (tetragonal P4(1)2(1)2). Solid-state NMR spectroscopy was employed to investigate the structure and molecular dynamics of 1, 2a, and 2b. By employing different NMR experiments (dipolar dephasing and PILGRIM) and an analysis of the (13)C principal elements of the chemical shift tensor (CST), it was proven that the main skeleton of tetrapeptides is rigid, whereas significant differences in the molecular motion of the aromatic residues were observed. Comparing current data with those of previous studies (J. Phys. Chem. B2004, 108, 4535-4545 and Cryst. Growth Des. 2009, 9, 4050-4059), it can be assumed that an important preorganization mechanism anticipating the formation of peptide crystals containing D-Ala in sequence is the intramolecular CH-π interaction, which occurs for the amino acid with D stereochemistry. This effect may be responsible for the formation of only one crystallographic form of D-Ala peptides.

  3. Patterson-function direct methods for structure determination of organic compounds from powder diffraction data. XVI.

    Science.gov (United States)

    Rius, Jordi

    2011-01-01

    A new type of direct methods (DM) called Patterson-function DM are presented that directly explore the Patterson instead of the modulus function. Since they work with the experimental intensities, they are particularly well suited for handling powder diffraction data. These methods are based on the maximization of the sum function S(P) ∝ ∑H(I(H)-)G(-H)(Φ) in terms of the Φ phases of the structure factors. The quantity accessible from the experiment is I(H), the equidistributed multiplet intensity of reflection H, and is the average intensity taken over all non-systematically absent reflections. G(-H)(Φ) is the calculated structure-factor amplitude of the squared structure that includes the positivity and the atomicity of the density function in its definition. The S(P) sum function can be optimized with the Patterson-function tangent formula (TF) using a variant of the S-FFT algorithm [Rius et al. (2007), Acta Cryst. A63, 131-134]. It is important that overlapped reflections also participate in the phase refinement, so that not only the resolved reflections but the whole pattern contribute decisively to the refinement. The increase in effective data resolution minimizes Fourier series termination effects and improves the accuracy of G(Φ). The Patterson-function TF has been applied to synchrotron powder data of various organic compounds. In all cases the molecules were easily identified in the respective Fourier maps. By way of illustration the method is applied to synchrotron powder data of a dimer formed by 30 symmetry-independent non-H atoms. Since single-crystal data may be regarded as overlap-free powder data, it is clear that Patterson-function DM can cope with powder and single-crystal data.

  4. Crystal structures of deuterated sodium molybdate dihydrate and sodium tungstate dihydrate from time-of-flight neutron powder diffraction.

    Science.gov (United States)

    Fortes, A Dominic

    2015-07-01

    Time-of-flight neutron powder diffraction data have been measured from ∼90 mol% deuterated isotopologues of Na2MoO4·2H2O and Na2WO4·2H2O at 295 K to a resolution of sin (θ)/λ = 0.77 Å(-1). The use of neutrons has allowed refinement of structural parameters with a precision that varies by a factor of two from the heaviest to the lightest atoms; this contrasts with the X-ray based refinements where precision may be > 20× poorer for O atoms in the presence of atoms such as Mo and W. The accuracy and precision of inter-atomic distances and angles are in excellent agreement with recent X-ray single-crystal structure refinements whilst also completing our view of the hydrogen-bond geometry to the same degree of statistical certainty. The two structures are isotypic, space-group Pbca, with all atoms occupying general positions, being comprised of edge- and corner-sharing NaO5 and NaO6 polyhedra that form layers parallel with (010) inter-leaved with planes of XO4 (X = Mo, W) tetra-hedra that are linked by chains of water mol-ecules along [100] and [001]. The complete structure is identical with the previously described molybdate [Capitelli et al. (2006 ▸). Asian J. Chem. 18, 2856-2860] but shows that the purported three-centred inter-action involving one of the water mol-ecules in the tungstate [Farrugia (2007 ▸). Acta Cryst. E63, i142] is in fact an ordinary two-centred 'linear' hydrogen bond.

  5. Three phenanthroline-metal complexes with topologically similar but geometrically different conformations.

    Science.gov (United States)

    Harvey, Miguel Angel; Suarez, Sebastián; Baggio, Ricardo

    2016-11-01

    The structures of three related complexes of general formula M(pds)(nab)2 [pds is the peroxodi-sulfate anion and nab is an nitro-gen-containing aromatic base], viz. bis(2,9-dimethyl-1,10-phenanthroline-κ(2)N,N')(peroxodi-sulfato-κ(2)O,O')cadmium, [Cd(S2O8)(C14H12N2)2], (V), bis-(3,4,7,8-tetra-methy-1,10-phenanthroline-κ(2)N,N')(peroxodi-sulfato-κ(2)O,O')zinc, [Zn(S2O8)(C16H16N2)2], (VI), and bis-(3,4,7,8-tetra-methy-1,10-phenanthroline-κ(2)N,N')(peroxodi-sulfato-κ(2)O,O')cadmium, [Cd(S2O8)(C16H16N2)2], (VII), present the same topological coordination, with three chelating ligands in an MN4O2 polyhedron. The main difference resides in the fact that the first two complexes are bis-ected by a crystallographic twofold axis, thus providing a symmetrical environment to the cation, while in the third one this symmetry is disrupted into a clearly unsymmetrical disposition, probably by way of an unusually strong intra-molecular C-H⋯O hydrogen bond. The situation is compared with similar inter-actions in the literature. The structure of (V) is based on a redetermination in the correct space group C2/c of the structure originally described in the Cc space group [Harvey et al. (2001). Aust. J. Chem.54, 307-311; Marsh (2004 ▸). Acta Cryst. B60, 252-253].

  6. 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

  7. 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.

  8. The application of eigensymmetries of face forms to X-ray diffraction intensities of crystals twinned by 'reticular merohedry'.

    Science.gov (United States)

    Klapper, H; Hahn, Th

    2012-01-01

    This paper is an extension of a previous treatment of `twins by merohedry' with full lattice coincidence [Σ = 1, Klapper & Hahn (2010). Acta Cryst. A66, 327-346] to `twins by reticular merohedry' with partial lattice coincidence (Σ > 1). Again, the sets of symmetrically equivalent reflections {hkl} are considered as sets of equivalent faces (face forms) {hkl}, and the behaviour of the oriented eigensymmetries of these forms under the action of a twin operation is used to determine the X-ray reflection sets, the intensities of which are affected or not affected by the twinning. The following cases are treated: rhombohedral obverse/reverse Σ3 twins, cubic Σ3 (spinel) twins, tetragonal Σ5 twins (twin elements m'(120), 2'[ ̅210]) and hexagonal Σ7 twins (m'(12 ̅30), 2'[2 ̅10]). For each case the twin laws for all relevant point groups are defined, and the twin diffraction cases A (intensity of twin-related reflection sets not affected), B1 (intensity affected), B2 (intensity affected only by anomalous scattering) and S (single, i.e. non-coincident reflection sets) are derived for all twin laws. A special treatment is provided for the cubic Σ3 twins, where the cubic face forms first have to be split into up to four rhombohedral subforms with a threefold axis along one of the four cube directions, here [111]. These subforms exhibit different twin diffraction cases analogous to those derived for the rhombohedral obverse/reverse Σ3 twins. A complete list of the split forms and their diffraction cases for all cubic point groups and all Σ3 twin elements is given. The application to crystal structure determination of crystals twinned by reticular merohedry and to X-ray topographic mapping of twin domains is discussed.

  9. Effect of the Ga Content on the Magnetic Properties for the Dual -phase Nanocrystalline Bonded Magnets%微量Ga元素对双相纳米晶磁体性能的影响

    Institute of Scientific and Technical Information of China (English)

    朱明刚; 董生智; 李岫梅; 李卫

    2001-01-01

    探讨了微量的Ga替代Fe对Nd2Fe14B/Fe3B+(少量)α-Fe永磁材料的晶体结构及磁性能的影响。结果表明:添加微量的Ga同样可减小晶粒尺寸;在Ga含量x<1%(原子百分比)的范围,随着x的增加,Br和(BH)max随晶化时间变化的曲线由非线性向线性转化;矫顽力jHc下降到一个最小值后,又缓慢上升;当x=0.2时,综合磁性能较好。%Effect of the Ga content substituting the Fe on the cryst alstructure and magnetic properties for the Nd2Fe14B/Fe3B+(little) α-Fe permanent magnetic materials was discussed. The results show that the crystal size was markedly decresed by adding Ga. With the increase of x, the curves of the Br and the (BH)max change wi th annealing time from non-linearity to linearity in the Ga content range of x<1at%, the coercive force jHc decreases at first to a minimum and then increaes slowly. The best value of the magnetic properties is obtained while the x=0.2.

  10. Dynamic and temperature dependent response of physical vapor deposited Se in freely standing nanometric thin films

    Science.gov (United States)

    Yoon, Heedong; McKenna, Gregory B.

    2016-05-01

    Here, we report results from an investigation of nano-scale size or confinement effects on the glass transition and viscoelastic properties of physical vapor deposited selenium films. The viscoelastic response of freely standing Se films was determined using a biaxial membrane inflation or bubble inflation method [P. A. O'Connell and G. B. McKenna, Science 307, 1760-1763 (2005)] on films having thicknesses from 60 to 267 nm and over temperatures ranging from Tg, macroscopic - 15 °C to Tg, macroscopic + 21 °C. Time-temperature superposition and time-thickness superposition were found to hold for the films in the segmental dispersion. The responses are compared with macroscopic creep and recoverable creep compliance data for selenium [K. M. Bernatz et al., J. Non-Cryst. Solids 307, 790-801 (2002)]. The time-temperature shift factors for the thin films show weaker temperature dependence than seen in the macroscopic behavior, being near to Arrhenius-like in their temperature dependence. Furthermore, the Se films exhibit a "rubbery-like" stiffening that increases as film thickness decreases similar to prior observations [P. A. O'Connell et al., Macromolecules 45(5), 2453-2459 (2012)] for organic polymers. In spite of the differences from the macroscopic behavior in the temperature dependence of the viscoelastic response, virtually no change in Tg as determined from the thickness dependence of the retardation time defining Tg was observed in the bubble inflation creep experiments to thicknesses as small as 60 nm. We also find that the observed rubbery stiffening is consistent with the postulate of K. L. Ngai et al. [J. Polym. Sci., Part B: Polym. Phys. 51(3), 214-224 (2013)] that it should correlate with the change of the macroscopic segmental relaxation.

  11. A new equilibrium form of zircon crystal

    Institute of Scientific and Technical Information of China (English)

    WANG; Xiang

    2001-01-01

    [1]Hartman, P., Perdok, G., On the relationship between structure and morphology of crystals, Acta Cryst., 1955, 8: 525-529.[2]Woensdregt, C. F., Computation of surface of energies in an electrostatic point charge model, Ⅱ. Application to zircon (ZrSiO4), Phys. Chem. Minerals, 1992, 19: 417-423.[3]Kern, R., The equilibrium form of a crystal, in Morphology of Crystal (ed. Sunnagawa, I.), Tokyo: Terra Scientific Publishing Company, 1970, 77-206.[4]Machenzie, J. K., Moore, J. W., Nickolas, J. F., Bond broken at atomically flat crystal surface, I. Face-centered and body-centered cubic crystal, J. Phys. Chem. Solids, 1962, 23: 185-196.[5]?. Machenzie, J. K., Nicholas, J. F., Bond broken at atomically flat crystal surface, ?. Crystals containing many atoms in a primitive unit cell, J. Phys. Chem. Solids, 1962, 23: 197-205.[6]Hazen, R. M., Finger, L. W., Crystal structure and compressibility of zircon at high pressure, Am. Mineral, 1979, 64:196-201.[7]Pupin, J. P., Zircon and granite petrology, Contrib. Mineral Petrol., 1980, 73: 207-220.[8]Wang, X., Kienast, J. R., Morphology and geochemistry of zircon: a case study on zircon from the microgranitoid enclaves,Science in China, Series D, 1999, 42(5): 544-552.[9]Wang, X., Li, W. X., Discovery of the { 211 }-type of zircon and its petrogenetic implication, Chinese Sci. Bull., 2001 (inpress).[10]Wang, X., Quantitative description of zircon morphology and its dynamics analysis, Science in China, Series D, 1998,41(4): 422-428.

  12. Heteropoly acids of the Keggin type with N-substituted

    Institute of Scientific and Technical Information of China (English)

    FU; Xiangkai

    2001-01-01

    [1]Hartman, P., Perdok, G., On the relationship between structure and morphology of crystals, Acta Cryst., 1955, 8: 525-529.[2]Woensdregt, C. F., Computation of surface of energies in an electrostatic point charge model, Ⅱ. Application to zircon (ZrSiO4), Phys. Chem. Minerals, 1992, 19: 417-423.[3]Kern, R., The equilibrium form of a crystal, in Morphology of Crystal (ed. Sunnagawa, I.), Tokyo: Terra Scientific Publishing Company, 1970, 77-206.[4]Machenzie, J. K., Moore, J. W., Nickolas, J. F., Bond broken at atomically flat crystal surface, I. Face-centered and body-centered cubic crystal, J. Phys. Chem. Solids, 1962, 23: 185-196.[5]?. Machenzie, J. K., Nicholas, J. F., Bond broken at atomically flat crystal surface, ?. Crystals containing many atoms in a primitive unit cell, J. Phys. Chem. Solids, 1962, 23: 197-205.[6]Hazen, R. M., Finger, L. W., Crystal structure and compressibility of zircon at high pressure, Am. Mineral, 1979, 64:196-201.[7]Pupin, J. P., Zircon and granite petrology, Contrib. Mineral Petrol., 1980, 73: 207-220.[8]Wang, X., Kienast, J. R., Morphology and geochemistry of zircon: a case study on zircon from the microgranitoid enclaves,Science in China, Series D, 1999, 42(5): 544-552.[9]Wang, X., Li, W. X., Discovery of the { 211 }-type of zircon and its petrogenetic implication, Chinese Sci. Bull., 2001 (inpress).[10]Wang, X., Quantitative description of zircon morphology and its dynamics analysis, Science in China, Series D, 1998,41(4): 422-428.

  13. Preparation of some new coumarin dyes

    Institute of Scientific and Technical Information of China (English)

    LUO; Xianjin

    2001-01-01

    [1]Hartman, P., Perdok, G., On the relationship between structure and morphology of crystals, Acta Cryst., 1955, 8: 525-529.[2]Woensdregt, C. F., Computation of surface of energies in an electrostatic point charge model, Ⅱ. Application to zircon (ZrSiO4), Phys. Chem. Minerals, 1992, 19: 417-423.[3]Kern, R., The equilibrium form of a crystal, in Morphology of Crystal (ed. Sunnagawa, I.), Tokyo: Terra Scientific Publishing Company, 1970, 77-206.[4]Machenzie, J. K., Moore, J. W., Nickolas, J. F., Bond broken at atomically flat crystal surface, I. Face-centered and body-centered cubic crystal, J. Phys. Chem. Solids, 1962, 23: 185-196.[5]?. Machenzie, J. K., Nicholas, J. F., Bond broken at atomically flat crystal surface, ?. Crystals containing many atoms in a primitive unit cell, J. Phys. Chem. Solids, 1962, 23: 197-205.[6]Hazen, R. M., Finger, L. W., Crystal structure and compressibility of zircon at high pressure, Am. Mineral, 1979, 64:196-201.[7]Pupin, J. P., Zircon and granite petrology, Contrib. Mineral Petrol., 1980, 73: 207-220.[8]Wang, X., Kienast, J. R., Morphology and geochemistry of zircon: a case study on zircon from the microgranitoid enclaves,Science in China, Series D, 1999, 42(5): 544-552.[9]Wang, X., Li, W. X., Discovery of the { 211 }-type of zircon and its petrogenetic implication, Chinese Sci. Bull., 2001 (inpress).[10]Wang, X., Quantitative description of zircon morphology and its dynamics analysis, Science in China, Series D, 1998,41(4): 422-428.

  14. 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.

  15. Crystal structure of an unknown solvate of (piperazine-κN){5,10,15,20-tetra­kis­[4-(benzo­yloxy)phen­yl]porphyrinato-κ4 N}zinc

    Science.gov (United States)

    Nasri, Soumaya; Ezzayani, Khaireddine; Turowska-Tyrk, Ilona; Roisnel, Thierry; Nasri, Habib

    2016-01-01

    The title compound, [Zn(C72H44N4O8)(C4H10N2)] or [Zn(TPBP)(pipz] (where TPBP and pipz are 5,10,15,20-tetra­kis­[4-(benzo­yloxy)phen­yl]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. PMID:27555935

  16. Crystal structure of an unknown solvate of (piperazine-κN){5,10,15,20-tetra-kis-[4-(benzo-yloxy)phen-yl]porphyrinato-κ(4) N}zinc.

    Science.gov (United States)

    Nasri, Soumaya; Ezzayani, Khaireddine; Turowska-Tyrk, Ilona; Roisnel, Thierry; Nasri, Habib

    2016-07-01

    The title compound, [Zn(C72H44N4O8)(C4H10N2)] or [Zn(TPBP)(pipz] (where TPBP and pipz are 5,10,15,20-tetra-kis-[4-(benzo-yloxy)phen-yl]porphyrinato and piperazine ligands respectively), features a distorted square-pyramidal coordin-ation geometry about the central Zn(II) atom. This central atom is chelated by the four N atoms of the porphyrinate anion and further coordinated by a nitro-gen 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 supra-molecular structure is made by parallel pairs of layers along (100), with an inter-layer 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 mol-ecules. The given chemical formula and other crystal data do not take into account these solvent mol-ecules.

  17. Crystal structure of tetra­kis­[μ2-2-(di­methyl­amino)­ethano­lato-κ3 N,O:O]di-μ3-hydroxido-di­thio­cyanato-κ2 N-dichromium(III)dilead(II) di­thio­cyanate aceto­nitrile monosolvate

    Science.gov (United States)

    Rusanova, Julia A.; Semenaka, Valentyna V.; Omelchenko, Irina V.

    2016-01-01

    The tetra­nuclear complex cation of the title compound, [Cr2Pb2(NCS)2(OH)2(C4H10NO)4](SCN)2·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-(di­methyl­amino)­ethano­late 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. PMID:27375871

  18. Large angle elastic and inelastic scattering of 14.93 keV photons

    Energy Technology Data Exchange (ETDEWEB)

    Singh, P.; Mehta, D.; Kumar, S.; Sharma, M.; Puri, S.; Shahi, J.S.; Singh, N. E-mail: nsingh@pu.ac.in

    2004-07-01

    Elastic and inelastic scattering cross-sections for the 14.93 keV photons (Y-K{alpha} X-rays) were measured at an angle of 141 deg. in the elements with 6 {<=} Z {<=} 92 and 1 {<=} Z {<=} 50, respectively. A reflection mode geometrical arrangement involving a Y-foil excited by the 59.54 keV {gamma}-rays from the {sup 241}Am radioisotope as photon source and an HPGe/Si(Li) detector was used. The measurements were performed under vacuum {approx}10{sup -2} Torr. Special care was taken in determination of the incident photon intensity and geometrical factors and to check effects due to occurrence of Bragg diffraction from the target lattice. The measured elastic scattering cross-sections have been compared with predictions from the form-factor formalism and relativistic second-order S-matrix calculations. The modified form-factor (MF) cross-sections are higher up to 50% than the measured ones in the case of elements with the electron binding energy (BE) in vicinity of the incident photon energy and are lower up to 20% for the other elements. These deviations are smoothed by incorporating the Anomalous Scattering Factors (ASFs) to the MF values [Acta Cryst. A 46 (1990) 170]. The S-matrix values exhibit general agreement with the measured cross-sections. The measured inelastic scattering cross-sections are found to be in good agreement with those calculated using the Klein-Nishina cross-section incorporating the Hartree-Fock incoherent scattering function (ISF)

  19. Steady needle growth with 3-D anisotropic surface tension

    Institute of Scientific and Technical Information of China (English)

    Xiao-jun CHEN; Yong-qiang CHEN; Jian-pu XU; Jian-jun XU

    2008-01-01

    The effect of the anisotropic interracial en-ergy on dendritic growth has been an important sub-ject, and has preoccupied many researchers in the field of materials science and condensed matter physics. The present paper is dedicated to the study of the effect of full 3-D anisotropic Surface tension on the steady state solution of dendritic growth. We obtain the analytical form of the first order approximation solution in the reg-ular asymptotic expansion around the Ivantsov's nee-dle growth solution, which extends the steady needle growth solution of the system with isotropic surface ten-sion obtained by Xu and Yu (J. J. Xu and D. S. Yu, J. Cryst. Growth, 1998, 187: 314; J. J. Xu, Interfa-cial Wave Theory of Pattern Formation: Selection of Dendrite Growth and Viscous Fingering in a Hele-Shaw Flow, Berlin: Springer-Verlag, 1997).The solution is expanded in the general Laguerre se-ries in any finite region around the needle-tip, and it is also expanded in a power series in the far field behind the tip. Both solutions are then numerically matched in the intermediate region. Based on this global valid solution, the dependence of Peclet number Pe and the interface's morphology on the anisotropy parameter of surface ten-sion as well as other physical parameters involved are determined. On the basis of this global valid solution, we explore the effect of the anisotropy parameter on the Peclet number of growth, as well as the morphology of the interface.

  20. An unexpected oxidation: NaK5Cl2(S2O6)2 revisited

    Science.gov (United States)

    Harrison, William T. A.; Plater, M. John

    2017-01-01

    The title compound, NaK5Cl2(S2O6)2 [systematic name: sodium penta­potassium dichloride bis­(di­thio­nate)], arose as an unexpected product from an organic synthesis that used di­thio­nite (S2O4 2−) 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. PMID:28217339

  1. Inhibition of lactoperoxidase by its own catalytic product: crystal structure of the hypothiocyanate-inhibited bovine lactoperoxidase at 2.3-A resolution.

    Science.gov (United States)

    Singh, A K; Singh, Nagendra; Sharma, Sujata; Shin, Kouichirou; Takase, Mitsunori; Kaur, Punit; Srinivasan, A; Singh, T P

    2009-01-01

    To the best of our knowledge, this is the first report on the structure of product-inhibited mammalian peroxidase. Lactoperoxidase is a heme containing an enzyme that catalyzes the inactivation of a wide range of microorganisms. In the presence of hydrogen peroxide, it preferentially converts thiocyanate ion into a toxic hypothiocyanate ion. Samples of bovine lactoperoxidase containing thiocyanate (SCN(-)) and hypothiocyanate (OSCN(-)) ions were purified and crystallized. The structure was determined at 2.3-A resolution and refined to R(cryst) and R(free) factors of 0.184 and 0.221, respectively. The determination of structure revealed the presence of an OSCN(-) ion at the distal heme cavity. The presence of OSCN(-) ions in crystal samples was also confirmed by chemical and spectroscopic analysis. The OSCN(-) ion interacts with the heme iron, Gln-105 N(epsilon1), His-109 N(epsilon2), and a water molecule W96. The sulfur atom of the OSCN(-) ion forms a hypervalent bond with a nitrogen atom of the pyrrole ring D of the heme moiety at an S-N distance of 2.8 A. The heme group is covalently bound to the protein through two ester linkages involving carboxylic groups of Glu-258 and Asp-108 and the modified methyl groups of pyrrole rings A and C, respectively. The heme moiety is significantly distorted from planarity, whereas pyrrole rings A, B, C, and D are essentially planar. The iron atom is displaced by approximately 0.2 A from the plane of the heme group toward the proximal site. The substrate channel resembles a long tunnel whose inner walls contain predominantly aromatic residues such as Phe-113, Phe-239, Phe-254, Phe-380, Phe-381, Phe-422, and Pro-424. A phosphorylated Ser-198 was evident at the surface, in the proximity of the calcium-binding channel.

  2. Crystal structures of two 2,3-di­ethyl­naphtho­[2,3-g]quinoxaline-6,11-dione derivatives

    Science.gov (United States)

    Forsyth, Craig M.

    2017-01-01

    Two new 5,12-disubstituted 2,3-di­ethyl­naphtho­[2,3-g]quinoxaline-6,11-dione compounds were readily synthesized from the commercial dye quinizarin. For 2,3-diethyl-5,12-di­hydroxy­naphtho­[2,3-g]quinoxaline-6,11-dione, (II), C20H16N2O4, the mol­ecule displays a near planar conformation and both hy­droxy groups participate in intra­molecular O—H⋯O(carbon­yl) hydrogen bonds. In the crystal, π–π ring inter­actions [minimum ring centroid separation = 3.5493 (9) Å] form stacks of co-planar mol­ecules down the c axis, while only minor inter­molecular C—H⋯O inter­actions are present. In contrast, in 2,3-diethyl-5,12-bis­(piperidin-1-yl)naphtho­[2,3-g]quinoxaline-6,11-dione, (IV), C30H34N4O2, which contains two independent, but similar, mol­ecules in the asymmetric unit, the polycyclic cores have a significant twist, with dihedral angles of 29.79 (6) and 29.31 (7)° between the terminal rings and only minor inter­molecular C—H⋯O hydrogen-bonding inter­actions are present. Electron density associated with additional solvent mol­ecules disordered about a fourfold axis was accounted for using the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18]. PMID:28932420

  3. Comparison of semi-insulating InAlAs and InP:Fe for InP-based buried-heterostructure QCLs

    Science.gov (United States)

    Flores, Y. V.; Aleksandrova, A.; Elagin, M.; Kischkat, J.; Kurlov, S. S.; Monastyrskyi, G.; Hellemann, J.; Golovynskyi, S. L.; Dacenko, O. I.; Kondratenko, S. V.; Tarasov, G. G.; Semtsiv, M. P.; Masselink, W. T.

    2015-09-01

    In a previous work [Flores et al., J. Cryst. Growth 398 (2014) 40] [3] we demonstrated the advantages of using a thin InAlAs spacer layer in the fabrication of buried-heterostructure quantum-cascade lasers (QCLs), as it improves the morphology of the interface between the laser core and the InP:Fe lateral cladding. In this paper we investigate aspects of InAlAs, which are relevant for its role as insulating lateral cladding of the laser sidewalls: carrier traps, electrical resistivity, and functionality as a sole lateral cladding. We find that a thin InAlAs spacer layer not only improves the regrowth interface morphology, but also eliminates interface-related shallow electronic states, thus improving the electrical resistivity of the interface. We further find that bulk InAlAs grown by gas-source molecular-beam epitaxy as well as InP:Fe are semi-insulating at room temperature, with specific resistivities of 3 ×107 Ω cm and 2 ×108 Ω cm, respectively. Both materials have also a high thermal activation energy for electrical conductivity (0.79 eV and 0.68 eV, respectively). In order to compare the performance of InP:Fe and InAlAs as a lateral cladding, lasers were fabricated from the same QCL wafer with differing stripe insulation materials. The resulting lasers differ mainly by the lateral insulation material: SiO2, InP:Fe (with InAlAs spacer), and pure InAlAs. All devices show a similar performance and similar temperature dependence, indicating insulating properties of InAlAs adequate for application in lateral regrowth of buried-heterostructure QCLs.

  4. Can X-ray constrained Hartree-Fock wavefunctions retrieve electron correlation?

    Science.gov (United States)

    Genoni, Alessandro; Dos Santos, Leonardo H R; Meyer, Benjamin; Macchi, Piero

    2017-03-01

    The X-ray constrained wavefunction (XC-WF) method proposed by Jayatilaka [Jayatilaka & Grimwood (2001) ▸, Acta Cryst. A57, 76-86] has attracted much attention because it represents a possible third way of theoretically studying the electronic structure of atoms and molecules, combining features of the more popular wavefunction- and DFT-based approaches. In its original formulation, the XC-WF technique extracts statistically plausible wavefunctions from experimental X-ray diffraction data of molecular crystals. A weight is used to constrain the pure Hartree-Fock solution to the observed X-ray structure factors. Despite the wavefunction being a single Slater determinant, it is generally assumed that its flexibility could guarantee the capture, better than any other experimental model, of electron correlation effects, absent in the Hartree-Fock Hamiltonian but present in the structure factors measured experimentally. However, although the approach has been known for long time, careful testing of this fundamental hypothesis is still missing. Since a formal demonstration is impossible, the validation can only be done heuristically and, to accomplish this task, X-ray constrained Hartree-Fock calculations have been performed using structure factor amplitudes computed at a very high correlation level (coupled cluster) for selected molecules in isolation, in order to avoid the perturbations due to intermolecular interactions. The results show that a single-determinant XC-WF is able to capture the electron correlation effects only partially. The largest amount of electron correlation is extracted when: (i) a large external weight is used (much larger than what has normally been used in XC-WF calculations using experimental data); and (ii) the high-order reflections, which carry less information on the electron correlation, are down-weighted (or even excluded), otherwise they would bias the fitting towards the unconstrained Hartree-Fock wavefunction.

  5. Can X-ray constrained Hartree–Fock wavefunctions retrieve electron correlation?

    Directory of Open Access Journals (Sweden)

    Alessandro Genoni

    2017-03-01

    Full Text Available The X-ray constrained wavefunction (XC-WF method proposed by Jayatilaka [Jayatilaka & Grimwood (2001, Acta Cryst. A57, 76–86] has attracted much attention because it represents a possible third way of theoretically studying the electronic structure of atoms and molecules, combining features of the more popular wavefunction- and DFT-based approaches. In its original formulation, the XC-WF technique extracts statistically plausible wavefunctions from experimental X-ray diffraction data of molecular crystals. A weight is used to constrain the pure Hartree–Fock solution to the observed X-ray structure factors. Despite the wavefunction being a single Slater determinant, it is generally assumed that its flexibility could guarantee the capture, better than any other experimental model, of electron correlation effects, absent in the Hartree–Fock Hamiltonian but present in the structure factors measured experimentally. However, although the approach has been known for long time, careful testing of this fundamental hypothesis is still missing. Since a formal demonstration is impossible, the validation can only be done heuristically and, to accomplish this task, X-ray constrained Hartree–Fock calculations have been performed using structure factor amplitudes computed at a very high correlation level (coupled cluster for selected molecules in isolation, in order to avoid the perturbations due to intermolecular interactions. The results show that a single-determinant XC-WF is able to capture the electron correlation effects only partially. The largest amount of electron correlation is extracted when: (i a large external weight is used (much larger than what has normally been used in XC-WF calculations using experimental data; and (ii the high-order reflections, which carry less information on the electron correlation, are down-weighted (or even excluded, otherwise they would bias the fitting towards the unconstrained Hartree–Fock wavefunction.

  6. Can X-ray constrained Hartree–Fock wavefunctions retrieve electron correlation?

    Science.gov (United States)

    Genoni, Alessandro; Dos Santos, Leonardo H. R.; Meyer, Benjamin; Macchi, Piero

    2017-01-01

    The X-ray constrained wavefunction (XC-WF) method proposed by Jayatilaka [Jayatilaka & Grimwood (2001) ▸, Acta Cryst. A57, 76–86] has attracted much attention because it represents a possible third way of theoretically studying the electronic structure of atoms and molecules, combining features of the more popular wavefunction- and DFT-based approaches. In its original formulation, the XC-WF technique extracts statistically plausible wavefunctions from experimental X-ray diffraction data of molecular crystals. A weight is used to constrain the pure Hartree–Fock solution to the observed X-ray structure factors. Despite the wavefunction being a single Slater determinant, it is generally assumed that its flexibility could guarantee the capture, better than any other experimental model, of electron correlation effects, absent in the Hartree–Fock Hamiltonian but present in the structure factors measured experimentally. However, although the approach has been known for long time, careful testing of this fundamental hypothesis is still missing. Since a formal demonstration is impossible, the validation can only be done heuristically and, to accomplish this task, X-ray constrained Hartree–Fock calculations have been performed using structure factor amplitudes computed at a very high correlation level (coupled cluster) for selected molecules in isolation, in order to avoid the perturbations due to intermolecular interactions. The results show that a single-determinant XC-WF is able to capture the electron correlation effects only partially. The largest amount of electron correlation is extracted when: (i) a large external weight is used (much larger than what has normally been used in XC-WF calculations using experimental data); and (ii) the high-order reflections, which carry less information on the electron correlation, are down-weighted (or even excluded), otherwise they would bias the fitting towards the unconstrained Hartree–Fock wavefunction. PMID:28250952

  7. Pallidol hexaacetate ethyl acetate monosolvate

    Directory of Open Access Journals (Sweden)

    Qinyong Mao

    2013-07-01

    Full Text Available The entire molecule of pallidol hexaacetate {systematic name: (±-(4bR,5R,9bR,10R-5,10-bis[4-(acetyloxyphenyl]-4b,5,9b,10-tetrahydroindeno[2,1-a]indene-1,3,6,8-tetrayl tetraacetate} is completed by the application of twofold rotational symmetry in the title ethyl acetate solvate, C40H34O12·C4H8O2. The ethyl acetate molecule was highly disordered and was treated with the SQUEEZE routine [Spek (2009. Acta Cryst. D65, 148–155]; the crystallographic data take into account the presence of the solvent. In pallidol hexaacetate, the dihedral angle between the fused five-membered rings (r.m.s. deviation = 0.100 Å is 54.73 (6°, indicating a significant fold in the molecule. Significant twists between residues are also evident as seen in the dihedral angle of 80.70 (5° between the five-membered ring and the pendent benzene ring to which it is attached. Similarly, the acetate residues are twisted with respect to the benzene ring to which they are attached [C—O(carboxy—C—C torsion angles = −70.24 (14, −114.43 (10 and −72.54 (13°]. In the crystal, a three-dimensional architecture is sustained by C—H...O interactions which encompass channels in which the disordered ethyl acetate molecules reside.

  8. 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).…

  9. An Evaluation of Stereoscopic Digital Mammography for Earlier Detection of Breast Cancer and Reduced Rate of Recall

    Science.gov (United States)

    2008-08-01

    LIQ   LOQ  7. BIRADS Category for patient: ________ Comments: Finding Code Confidence of True Finding (0 to 100...scale) Conspicuity (1=Barely visible to 10=Highly visible) Likelihood of Malignancy (0 to 100 scale) BIRADS Category for finding Indicate...Right Left  UOQ   UIQ   LIQ   LOQ  7. BIRADS Category for patient

  10. An experimental study on the effect of temperature and melt composition on the partitioning of nickel between olivine and silicate melt

    Energy Technology Data Exchange (ETDEWEB)

    Kinzler, R.J.; Grove, T.L.; Recca, S.I. (Massachusetts Institute of Technology, Cambridge (USA))

    1990-05-01

    Experiments in the simple system CaO-MgO-Al{sub 2}O{sub 3}-SiO{sub 2}Na{sub 2}O-FeO were carried out to investigate the control of temperature and melt composition on the partitioning of nickel between olivine and silicate melt (D{sup oliv/liq}{sub Ni}). Eleven experiments determine the influence of changing forsterite (Of) content on D{sup oliv/liq}{sub Ni} in this simple system. The equation of Hart and Davis (1978) that accounts for the variation of D{sup oliv/liq}{sub Ni} in terms of MgO content of the silicate liquid is tested using experimental data from iron-bearing simple and natural systems and found to be inadequate to explain the observed variation of D{sup oliv/liq}{sub Ni}. Two different equations are formulated to describe the partitioning behavior of Ni between olivine and silicate melt. The first is similar to that of Hart and Davis (1978) and uses an expression for Ni-Mg exchange between olivine and silicate melt. The second uses an expression for the Ni-olivine formation reaction. The Ni-Mg exchange equation for D{sup oliv/liq}{sub Ni} depends on the forsterite content of the olivine and the mole fraction MgO{sup liq}, and predicts the experimentally determined values within {plus minus}13% relative average error. The Ni-olivine formation reaction equation for D{sup oliv/liq}{sub Ni} depends on temperature, mole fraction SiO{sup liq}{sub 2}, and melt compositional terms that arise from a symmetric, binary, Margules formulation of the activity coefficients for NiO{sup liq} and SiO{sup liq}{sub 2}. This equation predicts the experimentally determined values within {plus minus}9% relative average error.

  11. Licorice root components in dietary supplements are selective estrogen receptor modulators with a spectrum of estrogenic and anti-estrogenic activities.

    Science.gov (United States)

    Boonmuen, Nittaya; Gong, Ping; Ali, Zulfiqar; Chittiboyina, Amar G; Khan, Ikhlas; Doerge, Daniel R; Helferich, William G; Carlson, Kathryn E; Martin, Teresa; Piyachaturawat, Pawinee; Katzenellenbogen, John A; Katzenellenbogen, Benita S

    2016-01-01

    Licorice root extracts are often consumed as botanical dietary supplements by menopausal women as a natural alternative to pharmaceutical hormone replacement therapy. In addition to their components liquiritigenin (Liq) and isoliquiritigenin (Iso-Liq), known to have estrogenic activity, licorice root extracts also contain a number of other flavonoids, isoflavonoids, and chalcones. We have investigated the estrogenic activity of 7 of these components, obtained from an extract of Glycyrrhiza glabra powder, namely Glabridin (L1), Calycosin (L2), Methoxychalcone (L3), Vestitol (L4), Glyasperin C (L5), Glycycoumarin (L6), and Glicoricone (L7), and compared them with Liq, Iso-Liq, and estradiol (E2). All components, including Liq and Iso-Liq, have low binding affinity for estrogen receptors (ERs). Their potency and efficacy in stimulating the expression of estrogen-regulated genes reveal that Liq and Iso-Liq and L2, L3, L4, and L6 are estrogen agonists. Interestingly, L3 and L4 have an efficacy nearly equivalent to E2 but with a potency ca. 10,000-fold less. The other components, L1, L5 and L7, acted as partial estrogen antagonists. All agonist activities were reversed by the antiestrogen, ICI 182,780, or by knockdown of ERα with siRNA, indicating that they are ER dependent. In HepG2 hepatoma cells stably expressing ERα, only Liq, Iso-Liq, and L3 stimulated estrogen-regulated gene expression, and in all cases gene stimulation did not occur in HepG2 cells lacking ERα. Collectively, these findings classify the components of licorice root extracts as low potency, mixed ER agonists and antagonists, having a character akin to that of selective estrogen receptor modulators or SERMs.

  12. 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

  13. Structure of lobster apocrustacyanin A1 using softer X-rays.

    Science.gov (United States)

    Cianci, M; Rizkallah, P J; Olczak, A; Raftery, J; Chayen, N E; Zagalsky, P F; Helliwell, J R

    2001-09-01

    The molecular basis of the camouflage colouration of marine crustacea is often provided by carotenoproteins. The blue colour of the lobster carapace, for example, is intricately associated with a multimacromolecular 16-mer complex of protein subunits each with a bound astaxanthin molecule. The protein subunits of crustacyanin fall into two distinct subfamilies, CRTC and CRTA. Here, the crystal structure solution of the A(1) protein of the CRTC subfamily is reported. The problematic nature of the structure solution of the CRTC proteins (both C(1) and A(1)) warranted consideration and the development of new approaches. Three putative disulfides per protein subunit were likely to exist based on molecular-homology modelling against known lipocalin protein structures. With two such subunits per crystallographic asymmetric unit, this direct approach was still difficult as it involved detecting a weak signal from these sulfurs and suggested the use of softer X-rays, combined with high data multiplicity, as reported previously [Chayen et al. (2000), Acta Cryst. D56, 1064-1066]. This paper now describes the structure solution of CRTC in the form of the A(1) dimer based on use of softer X-rays (2 A wavelength). The structure solution involved a xenon derivative with an optimized xenon L(I) edge f" signal and a native data set. The hand of the xenon SIROAS phases was determined by using the sulfur anomalous signal from a high-multiplicity native data set also recorded at 2 A wavelength. For refinement, a high-resolution data set was measured at short wavelength. All four data sets were collected at 100 K. The refined structure to 1.4 A resolution based on 60 276 reflections has an R factor of 17.7% and an R(free) of 22.9% (3137 reflections). The structure is that of a typical lipocalin, being closely related to insecticyanin, to bilin-binding protein and to retinol-binding protein. This A(1) monomer or dimer can now be used as a search motif in the structural studies of the

  14. Ginzburg-Landau theory of the bcc-liquid interface kinetic coefficient

    Science.gov (United States)

    Wu, Kuo-An; Wang, Ching-Hao; Hoyt, Jeffrey J.; Karma, Alain

    2015-01-01

    We extend the Ginzburg-Landau (GL) theory of atomically rough bcc-liquid interfaces [Wu et al., Phys. Rev. B 73, 094101 (2006), 10.1103/PhysRevB.73.094101] outside of equilibrium. We use this extension to derive an analytical expression for the kinetic coefficient, which is the proportionality constant μ (n ̂) between the interface velocity along a direction n ̂ normal to the interface and the interface undercooling. The kinetic coefficient is expressed as a spatial integral along the normal direction of a sum of gradient square terms corresponding to different nonlinear density wave profiles. Anisotropy arises naturally from the dependence of those profiles on the angles between the principal reciprocal lattice vectors K⃗i and n ̂. Values of the kinetic coefficient for the (100 ) ,(110 ) , and (111 ) interfaces are compared quantitatively to the prediction of linear Mikheev-Chernov (MC) theory [J. Cryst. Growth 112, 591 (1991), 10.1016/0022-0248(91)90340-B] and previous molecular dynamics (MD) simulation studies of crystallization kinetics for a classical model of Fe. Additional MD simulations are carried out here to compute the relaxation time of density waves in the liquid in order to make this comparison free of fit parameters. The GL theory predicts an expression for μ similar to the MC theory but yields a better agreement with MD simulations for both its magnitude and anisotropy due to a fully nonlinear description of density wave profiles across the solid-liquid interface. In particular, the overall magnitude of μ predicted by GL theory is an order of magnitude larger than predicted by the MC theory. GL theory is also used to derive an inverse relation between μ and the solid-liquid interfacial free energy. The general methodology used here to derive an expression for μ (n ̂) also applies to amplitude equations derived from the phase-field-crystal model, which only differ from GL theory by the choice of cubic and higher order nonlinearities in the

  15. Scattering studies on cryoglobulins stability and aggregation properties

    Energy Technology Data Exchange (ETDEWEB)

    Bicev, R.N.; Oliveira, E.A.; Oliveira, C.L.P.; Brandao, H. [Universidade de Sao Paulo (USP), SP (Brazil); Andrade, L.E.C. [Universidade Federal de Sao Paulo (UNIFESP), SP (Brazil)

    2012-07-01

    configurations for the protein in solution in each temperature. [1]Dammacco F. et al. Eur J Clin Invest 2001; 31:628-38. [2]Semenyuk V and Svergun DI. J. Appl. Cryst., 1991, 24, 537-540; [3]Schmidt, Manfred; Burchard, Walter. Macromolecules, 1981, 14, 210-211 [4]Bernardo, Pau et al. Jacs, 2007, 129, 17, 5656-5664. (author)

  16. Determinants of cyanuric acid and melamine assembly in water.

    Science.gov (United States)

    Ma, Mingming; Bong, Dennis

    2011-07-19

    While the recognition of cyanuric acid (CA) by melamine (M) and their derivatives has been known to occur in both water and organic solvents for some time, analysis of CA/M assembly in water has not been reported (Ranganathan, A.; Pedireddi, V. R.; Rao, C. N. R. J. Am. Chem. Soc.1999, 121, 1752-1753; Mathias, J. P.; Simanek, E. E.; Seto, C. T.; Whitesides, G. M. Macromol. Symp.1994, 77, 157-166; Zerkowski, J. A.; MacDonald, J. C.; Seto, C. T.; Wierda, D. A.; Whitesides, G. M. J. Am. Chem. Soc.1994, 116, 2382-2391; Mathias, J. P.; Seto, C. T.; Whitesides, G. M. Polym. Prepr.1993, 34, 92-93; Seto, C. T.; Whitesides, G. M. J. Am. Chem. Soc.1993, 115, 905-916; Zerkowski, J. A.; Seto, C. T.; Whitesides, G. M. J. Am. Chem. Soc.1992, 114, 5473-5475; Seto, C. T.; Whitesides, G. M. J. Am. Chem. Soc.1990, 112, 6409-6411; Wang, Y.; Wei, B.; Wang, Q. J. Chem. Cryst.1990, 20, 79-84; ten Cate, M. G. J.; Huskens, J.; Crego-Calama, M.; Reinhoudt, D. N. Chem.-Eur. J.2004, 10, 3632-3639). We have examined assembly of CA/M, as well as assembly of soluble trivalent CA and M derivatives (TCA/TM), in aqueous solvent, using a combination of solution phase NMR, isothermal titration and differential scanning calorimetry (ITC/DSC), cryo-transmission electron microscopy (cryo-TEM), and synthetic chemistry. While the parent heterocycles coprecipitate in water, the trivalent system displays more controlled and cooperative assembly that occurs at lower concentrations than the parent and yields a stable nanoparticle suspension. The assembly of both parent and trivalent systems is rigorously 1:1 and proceeds as an exothermic, proton-transfer coupled process in neutral pH water. Though CA and M are considered canonical hydrogen-bonding motifs in organic solvents, we find that their assembly in water is driven in large part by enthalpically favorable surface-area burial, similar to what is observed with nucleic acid recognition. There are currently few synthetic systems capable of robust molecular

  17. The mechanical and strength properties of diamond.

    Science.gov (United States)

    Field, J E

    2012-12-01

    Diamond is an exciting material with many outstanding properties; see, for example Field J E (ed) 1979 The Properties of Diamond (London: Academic) and Field J E (ed) 1992 The Properties of Natural and Synthetic Diamond (London: Academic). It is pre-eminent as a gemstone, an industrial tool and as a material for solid state research. Since natural diamonds grew deep below the Earth's surface before their ejection to mineable levels, they also contain valuable information for geologists. The key to many of diamond's properties is the rigidity of its structure which explains, for example, its exceptional hardness and its high thermal conductivity. Since 1953, it has been possible to grow synthetic diamond. Before then, it was effectively only possible to have natural diamond, with a small number of these found in the vicinity of meteorite impacts. Techniques are now available to grow gem quality synthetic diamonds greater than 1 carat (0.2 g) using high temperatures and pressures (HTHP) similar to those found in nature. However, the costs are high, and the largest commercially available industrial diamonds are about 0.01 carat in weight or about 1 mm in linear dimension. The bulk of synthetic diamonds used industrially are 600 µm or less. Over 75% of diamond used for industrial purposes today is synthetic material. In recent years, there have been two significant developments. The first is the production of composites based on diamond; these materials have a significantly greater toughness than diamond while still maintaining very high hardness and reasonable thermal conductivity. The second is the production at low pressures by metastable growth using chemical vapour deposition techniques. Deposition onto non-diamond substrates was first demonstrated by Spitsyn et al 1981 J. Cryst. Growth 52 219-26 and confirmed by Matsumoto et al 1982 Japan J. Appl. Phys. 21 L183-5. These developments have added further to the versatility of diamond. Two other groups of

  18. Trinuclear nickel coordination complexes of phenanthrene-9,10-dione dioxime

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    Owen M. Williams

    2016-04-01

    fluoridoboronate structure, the solvent (DCM was too badly disordered to be modelled, so its contribution was removed using SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18].

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

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    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

  20. 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

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    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.

  1. 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

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    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.

  2. Crystal structures of tris[1-oxopyridine-2-olato(1−]silicon(IV chloride chloroform-d1 disolvate, tris[1-oxopyridine-2-olato(1−]silicon(IV chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−]silicon(IV chloride chloroform-d1 disolvate

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    Bradley M. Kraft

    2015-12-01

    Full Text Available The cations in the title salts, [Si(OPO3]Cl·2CDCl3, (I, [Si(OPO3]Cl·xCH3CN, (II, and fac-[Si(OPTO3]Cl·2CDCl3, (III (OPO = 1-oxo-2-pyridinone, C5H4NO2, and OPTO = 1-oxo-2-pyridinethione, C5H4NOS, have distorted octahedral coordination spheres. The first two structures contain the same cation and anion, but different solvents of crystallization led to different solvates and packing arrangements. In structures (I and (III, the silicon complex cations and chloride anions are well separated, while in (II, there are two C—H...Cl distances that fall just within the sum of the van der Waals radii of the C and Cl atoms. The pyridine portions of the OPO ligands in (I and (II are modeled as disordered with the planar flips of themselves [(I: 0.574 (15:0.426 (15, 0.696 (15:0.304 (15, and 0.621 (15:0.379 (15; (II: 0.555 (13:0.445 (13, 0.604 (14:0.396 (14 and 0.611 (13:0.389 (13], demonstrating that both fac and mer isomers are co-crystallized. In (II, highly disordered solvent, located in two independent channels along [100], was unable to be modeled. Reflection contributions from this solvent were fixed and added to the calculated structure factors using the SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] function of program PLATON, which determined there to be 54 electrons in 225 Å3 accounted for per unit cell (25 electrons in 109 Å3 in one channel, and 29 electrons in 115 Å3 in the other. In (I and (II, all species lie on general positions. In (III, all species are located along crystallographic threefold axes.

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

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    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.

  4. Chelate Ring Size Effect as a Factor of Selective Fluorescent Recognition of Zn(2+) Ions by Pyrrolo[2,3-b]quinoxaline with a Substituted 2-Pyridyl Group Receptor.

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    Ostrowska, Katarzyna; Musielak, Bogdan; Szneler, Edward; Dudek, Łukasz; Gryl, Marlena; Stadnicka, Katarzyna

    2015-09-01

    Analysis of the spectral properties and structural differences of two turn-on ratiometric fluorescent receptors for Zn(2+) and Cd(2+) ions, derivatives of pyrrolo[2,3-b]quinoxaline (2), and earlier published 3 (Ostrowska et al. CrystEngComm 2015, 17, 498-502) was performed. Both ligands are E/Z push-pull olefins interconverting at room temperature, with barriers to rotation about enamine double bonds, from E to Z isomers of 19.3 ± 0.1 and 16.9 ± 0.3 kcal/mol and from Z to E of 16.9 ± 0.3 and 15.7 ± 0.2 kcal/mol, respectively. Diastereoisomers (E)-2 and (Z)-2 were isolated and characterized by X-ray structural analysis. The formation of complexes by (E/Z)-2 with acetates and acetylacetonates of Zn(2+) and Cd(2+) was monitored by UV-vis, fluorescence, and (1)H NMR titrations in acetonitrile, respectively. X-ray structural analysis for isolated [(E)-2]2Zn in relation to earlier published (E)-3-ZnOAc revealed the formation of a six-coordinated zinc ion with six- and four-membered bis-chelate rings by (E)-2. The chelate effect increases the ligand affinity for Zn(2+) (log β12 = 12.45) and causes the elongation of nitrogen-metal bonds. Extension of the coordination cavity size allows coordination of a cadmium ion. The introduction of a flexible ethylene linker between the fluorophore and ionophore pyridyl groups in 3 significantly affects the selectivity of zinc-ion recognition. The distorted tetrahedral geometry of (E)-3-ZnOAc with a four-coordinated zinc ion appears to be the most preferred because of the short donor-zinc distance with a 1:1 binding mode. The formation of the small coordination cavity size with six-membered bis-chelate rings provides an effective overlap of zinc and donor orbitals, precluding the coordination of a cadmium ion in the same manner as zinc.

  5. Polarised neutron scattering from dynamic polarised targets in biology

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    Knop, W.; Hirai, M.; Olah, G.; Meerwinck, W.; Schink, H.-J.; Stuhrman, H. B.; Wagner, R.; Wenkow-EsSouni, M.; Zhao, J.; Schärpf, O.; Crichton, R. R.; Krumpolc, M.; Nierhaus, K. H.; Niinikoski, T. O.; Rijllart, A.

    1991-10-01

    The contrast giving rise to neutron small-angle scattering can be enhanced considerably by polarisation of the hydrogen nuclei [J. des Coizeaux and G. Jannink, Les Polymères en Solution, Les Editions de Physique, F-91944 Les Ulis, France (1987)]. Using polarised neutrons the scattering from protonated labels in a deuterated matrix will increase by an order of magnitude. This is the basis of nuclear spin contrast variation, a method which is of particular interest for the in situ structure determination of macromolecular components. A new polarised target for neutron scattering has been designed by CERN and tested successfully at FRG-1 of the GKSS research centre. For the purpose of thermal-neutron scattering the frozen solutions of biomolecules are immersed in liquid helium 4, which is thermally coupled to the cooling mixture of helium 3/helium 4 of the dilution refrigerator. The nuclear spins are aligned with respect to the external magnetic field-parallel or antiparallel-by dynamic nuclear polarisation (DNP). The gain in neutron scattering compared to earlier experiments using direct cooling of the sample by helium 3 is a factor of 30. Another factor of 30 arises from the installation of the cold source and the beryllium reflector in FRG-1 [W. Knop et al., J. Appl. Cryst. 22 (1989) 352]. Pure nuclear spin targets are produced from dynamic polarised targets by selective depolarisation. In biological material only the hydrogen isotopes contribute significantly to polarised neutron scattering. Thus, saturation of the proton NMR yields a deuteron target, provided the target material has been enriched by the latter isotope. A proton target is obtained from the dynamic polarised target by saturation of deuteron NMR. This leads to six additional scattering functions reflecting the proton and deuteron spin densities and the correlations between the polarised isotopes. Polarised neutron scattering from nuclear spin targets of apoferritin and various derivatives of the

  6. Crystal structures of tris-[1-oxo-pyridine-2-olato(1-)]silicon(IV) chloride chloro-form-d 1 disolvate, tris-[1-oxo-pyridine-2-olato(1-)]silicon(IV) chloride aceto-nitrile unqu-anti-fied solvate, and fac-tris-[1-oxo-pyridine-2-thiol-ato(1-)]silicon(IV) chloride chloro-form-d 1 disolvate.

    Science.gov (United States)

    Kraft, Bradley M; Brennessel, William W; Ryan, Amy E; Benjamin, Candace K

    2015-12-01

    The cations in the title salts, [Si(OPO)3]Cl·2CDCl3, (I), [Si(OPO)3]Cl·xCH3CN, (II), and fac-[Si(OPTO)3]Cl·2CDCl3, (III) (OPO = 1-oxo-2-pyridin-one, C5H4NO2, and OPTO = 1-oxo-2-pyridine-thione, C5H4NOS), have distorted octa-hedral coordination spheres. The first two structures contain the same cation and anion, but different solvents of crystallization led to different solvates and packing arrangements. In structures (I) and (III), the silicon complex cations and chloride anions are well separated, while in (II), there are two C-H⋯Cl distances that fall just within the sum of the van der Waals radii of the C and Cl atoms. The pyridine portions of the OPO ligands in (I) and (II) are modeled as disordered with the planar flips of themselves [(I): 0.574 (15):0.426 (15), 0.696 (15):0.304 (15), and 0.621 (15):0.379 (15); (II): 0.555 (13):0.445 (13), 0.604 (14):0.396 (14) and 0.611 (13):0.389 (13)], demonstrating that both fac and mer isomers are co-crystallized. In (II), highly disordered solvent, located in two independent channels along [100], was unable to be modeled. Reflection contributions from this solvent were fixed and added to the calculated structure factors using the SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9-18] function of program PLATON, which determined there to be 54 electrons in 225 Å(3) accounted for per unit cell (25 electrons in 109 Å(3) in one channel, and 29 electrons in 115 Å(3) in the other). In (I) and (II), all species lie on general positions. In (III), all species are located along crystallographic threefold axes.

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

    Science.gov (United States)

    Chetioui, Souheyla; Rouag, Djamil-Azzeddine; Djukic, Jean-Pierre; Bochet, Christian G.; Touzani, Rachid; Bailly, Corinne; Crochet, Aurélien; Fromm, Katharina M.

    2016-01-01

    In the copper(II) complex, bis­{(E)-1-[(2,4,6-tri­bromo­phen­yl)diazen­yl]naph­thalen-2-olato}copper(II), [Cu(C16H8Br3N2O)2], (I), the metal cation is coord­inated by two N atoms and two O atoms from two bidentate (E)-1-[(2,4,6-tri­bromo­phen­yl)diazen­yl]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-tri­bromo­phen­yl)diazen­yl]naphthalen-2-olato}nickel(II), [Ni(C16H8Br3N2O)2], (II), and bis­{(E)-1-[(2,4,6-tri­bromo­phen­yl)diazen­yl]naphthalen-2-olato}palladium(II), [Pd(C16H8Br3N2O)2], (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. PMID:27536389

  8. Crystal structures of a copper(II) and the isotypic nickel(II) and palladium(II) complexes of the ligand (E)-1-[(2,4,6-tri-bromo-phen-yl)diazen-yl]naphthalen-2-ol.

    Science.gov (United States)

    Chetioui, Souheyla; Rouag, Djamil-Azzeddine; Djukic, Jean-Pierre; Bochet, Christian G; Touzani, Rachid; Bailly, Corinne; Crochet, Aurélien; Fromm, Katharina M

    2016-08-01

    In the copper(II) complex, bis-{(E)-1-[(2,4,6-tri-bromo-phen-yl)diazen-yl]naph-thalen-2-olato}copper(II), [Cu(C16H8Br3N2O)2], (I), the metal cation is coord-inated by two N atoms and two O atoms from two bidentate (E)-1-[(2,4,6-tri-bromo-phen-yl)diazen-yl]naphthalen-2-olate ligands, forming a slightly distorted square-planar environment. In one of the ligands, the tri-bromo-benzene ring is inclined to the naphthalene ring system by 37.4 (5)°, creating a weak intra-molecular Cu⋯Br inter-action [3.134 (2) Å], while in the other ligand, the tri-bromo-benzene 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-tri-bromo-phen-yl)diazen-yl]naphthalen-2-olato}nickel(II), [Ni(C16H8Br3N2O)2], (II), and bis-{(E)-1-[(2,4,6-tri-bromo-phen-yl)diazen-yl]naphthalen-2-olato}palladium(II), [Pd(C16H8Br3N2O)2], (III), respectively, the metal atoms are located on centres of inversion, hence the metal coordination spheres have perfect square-planar geometries. The tri-bromo-benzene 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), mol-ecules are linked by C-H⋯Br hydrogen bonds, forming chains along [010]. The chains are linked by C-H⋯π inter-actions, forming sheets parallel to (011). In the crystals of (II) and (III), mol-ecules are linked by C-H⋯π inter-actions, 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 mol-ecules were not taken into account during refinement.

  9. Crystal structures of N(2),N(3),N(5),N(6)-tetra-kis-(pyridin-2-ylmeth-yl)pyrazine-2,3,5,6-tetra-carboxamide and N(2),N(3),N(5),N(6)-tetra-kis-(pyridin-4-ylmeth-yl)pyrazine-2,3,5,6-tetra-carboxamide.

    Science.gov (United States)

    Cati, Dilovan S; Stoeckli-Evans, Helen

    2017-02-01

    The title compounds, C32H28N10O4· unknown solvent, (I), and C32H28N10O4, (II), are pyrazine-2,3,5,6-tetra-carboxamide derivatives. In (I), the substituents are (pyridin-2-ylmeth-yl)carboxamide, while in (II), the substituents are (pyridin-4-ylmeth-yl)carboxamide. Both compounds crystallize in the monoclinic space group P21/n, with Z' = 1 for (I), and Z' = 0.5 for (II). The whole mol-ecule 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 intra-molecular 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 intra-molecular C-H⋯O hydrogen bonds present in (II). In the crystal of (I), mol-ecules 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), mol-ecules 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).

  10. Crystal structure of an unknown solvate of dodecakis(μ2-alaninato-1:2κ2O:N,Ocerium(IIIhexanickel(II aquatris(hydroxido-κOtris(nitrato-κ2O,O′cerate(III

    Directory of Open Access Journals (Sweden)

    Stanislav I. Bezzubov

    2015-10-01

    Full Text Available The chiral title compound, [CeNi6(C3H6NO212][Ce(NO33(OH3(H2O], comprises a complex heterometallic Ni/Ce cation and a homonuclear Ce anion. Both the cation and anion exhibit point group symmetry 3. with the CeIII atom situated on the threefold rotation axis. The cation metal core consists of six NiII atoms coordinated in a slightly distorted octahedral N2O4 configuration by N and O atoms of 12 deprotonated l-alaninate ligands exhibiting both bridging and chelating modes. This metal–organic coordination motif encapsulates one CeIII atom that shows an icosahedral coordination by the O-donor atoms of the l-alaninate ligands, with Ce—O distances varying in the range 2.455 (5–2.675 (3 Å. In the anion, the central CeIII ion is bound to three bidentate nitrate ligands, to three hydroxide ligands and to one water molecule, with Ce—O distances in the range 2.6808 (19–2.741 (2 Å. The H atoms of the coordinating water molecule are disordered over three positions due to its location on a threefold rotation axis. Disorder is also observed in fragments of two l-alaninate ligands, with occupancy ratios of 0.608 (14:0.392 (14 and 0.669 (8:0.331 (8, respectively, for the two sets of sites. In the crystal, the complex cations and anions assemble through O—H...O and N—H...O hydrogen bonds into a three-dimensional network with large voids of approximately 1020 Å3. The contributions of highly disordered ethanol and water solvent molecules to the diffraction data were removed with the SQUEEZE procedure [Spek (2015. Acta Cryst. C71, 9–18]. The given chemical formula and other crystal data do not take into account the unknown amount of these solvent molecules.

  11. Crystal structure of lactoperoxidase at 2.4 A resolution.

    Science.gov (United States)

    Singh, Amit Kumar; Singh, Nagendra; Sharma, Sujata; Singh, S Baskar; Kaur, Punit; Bhushan, A; Srinivasan, A; Singh, Tej P

    2008-02-29

    Lactoperoxidase (LPO) is a member of the mammalian peroxidase superfamily. It catalyzes the oxidation of thiocyanate and halides. Freshly isolated and purified samples of caprine LPO were saturated with ammonium iodide and crystallized using 20% polyethylene glycol 3350 in a hanging drop vapor diffusion setup. The structure has been determined using X-ray crystallographic method and refined to R(cryst) and R(free) factors of 0.196 and 0.203, respectively. The structure determination revealed an unexpected phosphorylation of Ser198 in LPO, which is also confirmed by anti-phosphoserine antibody binding studies. The structure is also notable for observing densities for glycan chains at all the four potential glycosylation sites. Caprine LPO consists of a single polypeptide chain of 595 amino acid residues and folds into an oval-shaped structure. The structure contains 20 well-defined alpha-helices of varying lengths including a helix, H(2a), unique to LPO, and two short antiparallel beta-strands. The structure confirms that the heme group is covalently linked to the protein through two ester linkages involving carboxylic groups of Glu258 and Asp108 and modified methyl groups of pyrrole rings A and C, respectively. The heme moiety is slightly distorted from planarity, but pyrrole ring B is distorted considerably. However, an iron atom is displaced only by 0.1 A from the plane of the heme group toward the proximal site. The substrate diffusing channel in LPO is cylindrical in shape with a diameter of approximately 6 A. Two histidine residues and six buried water molecules are connected through a hydrogen-bonded chain from the distal heme cavity to the surface of protein molecule and seemingly form the basis of proton relay for catalytic action. Ten iodide ions have been observed in the structure. Out of these, only one iodide ion is located in the distal heme cavity and is hydrogen bonded to the water molecule W1. W1 is also hydrogen bonded to the heme iron as well as

  12. PLATON SQUEEZE: a tool for the calculation of the disordered solvent contribution to the calculated structure factors.

    Science.gov (United States)

    Spek, Anthony L

    2015-01-01

    The completion of a crystal structure determination is often hampered by the presence of embedded solvent molecules or ions that are seriously disordered. Their contribution to the calculated structure factors in the least-squares refinement of a crystal structure has to be included in some way. Traditionally, an atomistic solvent disorder model is attempted. Such an approach is generally to be preferred, but it does not always lead to a satisfactory result and may even be impossible in cases where channels in the structure are filled with continuous electron density. This paper documents the SQUEEZE method as an alternative means of addressing the solvent disorder issue. It conveniently interfaces with the 2014 version of the least-squares refinement program SHELXL [Sheldrick (2015). Acta Cryst. C71. In the press] and other refinement programs that accept externally provided fixed contributions to the calculated structure factors. The PLATON SQUEEZE tool calculates the solvent contribution to the structure factors by back-Fourier transformation of the electron density found in the solvent-accessible region of a phase-optimized difference electron-density map. The actual least-squares structure refinement is delegated to, for example, SHELXL. The current versions of PLATON SQUEEZE and SHELXL now address several of the unnecessary complications with the earlier implementation of the SQUEEZE procedure that were a necessity because least-squares refinement with the now superseded SHELXL97 program did not allow for the input of fixed externally provided contributions to the structure-factor calculation. It is no longer necessary to subtract the solvent contribution temporarily from the observed intensities to be able to use SHELXL for the least-squares refinement, since that program now accepts the solvent contribution from an external file (.fab file) if the ABIN instruction is used. In addition, many twinned structures containing disordered solvents are now also

  13. Polymorphism of NaVO2F2: a P2₁/c superstructure with pseudosymmetry of P2₁/m in the subcell.

    Science.gov (United States)

    Yu, Zi-Qun; Wang, Jing-Quan; Huang, Ya-Xi; Botis, Sanda M; Pan, Yuanming; Mi, Jin-Xiao

    2015-06-01

    The ADDSYM routine in the program PLATON [Spek (2015). Acta Cryst. C71, 9-18] has helped researchers to avoid structures of (metal-)organic compounds being reported in an unnecessarily low symmetry space group. However, determination of the correct space group may get more complicated in cases of pseudosymmetric inorganic compounds. One example is NaVO2F2, which was reported [Crosnier-Lopez et al. (1994). Eur. J. Solid State Inorg. Chem. 31, 957-965] in the acentric space group P2₁ based on properties but flagged by ADDSYM as (pseudo)centrosymmetric P2₁/m within default distance tolerances. Herein a systematic investigation reveals that NaVO2F2 exists in at least four polymorphs: P2₁, (I), P2₁/m, (II), P2₁/c, (III), and one or more low-temperature ones. The new centrosymmetric modification, (III), with the space group P2₁/c has a similar atomic packing geometry to phase (I), except for having a doubled c axis. The double-cell of phase (III) arises from atomic shifts from the glide plane c at (x, ¼, z). With increasing temperature, the number of observed reflections decreases. The odd l reflections gradually become weaker and, correspondingly, all atoms shift towards the glide plane, resulting in a gradual second-order transformation of (III) into high-temperature phase (II) (P2₁/m) at below 493 K. At least one first-order enantiotropic phase transition was observed below 139 K from both the single-crystal X-ray diffraction and the differential scanning calorimetry analyses. Periodic first-principles calculations within density functional theory show that both P2₁/c superstructure (III) and P2₁ substructure (I) are more stable than P2₁/m structure (II), and that P2₁/c superstructure (III) is more stable that P2₁ substructure (I).

  14. Crystal structures of N 2,N 3,N 5,N 6-tetra­kis­(pyridin-2-ylmeth­yl)pyrazine-2,3,5,6-tetra­carboxamide and N 2,N 3,N 5,N 6-tetra­kis­(pyridin-4-ylmeth­yl)pyrazine-2,3,5,6-tetra­carboxamide

    Science.gov (United States)

    Cati, Dilovan S.; Stoeckli-Evans, Helen

    2017-01-01

    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-ylmeth­yl)carboxamide, while in (II), the substituents are (pyridin-4-ylmeth­yl)carboxamide. 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). PMID:28217363

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

    Science.gov (United States)

    Luong Thi Thu, Thuy; Nguyen Bich, Ngan; Nguyen, Hien

    2017-01-01

    Facile synthetic routes for three 4-substituted 2,2′-bi­pyridine derivatives, 4-[2-(4-methyl­phenyl)­ethyn­yl]-2,2′-bi­pyridine, C19H14N2, (I), 4-[2-(pyridin-3-yl)ethyn­yl]-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. PMID:28435732

  16. Three new [XC(O)NH]P(O)[N(CH2C6H5)2]2 phosphoric triamides (X = CClF2, 3-F-C6H4 and 3,5-F2-C6H3): a database analysis of tertiary N-atom geometry in compounds with a C(O)NHP(O)[N]2 core.

    Science.gov (United States)

    Pourayoubi, Mehrdad; Jasinski, Jerry P; Shoghpour Bayraq, Samad; Eshghi, Hossein; Keeley, Amanda C; Bruno, Giuseppe; Amiri Rudbari, Hadi

    2012-10-01

    In the phosphoric triamides N,N,N',N'-tetrabenzyl-N''-(2-chloro-2,2-difluoroacetyl)phosphoric triamide, C(30)H(29)ClF(2)N(3)O(2)P, (I), N,N,N',N'-tetrabenzyl-N''-(3-fluorobenzoyl)phosphoric triamide, C(35)H(33)FN(3)O(2)P, (II), and N,N,N',N'-tetrabenzyl-N''-(3,5-difluorobenzoyl)phosphoric triamide, C(35)H(32)F(2)N(3)O(2)P, (III), the tertiary N atoms of the dibenzylamido groups have sp(2) character with minimal deviation from planarity. The sums of the three bond angles about the N atoms in (I)-(III) deviate by less than 8° from the planar value of 360°. The geometries of the tertiary N atoms in all phosphoric triamides with C(O)NHP(O)[N](2) skeletons deposited in the Cambridge Structural Database [CSD; Allen (2002). Acta Cryst. B58, 380-388] have been examined and the bond-angle sums at the two tertiary N atoms (SUM1 and SUM2) and the parameter ΔSUM (= SUM1 - SUM2) considered. It was found that in compounds with a considerable ΔSUM value, the more pyramidal N atoms are usually oriented so that the corresponding lone electron pair is anti with respect to the P=O group. In (I), (II) and (III), the phosphoryl and carbonyl groups, separated by an N atom, are anti with respect to each other. In the C(O)NHP(O) fragment of (I)-(III), the P-N bond is longer and the O-P-N angle is contracted compared with the other two P-N bonds and the O-P-N angles in the molecules. These effects are also seen in analogous compounds deposited in the CSD. Compounds with [C(O)NH]P(O)[N]X (X ≠ N), such as compounds with a [C(O)NH]P(O)[N][O] skeleton, have not been considered here. Also, compounds with a [C(O)NH](2)P(O)[N] fragment have not been reported to date. In the crystal structures of all three title compounds, adjacent molecules are linked via pairs of P=O···H-N hydrogen bonds, forming dimers with C(i) symmetry.

  17. 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.

  18. Effects of temperature and sodium carboxylate additives on mineralization of calcium oxalate in silica gel systems

    Institute of Scientific and Technical Information of China (English)

    OUYANG; Jianming; DENG; Suiping; LI; Xiangping; TAN; Yanh

    2004-01-01

    [1]Ouyang, J. M., Yao, X. Q., Su, Z. X. et al., Simulation of calcium oxalate stone in Vitro, Science in China, Ser. B, 2003, 46(3):234-242.[2]Xu, S. H., Chen, J. Q., Zhou, H., Nepidemiological study of renal calculus in Shenshen region, Chin. J. Urol. (in Chinese), 1999,20(11): 655-657.[3]Bretherton, T., Rodgers, A., Crystallization of calcium oxalate in minimally diluted urine, J. Crystal Growth, 1998, 192: 448-455.[4]Grover, P. K., Ryall, R. L., Effect of seed crystals of uric acid and monosodium urate on the crystallization of CaOxa in undiluted human urine in vitro, Clin. Sci., 1997, 92: 205-213.[5]Laube, N., Mohr, B., Hesse, A., Laser-probe-based investigation of the evolution of particle size distributions of calcium oxalate particles formed in artificial urines, J. Crystal Growth, 2001, 233:367-374.[6]Tunik, L., Fueredi-Milhofer, H., Garti, N., Adsorption of sodium diisooctyl sulfosuccinate onto calcium oxalate crystals, Langmuir,1998, 14: 3351-3355.[7]Cody, A. M., Cody, R. D., Calcium oxalate trihydrate phase control by structurally-specific carboxylic acids, J. Cryst. Growth,1994, 135: 234-245.[8]Ouyang, J. M., Duan, L., Tieke, B., Effects of carboxylic acids on the crystal growth of calcium oxalate nanoparticles in lecithin-water liposome systems, Langmuir, 2003, 19: 8980-8985.[9]Guo, S., Ward, M. D., Wesson, J. A., Direct visualization of calcium oxalate monohydrate crystallization and dissolution with atomic force microscopy and the role of polymeric additives,Langmuir, 2002, 18:4284-4291.[10]Yasui, T., Sato, M., Fujita, K., Effects of citrate on renal stone formation and osteopontin expression in a rat urolithiasis model,Urol. Res., 2001,29: 50-56.[11]Ouyang, J. M., Deng, S. P., Controlled and uncontrolled crystallization of calcium oxalate monohydrate in the presence of citric acid, Dalton Transactions, 2003, (14): 2846-2851.[12]Khan, S. R., Whalen, P. O., Glenton, P. A., Heterogeneous nucleation of

  19. Multi-​Dimensional Separations of Polymers

    NARCIS (Netherlands)

    Schoenmakers, P.; Aarnoutse, P.

    2014-01-01

    Synthetic polymers and comprehensive two-​dimensional liq. chromatog. (LC×LC) are a synergistic combination. LC×LC provides unique insights in mutually dependent mol. distributions. Synthetic polymers offer clear demonstrations of the value of LC×LC.

  20. Liquid polystyrene: a room-temperature photocurable soft lithography compatible pour-and-cure-type polystyrene.

    Science.gov (United States)

    Nargang, Tobias M; Brockmann, Lara; Nikolov, Pavel Mitkov; Schild, Dieter; Helmer, Dorothea; Keller, Nico; Sachsenheimer, Kai; Wilhelm, Elisabeth; Pires, Leonardo; Dirschka, Marian; Kolew, Alexander; Schneider, Marc; Worgull, Matthias; Giselbrecht, Stefan; Neumann, Christiane; Rapp, Bastian E

    2014-08-07

    Materials matter in microfluidics. Since the introduction of soft lithography as a prototyping technique and polydimethylsiloxane (PDMS) as material of choice the microfluidics community has settled with using this material almost exclusively. However, for many applications PDMS is not an ideal material given its limited solvent resistance and hydrophobicity which makes it especially disadvantageous for certain cell-based assays. For these applications polystyrene (PS) would be a better choice. PS has been used in biology research and analytics for decades and numerous protocols have been developed and optimized for it. However, PS has not found widespread use in microfluidics mainly because, being a thermoplastic material, it is typically structured using industrial polymer replication techniques. This makes PS unsuitable for prototyping. In this paper, we introduce a new structuring method for PS which is compatible with soft lithography prototyping. We develop a liquid PS prepolymer which we term as "Liquid Polystyrene" (liqPS). liqPS is a viscous free-flowing liquid which can be cured by visible light exposure using soft replication templates, e.g., made from PDMS. Using liqPS prototyping microfluidic systems in PS is as easy as prototyping microfluidic systems in PDMS. We demonstrate that cured liqPS is (chemically and physically) identical to commercial PS. Comparative studies on mouse fibroblasts L929 showed that liqPS cannot be distinguished from commercial PS in such experiments. Researchers can develop and optimize microfluidic structures using liqPS and soft lithography. Once the device is to be commercialized it can be manufactured using scalable industrial polymer replication techniques in PS--the material is the same in both cases. Therefore, liqPS effectively closes the gap between "microfluidic prototyping" and "industrial microfluidics" by providing a common material.

  1. Role of basicity and tetrahedral speciation in controlling the thermodynamic properties of silicate liquids, part 1: the system CaO-MgO-Al 2O 3-SiO 2

    Science.gov (United States)

    Beckett, John R.

    2002-01-01

    Activity coefficients of oxide components in the system CaO-MgO-Al 2O 3-SiO 2 (CMAS) were calculated with the model of Berman (Berman R. G., "A thermodynamic model for multicomponent melts with application to the system CaO-MgO-Al 2O 3-SiO 2," Ph.D. dissertation, University of British Columbia, 1983) and used to explore large-scale relationships among these variables and between them and the liquid composition. On the basis of Berman's model, the natural logarithm of the activity coefficient of MgO, ln(γ MgOLiq), and ln(γ MgOLiq/γ SiO 2Liq) are nearly linear functions of ln(γ CaOLiq). All three of these variables are simple functions of the optical basicity Λ with which they display minima near Λ ˜ 0.54 that are generated by liquids with low ratios of nonbridging to tetrahedral oxygens (NBO/T) (factor in determining the thermodynamic properties of aluminosilicate liquids. For a constant NBO/T, ln(γ CaOLiq/γ Al 2O 3Liq) and ln(γ MgOLiqγ Al 2O 3Liq) form curves in terms of X SiO 2Liq/X Al 2O 3Liq. The same liquids that generate minima in the Λ plots are also associated with minima in ln(γ CaOLiqγ Al 2O 3Liq) and ln(γ MgOLiqγ Al 2O 3Liq) as a function of X SiO 2Liq/X Al 2O 3Liq. In addition, there are maxima or sharp changes in slope for NBO/T > 0.3, which occur for X SiO 2Liq/X Al 2O 3Liq ranging from ˜0 to ˜6 and increase with increasing NBO/T. The systematic variations in activity coefficients as a function of composition and optical basicity reflect underlying shifts in speciation as the composition of the liquid is changed. On the basis of correlations among the activity coefficients, it is likely that the use of CaO, an exchange component such as SiMg -1 and two of MgO, CaAl 2O 4, or MgAl 2O 4 would yield significant savings in the number of parameters required to model the excess free energy surface of liquids over large portions of CMAS relative to the use of oxide end members. Systematic behavior of thermodynamic properties extends to small

  2. 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.

  3. 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

  4. Exploring Jupiter's icy moons with old techniques and big facilities - new insights on sulfuric acid hydrates

    Science.gov (United States)

    Maynard-Casely, H. E.; Avdeev, M.; Brand, H.; Wallwork, K.

    2013-12-01

    ., AIP Conf Proc, 2007. 879: p. 879-882. [5] Liss, K.D., et al., Phys B-Cond Mat, 2006. 385-86: p. 1010-1012. [6] Maynard-Casely, H.E., K.S. Wallwork, and M. Avdeev, (In review). [7] Maynard-Casely, H.E., H.E.A. Brand, and K.S. Wallwork, J.of App.Cryst, 2012. 45: p.1198-1207. [8] Maynard-Casely, H.E., K.S. Wallwork, and H.E.A. Brand, (In Preparation). Stages of the crystal structure determination of sulfruic acid octahydrate a) the oxygen and sulfur postions were determined from the synchrotron x-ray data b) Once neutron diffraction data was collected Fourier difference methods were used to locate hydrogen positions to determine c) the full structure of sulfuric acid octahydrate.

  5. Synchrotron X-ray Scattering from Self-organized Soft Nanostructures in Clays

    Science.gov (United States)

    Fossum, J. O.

    2009-04-01

    . Gog, C. Venkataraman, Observations of orientational ordering in aqueous suspensions of a nano-layered silicate, ENERGY The International Journal 30, 873 (2005). 2. D. M. Fonseca, Y. Méheust, J. O. Fossum, K. D. Knudsen, K. J. Måløy and K. P. S. Parmar, Phase behavior of platelet-shaped nanosilicate colloids in saline solutions: A small-angle X-ray scattering study J. Appl. Cryst. 40 292 (2007) 3. E. N. de Azevedo, M. Engelsberg, J. O. Fossum, R. E. de Souza, Anisotropic water diffusion in nematic self-assemblies of clay nano-platelets suspended in water, Langmuir 23, 5100 (2007) 4. Nils Ivar Ringdal, Master thesis, Department of Physics, NTNU (2008) 5. J.O. Fossum, Y. Meheust, K.P.S. Parmar, K.D. Knudsen, K.J. Maloy, D.d.M. Fonseca, Intercalation-enhanced electric polarization and chain formation of nano-layered particles, Europhys. Lett., 74, 438 (2006), and in the Scientific Highlights 2006 of the European Synchrotron Radiation Facility - ESRF (2007) 6. K.P.S. Parmar, Y. Meheust, B. Schelderupsen and J.O. Fossum, Electrorheological suspensions of laponite in oil: rheometry studies, Langmuir 24,1814 (2008) 7. F. Bergaya, B. K. G. Theng, and G. Lagaly, editors. Handbook of Clay Science. Elsevier (2006)

  6. 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.

  7. Analyses of Cometary Silicate Crystals: DDA Spectral Modeling of Forsterite

    Science.gov (United States)

    Wooden, Diane

    2012-01-01

    Comets are the Solar System's deep freezers of gases, ices, and particulates that were present in the outer protoplanetary disk. Where comet nuclei accreted was so cold that CO ice (approximately 50K) and other supervolatile ices like ethane (C2H2) were preserved. However, comets also accreted high temperature minerals: silicate crystals that either condensed (greater than or equal to 1400 K) or that were annealed from amorphous (glassy) silicates (greater than 850-1000 K). By their rarity in the interstellar medium, cometary crystalline silicates are thought to be grains that formed in the inner disk and were then radially transported out to the cold and ice-rich regimes near Neptune. The questions that comets can potentially address are: How fast, how far, and over what duration were crystals that formed in the inner disk transported out to the comet-forming region(s)? In comets, the mass fractions of silicates that are crystalline, f_cryst, translate to benchmarks for protoplanetary disk radial transport models. The infamous comet Hale-Bopp has crystalline fractions of over 55%. The values for cometary crystalline mass fractions, however, are derived assuming that the mineralogy assessed for the submicron to micron-sized portion of the size distribution represents the compositional makeup of all larger grains in the coma. Models for fitting cometary SEDs make this assumption because models can only fit the observed features with submicron to micron-sized discrete crystals. On the other hand, larger (0.1-100 micrometer radii) porous grains composed of amorphous silicates and amorphous carbon can be easily computed with mixed medium theory wherein vacuum mixed into a spherical particle mimics a porous aggregate. If crystalline silicates are mixed in, the models completely fail to match the observations. Moreover, models for a size distribution of discrete crystalline forsterite grains commonly employs the CDE computational method for ellipsoidal platelets (c:a:b=8

  8. Crystal structures of a novel NNN pincer ligand and its dinuclear titanium(IV alkoxide pincer complex

    Directory of Open Access Journals (Sweden)

    Jakub Pedziwiatr

    2017-02-01

    is found in either one, perhaps due to the bulky groups around them. One of the ethyl groups of the ether ligand of 1 is disordered and refined in two parts with site-occupation factors of 0.812 (8 and 0.188 (8. One and a half toluene solvent molecules are also present in the asymmetric unit of 2. The toluene molecules were significantly disordered and could not be modeled properly, thus SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] was used to remove their contributions to the overall intensity data.

  9. Estimation of electron mobility of n-doped 4, 7-diphenyl-1, 10-phenanthroline using space-charge-limited currents

    Institute of Scientific and Technical Information of China (English)

    Khizar-ul-Haq; Khan M A; Jiang Xueyin; Zhang Zhilin; Zhang Xiaowen; Zhang Liang; Li Jun

    2009-01-01

    The electron mobilities of 4, 7-diphenyl-1, 10-phenanthroline (BPhen) doped 8-hydroxyquinolinatolithium (Liq) at various thicknesses (50-300 nm) have been estimated by using space-charge-limited current measurements. It is observed that the electron mobility of 33 wt% Liq doped BPhen approaches its true value when the thickness is more than 200 nm. The electron mobility of 33 wt% Liq doped BPhen at 300 nm is found to be ~5.2 × 10~(-3) cm~2/(V·s) (at 0.3 MV/cm) with weak dependence on electric field, which is about one order of magnitude higher than that of pristine BPhen (3.4 × 10~(-4) cm~2/(V·s)) measured by SCLC. For the typical thickness of organic light-emitting devices, the electron mobility of doped BPhen is also investigated.

  10. [In vitro absorption mechanism of strychnine and the transport interaction with liquiritin in Caco-2 cell monolayer model].

    Science.gov (United States)

    Wang, Jun-jun; Liao, Xiao-huan; Ye, Min; Chen, Yong

    2010-09-01

    To study the effect of liquiritin (Liq) on the transport of strychnine (Str) in Caco-2 cell monolayer model, the transport parameters of Str, such as apparent permeability coefficient (P app (B-->A) and P app (A-->B)) and cumulative transport amount (TRcum), were determined and comparatively analyzed when Str was used solely and co-used with Liq. The effect of drug concentrations, conveying times, P-glycoprotein (P-gp) inhibitor verapamil and conveying liquor pH values on the transport of Str were also investigated. The results indicated that the absorption of Str in Caco-2 cell monolayer model was well and the passive transference was the main intestinal absorption mechanism of Str in the Caco-2 monolayer model, along with the excretion action mediated by P-gp. Liq enhanced the absorption of Str. Meanwhile, conveying liquor pH value had significant influence on the excretion transport of Str.

  11. Pharm GKB: menthol [PharmGKB

    Lifescience Database Archive (English)

    Full Text Available strength with menthactin (dextromethorphan hydrobromide + guaifenesin + menthol + pseudoephedrine hydrochlo...ride) Benylin DM-e extra strength with menthactin (dextromethorphan hydrobromide + guaifenesin + menthol) Be... - CRM (menthol + methyl salicylate) Koffex DM-d-e - liq (dextromethorphan hydrobromide + guaifenesin + pseu

  12. AcEST: DK960040 [AcEST

    Lifescience Database Archive (English)

    Full Text Available Glutamate racemase OS=Brucella suis (strain... 31 7.1 sp|A5VQW7|MURI_BRUO2 Glutamate racemase OS=Brucella ov...AYPSVPFVGMV-PAIKPAAERTSSGLVSVLATPGTVKRAYTRD 144 Query: 180 LVQ 188 L+Q Sbjct: 145 LIQ 147 >sp|A5VQW7|MURI_BRUO2

  13. An Assessment of Hydrazine, Hydrazine Hydrate and Liquid Ammonia as Fuels for Rocket Propulsion

    Science.gov (United States)

    1949-08-01

    problems. Finally it should be mentioned that the Acre jet Engineering Corporation (33) have found that in solutions of Li in liq.i the metal amido is...also be stressed that the stability of the solutions of those borohydrides in NH3 and N2H4 does not seem to have been investigated. A summary of the

  14. Dynamics of a Disturbed Sessile Drop Measured by Atomic Force Microscopy (AFM)

    NARCIS (Netherlands)

    McGuiggan, Patricia M.; Grave, Daniel A.; Wallace, Jay S.; Cheng, Shengfeng; Prosperetti, Andrea; Robbins, Mark O.

    2011-01-01

    A new method for studying the dynamics of a sessile drop by atomic force microscopy (AFM) is demonstrated. A hydrophobic microsphere (radius, r 20–30 μm) is brought into contact with a small sessile water drop resting on a polytetrafluoroethylene (PTFE) surface. When the microsphere touches the liq

  15. S.H. Baxter

    African Journals Online (AJOL)

    day for dairy cows or mature fat cattle and the littering operations would ... ceased to function effectively and then a new development would occur based on a ... the capacity to absorb almost twice its weight of liqUidand therefore when used in ...

  16. 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.

  17. Market liquidity around earnings announcements

    NARCIS (Netherlands)

    Pronk, M.

    2002-01-01

    Prior literature indicates that bid-ask spreads are higher and depths are lower around earnings announcements than during non-announcement periods. This thesis investigates two important aspects of this drop in market liquidity, namely (a) the ability of management to mitigate the drop in market liq

  18. Thermodynamic and Gasdynamic Aspects of a Boiling Liquid Expanding Vapour Explosion

    NARCIS (Netherlands)

    Xie, M.

    2013-01-01

    The risk of explosion due to rupture of a tank filled with pressurized liquefied gas (PLG) is one of the risks to be considered in the context of studies on tunnel safety. When a vessel containing liquid well above its boiling point at normal atmospheric pressure fails catastrophically a Boiling Liq

  19. Separating mixtures by exploiting molecular packing effects in microporous materials

    NARCIS (Netherlands)

    Krishna, R.

    2014-01-01

    We examine mixt. sepns. with microporous adsorbents such as zeolites, metal-​org. frameworks (MOFs) and zeolitic imidazolate frameworks (ZIFs)​, operating under conditions close to pore satn. Pore satn. is realized, for example, when sepg. bulk liq. phase mixts. of polar compds. such as water, alcs.

  20. Accurate quantitation of pentaerythritol tetranitrate and its degradation products using liquid chromatography-​atmospheric pressure chemical ionization-​mass spectrometry

    NARCIS (Netherlands)

    Brust, H.; van Asten, A.; Koeberg, M.; Dalmolen, J.; van der Heijden, A.; Schoenmakers, P.

    2014-01-01

    After an explosion of pentaerythritol tetranitrate (PETN)​, its degrdn. products pentaerythritol trinitrate (PETriN)​, dinitrate (PEDiN)​, and mononitrate (PEMN) were detected using liq. chromatog.-​atm.-​pressure chem.-​ionization-​mass spectrometry (LC-​APCI-​MS)​. Discrimination between

  1. Novel method for non-intrusive measurement of velocity and slug length in two- and three-phase slug flow in capillaries

    NARCIS (Netherlands)

    Wolffenbuttel, BMA; Nijhuis, TA; Stankiewicz, A; Moulijn, JA

    2002-01-01

    A method was developed for the measurement of velocity and slug length of two and three-phase flow in capillaries. The method consists of the combination of an impedance meter and two IR sensors. Non-intrusive measurement of the velocity can be performed with the IR sensors in gas-liquid and gas-liq

  2. Directional flow induced by synchronized longitudinal and zeta-potential controlling AC-electrical fields

    NARCIS (Netherlands)

    Wouden, van der E.J.; Hermes, D.C.; Gardeniers, J.G.E.; Berg, van den A.

    2006-01-01

    Electroosmotic flow (EOF) in a microchannel can be controlled by electronic control of the surface charge using an electrode embedded in the wall of the channel. By setting a voltage to the electrode, the zeta-potential at the wall can be changed locally. Thus, the electrode acts as a "gate" for liq

  3. Relaxation phenomena in dense gas separation membranes

    NARCIS (Netherlands)

    Wessling, Matthias

    1993-01-01

    Solution-diffusion membranes are widely used for the separation of gaseous and liquid mixtures. The separation of air (O2/N2), landfill gas (CH4/CO2) and purge gas streams (NH3/H2) in the ammonia synthesis are examples for state-of-the-art membrane gas separation processes. For the separation of liq

  4. Lignin solubilisation and gentle fractionation in liquid ammonia

    NARCIS (Netherlands)

    Strassberger, Z.; Prinsen, P.; van der Klis, F.; van Es, D.S.; Tanase, S.; Rothenberg, G.

    2015-01-01

    We present a simple method for solubilizing lignin using liq. ammonia. Unlike water, which requires harsh conditions, ammonia can solubilize tech. lignins, in particular kraft lignin. A com. pine wood Kraft lignin (Indulin AT) was solubilized instantaneously at room temp. and 7-​11 bars autogenous

  5. Multiple testing issues in discriminating compound-related peaks and chromatograms from high frequency noise, spikes and solvent-based nois in LC-MS data sets

    NARCIS (Netherlands)

    Nyangoma, S.O.; Van Kampen, A.A.; Reijmers, T.H.; Govorukhina, N.I; van der Zee, A.G.; Billingham, I.J; Bischoff, Rainer; Jansen, R.C.

    2007-01-01

    Multiple testing issues in discriminating compound-related peaks and chromatograms from high frequency noise, spikes and solvent-based noise in LC-MS data sets.Nyangoma SO, van Kampen AA, Reijmers TH, Govorukhina NI, van der Zee AG, Billingham LJ, Bischoff R, Jansen RC. University of Birmingham. Liq

  6. 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...

  7. Download this PDF file

    African Journals Online (AJOL)

    day on daily record forms throughout the experiment. The crisps ... groups were combined (table 2). By t-test than the mean differences between canola and palmolein were ... Plasma Total Ch0lBSl€r()|i(mm0l/IQ First Series. Plamolein (3 wks) ...

  8. 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.

  9. 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.

  10. Annual report of Naka Fusion Research Establishment. From April 1,2000 to March 31, 2001

    Energy Technology Data Exchange (ETDEWEB)

    Kuriyama, Masaaki; Kizu, Kaname; Kusakawa, Fumio; Matsumoto, Hiroshi; Sakamoto, Keishi; Sengoku, Seio (eds.) [Japan Atomic Energy Research Inst., Naka, Ibaraki (Japan). Naka Fusion Research Establishment

    2001-11-01

    and groove by remote handling. 8) Fusion Neutronics: Radiation detectors using single cryst

  11. Termochemical Models For Slags and Silicate Melts, Review and Perspectives

    Science.gov (United States)

    Ottonello, G.

    R.O. (1983) Contrib. Mineral. Petrol., 84, 107-145. [3] Papale P. (1997) Contrib. Mineral. Petrol., 126, 237-251. [4] Papale P. (1999) Amer. Mineral., 84, 477-492. [5] Nuccio P.M. and Paonita A. (2999) Earth Planet. Sci. Letters., 183, 499-512. [6] Berman R.G. and Brown T.H. (1984) Geochim. Cosmochim. Acta, 48, 661-678. [7] Lin P.L. and Pelton A.D. (1979) Metall. Trans. B., 10B, 667-675. [8] Pelton A.D. and Blander M. (1986) Metall. Trans. B., 17B, 805-15. [9] Kapoor M.L., Mehrotre G.M. and Frohberg M.G. (1975) Proc. Aust. Inst. Mining Metall., 254, 11. [10] Kapoor M.L., Frohberg G.M. (1971) Proc. Symp. "Chemical Metallurgy of Iron and Steel" Sheffield. [11] Taylor J.R. and Dinsdale A.T. (1990] CALPHAD, 14, 71-88. [12] Sastri P. and Lahiri A.K. (1986) Metall. Trans. B., 17B, 105-110. [13] Bjorkman B. (1985) CALPHAD, 9, 271-282. [14] Hastie J.W., Horton W.S., Plante E.R. and Bonnell D.W. (1982) High Temp. High Press., 14, 669-679. [15] Goel R.P., Kellogg H.H. and Larrain J.M. (1980) Metall. Trans. B., 11B, 107-117. [16] Hillert M., Sundman B. and Wang X. (1990) Metall. Trans. B., 21B, 303-12. [17] Hoch M. and Arpshofen I. (1984) Zeits. fur Metallkde., 75, 23-29. [18] Masson C.R. (1965) Proc. Roy. Soc. London, A287, 201-221. [19] Masson C.R. (1968) J. Amer. Ceram. Soc., 51, 134-143. [20] Masson C.R. (1972) Jour. Iron Steel Inst., 210, 89-96. [21] Toop G.W. and Samis C.S. (1962) Can. Met. Quart., 1, 129-52. [22] Toop G.W. and Samis C.S. (1962) Trans. AIME, 224, 878-87. [23] Ottonello G., Moretti R., Marini L. and Vetuschi Zuccolini M. (2000) Chem. Geol., 174, 157-179. [24] Ottonello G. (2001) J. Non-Cryst. Solids, 282, 72-85. [25] Moretti R. and Ottonello G. (2002) , Metall. Trans. (submitted).

  12. Model-Driven Development for scientific computing. Computations of RHEED intensities for a disordered surface. Part I

    Science.gov (United States)

    Daniluk, Andrzej

    2010-03-01

    separate thread inside each transaction generated by the master Growth09 program (see pii:S0010-4655(09)00386-5 A. Daniluk, Model-Driven Development for scientific computing. Computations of RHEED intensities for a disordered surface. Part II The RHEED1DProcess requires the user to provide the appropriate parameters for the crystal structure under investigation. These parameters are loaded from the parameters.ini file at run-time. Instructions on the preparation of the .ini files can be found in the new distribution. The RHEED1DProcess requires the user to provide the appropriate values of the layers of coverage profiles. The CoverageProfiles.dat file (generated by Growth09 master application) at run-time loads these values. The RHEED1DProcess enables carrying out one-dimensional dynamical calculations for the fcc lattice, with a two-atoms basis and fcc lattice, with one atom basis but yet the zeroth Fourier component of the scattering potential in the TRHEED1D::crystPotUg() function can be modified according to users' specific application requirements. * The figures mentioned can be downloaded, see "Supplementary material" below. Unusual features: The program is distributed in the form of main projects RHEED1DProcess.cbproj and Graph2D0x.cbproj with associated files, and should be compiled using Embarcadero RAD Studio 2010 along with Together visual-modelling platform. The program should be compiled with English/USA regional and language options. Additional comments: This version of the RHEED program is designed to run in conjunction with the GROWTH09 (ADVL_v3_0) program. It does not replace the previous, stand alone, RHEEDGR-09 (ADUY_v3_0) version. Running time: The typical running time is machine and user-parameters dependent. References:[1] OMG, Model Driven Architecture Guide Version 1.0.1, 2003.

  13. Model-Driven Development for scientific computing. An upgrade of the RHEEDGr program

    Science.gov (United States)

    Daniluk, Andrzej

    2009-11-01

    calculations for the fcc lattice, with a two-atoms basis and fcc lattice, with one atom basis but yet the zeroth Fourier component of the scattering potential in the TRHEED1D::crystPotUg() function can be modified according to users' specific application requirements. A graphical user interface (GUI) for the program has been reconstructed. The program has been compiled with English/USA regional and language options. Unusual features: The program is distributed in the form of main projects RHEEDGr_09.cbproj and Graph2D0x.cbproj with associated files, and should be compiled using Code Gear C++ Builder 2009 compilers. Running time: The typical running time is machine and user-parameters dependent. References: OMG, Model Driven Architecture Guide Version 1.0.1, 2003, http://www.omg.org/cgi-bin/doc?omg/03-06-01. A. Daniluk, Comput. Phys. Comm. 166 (2005) 123.

  14. 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

  15. BARRINGER AWARD ADDRESS: Shock Metamorphism of Quartz in Nature and Experiment: A Review

    Science.gov (United States)

    Stoffler, D.

    1993-07-01

    . (1985) Phys. Chem. Mineral., 11, 241- 249. [8] Stoffler D. (1984) J. Non-Cryst. Solids, 67, 465-502, and references therein. [9] Gratz A. J. (1992) Phys. Chem. Mineral., 19, 267-288, [10] Rehfeldt-Oskierski A. (1986) Ph.D. thesis, Univ. of Munster. [11] Grothues J. (1988) Diploma thesis, Univ. of Muenster [12] Langenhorst F. (1993), Ph.D. thesis, Univ. of Munster. [13] Kieffer S. W. et al. (1976) Contr. Mineral. Petrol., 59, 41-93, [14] Langenhorst F. (1992) Nature, 356, 507-509.

  16. Interaction of host-guest complexes of cucurbit[n]urils with double probe guests

    Institute of Scientific and Technical Information of China (English)

    MA; Peihua; DONG; Jun; XIANG; Shuangchun; XUE; Saifeng; ZH

    2004-01-01

    -cucurbituril: cis-SnCl4(OH2)2 @cucurbit[7]uril, Cryst. Eng.Comm., 2001, 49: 1-7.[13]Krasia, T. C., Steinke, J. H. G., Formation of oligotriazoles catalysed by cucurbituril, Chem. Commun. (Camb.), 2002, 1: 22-23.[14]Kim, H. J., Heo, J., Jeon, W. S. et al., Selective inclusion of a hetero-guest pair in a molecular host: formation of stable charge-transfer complexes in cucurbit[8]uril, Angew. Chem. Int.Ed., 2001, 40(8): 1526-1529.[15]Burnett, C. A., Witt, D., Fettinger, J. C. et al., A cyclic congener of cucurbituril: synthesis and recognition properties, J. Org.Chem., 2003, 68(16): 6184-6191.[16]Samsonenko, D. G., Virovets, A. V., Lipkowski, J. et al., Distortion of the cucurbituril molecule by an included 4-methylpyridinum cation, J. Struc. Chem. (Translation of Zhurnal Strukturnoi Khimii), 2002, 43(4): 664-668.[17]Lim, Y. b., Kim, T., Lee, J. W. et al., Self-assembled ternary complex of cationic dendrimer, cucurbituril, and DNA: noncovalent strategy in developing a gene delivery carrier, Bioconjugate Chem., 2002, 13(6): 1181-1185.[18]Miyahara, Y., Abe, K., Inazu, T., "Molecular" molecular sieves:lid-free decamethylcucurbit[5]uril absorbs and desorbs gases selectively, Angew. Chem. Int. Ed., 2002, 41 (16): 3020-3023.[19]Tan, Y., Choi, S. W., Lee, J. W. et al., Synthesis and characterization of novel side-chain pseudopol- yrotaxanes containing cucurbituril, Macromolecules, 2002, 35(18): 7161-7165.[20]Ong, W., Gomez, K. M., Kaifer, A. E., Cucurbit[7]uril: a very effective host for viologens and their cation radicals, Org. Lett.,2002, 4(10): 1791-1794.[21]Shen, Y. Q., Xue, S. F., Zhao, Y. J. et al., NMR study on self-assembled cage complex of hexamethylenetetramine and cucurbit[n]urils, Chinese Science Bulletin, 2004, 48(1): 2694-2697.[22]Luo, X. Q., Xue, S. F., Zhu, Q. J., A new method for synthesis and separation of a new family cage compounds-cucurbit[n = 5-8]urils, J. Guizhou Univ. (Nat. Sci.), 2003, 20(1): 184-187.

  17. 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

  18. 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.

  19. Absolute-magnetic-field measurement using nanogranular in-gap magnetic sensor with second-harmonic and liquid-nitrogen-temperature operation

    Science.gov (United States)

    Tsukada, Keiji; Yasugi, Takuya; Majima, Yatsuse; Sakai, Kenji; Kiwa, Toshihiko

    2017-05-01

    To detect the absolute magnetic field, such as the earth's magnetic field, a linear magnetic response, a zero point, and thermal stability are required. We thus propose an operating method and sensor probe consisting of a nanogranular in-gap magnetic sensor (GIGS), an operational amplifier integrated circuit, and a modulation coil. The sensor probe was operated in second-harmonic mode at a liquid-nitrogen (Liq. N2) temperature. When an AC magnetic field was applied to GIGS, the second-harmonic signal was generated and modulated by the outer magnetic field to be measured. After lock-in detection, the modulated output signal showed good linearity and a zero point. Moreover, higher sensitivity and low noise with low thermal fluctuation was obtained by the cooling at Liq. N2 temperature.

  20. Absolute-magnetic-field measurement using nanogranular in-gap magnetic sensor with second-harmonic and liquid-nitrogen-temperature operation

    Directory of Open Access Journals (Sweden)

    Keiji Tsukada

    2017-05-01

    Full Text Available To detect the absolute magnetic field, such as the earth’s magnetic field, a linear magnetic response, a zero point, and thermal stability are required. We thus propose an operating method and sensor probe consisting of a nanogranular in-gap magnetic sensor (GIGS, an operational amplifier integrated circuit, and a modulation coil. The sensor probe was operated in second-harmonic mode at a liquid-nitrogen (Liq. N2 temperature. When an AC magnetic field was applied to GIGS, the second-harmonic signal was generated and modulated by the outer magnetic field to be measured. After lock-in detection, the modulated output signal showed good linearity and a zero point. Moreover, higher sensitivity and low noise with low thermal fluctuation was obtained by the cooling at Liq. N2 temperature.

  1. Meningite pneumocócica: Tratamento pela penicilina associada a sulfapiridina

    Directory of Open Access Journals (Sweden)

    J. M. Taques Bittencourt

    1945-09-01

    Full Text Available E' relatado um caso de meningite pneumocócica pós-otite e mastoidite, tratado com sucesso pela penicilina associada à sulfapiridina. Tanto o composto sulfonamídico como a penicilina isoladamente não tiveram efeito terapêutico satisfatório. A evolução da meningite é estudada por exames diários do liqüido cefalorraquidiano.

  2. Two-Dimensional Electrons.

    Science.gov (United States)

    2014-09-26

    Isihara and Y. Nalane, Elementary Excitations and Energy Dispersion in TTF-TCNQ;Proc. Internat. Conf. on Phys. and Chem. of Low-Dimen. Syn. Conductors ...Abano Terme, Molec. Crys. Liq. Crys. 120, 85 (1984). One-dimensiona4 conductors such as TTF-TCNQ are attracting considerable attention for their...A. Isihara and Y. Nakane; Magnetoconductivity of 2D Conductors ; Proc. Internat. Conf. on Phys. and Chem. of Low-Dimen. Syn. Conductors , Abano Terme

  3. The thickness of native oxides on aluminum alloys and single crystals

    OpenAIRE

    Evertsson, J.; Bertram, F.; Weissenrieder, J.; Goethelid, Mats; Pan, J; Mikkelsen, A.; Nilsson, J.-O.; Lundgren, E.; Zhang, F.; Rullik, L.; Merte, L. R.; Shipilin, Mikhail; Soldemo, M.; S Ahmadi; Vinogradov, N.

    2015-01-01

    We present results from measurements of the native oxide film thickness on four different industrial aluminum alloys and three different aluminum single crystals. The thicknesses were determined using X-ray reflectivity, X-ray photoelectron spectroscopy, and electrochemical impedance spectroscopy. In addition, atomic force microscopy was used for micro-structural studies of the oxide surfaces. The reflectivity measurements were performed in ultra-high vacuum, vacuum, ambient, nitrogen and liq...

  4. Nuclear Blast Response Computer Program. Volume I. Program Description.

    Science.gov (United States)

    1981-08-01

    TIMG GUST VELOCITY TIMES 15 Lii NTMGST RHO GUST DENSITY 16 L12 NFPEQ PLOTF PLOT ARRAY 17 L13 NFFEC PLOTA PLOT ARRAY 18 LIQ 2-NFPEQ FTG FOURIER... PLOTF PLOT ARRAY 6P4 L17 MAX3 PLOTA PLOT ARRAY 6P5 L18 2-NFEEQ FTG FOURIER TRANSFORM OF VG-RHO 6B6 L19 NFORC-NTRSP P FORCES & PRESSURES VS TIME

  5. Samarium—promoted Chemoselective Reduction of Aromatic Nitro Compounds in Ionic Liquid

    Institute of Scientific and Technical Information of China (English)

    郑兴良; 张永敏; 等

    2002-01-01

    The differently substituted aromatic nitro compounds were chemoselectively reduced by Sm/HOAc system in an ionic liq-uid medium to afford aromatic amines,Under these conditions the other substituents,such as -X,-CHO,-COOH,-CN,-NHTos and -alkyl,remained intact,the notable advan-tages of this reaction are its mild conditions ,simple operation,short reaction time,high yields and easy recycling of ionic liquid.

  6. PRIVATE INVESTMENT AND FINANCIAL SECTOR POLICIES IN DEVELOPING COUNTRIES

    OpenAIRE

    James Ang

    2008-01-01

    This paper examines the role of financial sector policies in determining private investment in the economies of India and Malaysia. The results suggest that the presence of significant directed credit programs favoring certain priority sectors in the economies appear to be harmful for private capital formation in both countries. Interest rate controls seem to have a positive impact on investment in the private sector, and the effect is found to be stronger in India. While high reserve and liq...

  7. 兵庫県南部地震による液状化災害(<特集>阪神・淡路大震災特集)

    OpenAIRE

    嘉門, 雅史; 三村, 衛; Masashi, KAMON; Mamoru, MIMURA; 京都大学防災研究所; Disaster Prevention Research Institute, Kyoto University

    1995-01-01

    The 1995 Hyogoken-nambu earthquake struck the Kansai area at 5 : 46 on January 17,1995,causing catastrophic damage in Kobe and adjacent cities. In terms of geotechnical problems, liquefaction of loose sand deposits occurred mainly in reclaimed land. It is noted that non-liquefiable soils such as decomposed granite as well as cohesive soils with fine particles were ejected during this eartquake. Based on the field survey, ground improvement is proved to be effective as a countermeasure for liq...

  8. Enrichissement nutritionnel de l'huile d'olive : entre tradition et innovation

    OpenAIRE

    Veillet, Sébastien

    2010-01-01

    Olive oil is an ancestral product widely known for its benefic effects on human health. Its processing has changed a lot through centuries, especially these past few years with the increasing automation of the production lines. The first part of this manuscript describes these evolutions while the second part gives details on the influence of each processing step on the nutritional composition of the olive oil. We have studied the influence of the crushing systems, liquid-liquid and solid-liq...

  9. Incoporating Ammonia Synthesis for an Offshore Gas-to-Liquid Process

    OpenAIRE

    2016-01-01

    The world energy demand is increasing, and so is the demand for fertilizer to sustain an exponential population growth. Currently, with low oil prices, asso- ciated natural gas is flared off or re-injected into oil reservoirs for enhanced oil recovery (EOR). A gas-to-liquid process (GTL) for offshore applications aboard a foating production, storage, and offoading vessel (FPSO) incorpo- rating Fischer-Tropsch Synthesis (FTS) seeks to reform natural gas into more valuable liq...

  10. Internal Wave Generation by Convection

    OpenAIRE

    Lecoanet, Daniel

    2016-01-01

    In nature, it is not unusual to find stably stratified fluid adjacent to convectively unstable fluid. This can occur in the Earth's atmosphere, where the troposphere is convective and the stratosphere is stably stratified; in lakes, where surface solar heating can drive convection above stably stratified fresh water; in the oceans, where geothermal heating can drive convection near the ocean floor, but the water above is stably stratified due to salinity gradients; possible in the Earth's liq...

  11. Identification of Eupatilin from Artemisia argyi as a Selective PPARα Agonist Using Affinity Selection Ultrafiltration LC-MS

    OpenAIRE

    Yongsoo Choi; Yujung Jung; Su-Nam Kim

    2015-01-01

    Peroxisome proliferator-activated receptors (PPARs) are key nuclear receptors and therapeutic targets for the treatment of metabolic diseases through the regulation of insulin resistance, diabetes, and dyslipidemia. Although a few drugs that target PPARs have been approved, more diverse and novel PPAR ligands are necessary to improve the safety and efficacy of available drugs. To expedite the search for new natural agonists of PPARs, we developed a screening assay based on ultrafiltration liq...

  12. High-Pressure Fibrin Sealant Foam: An Effective Hemostatic Agent for Treating Severe Parenchymal Hemorrhage

    Science.gov (United States)

    2008-01-01

    compression or vascular control. Materials and methods. FSF with high fibrinogen concentration (20 mg/mL) and low thrombin activity (5 U/mL) was prepared and...fibrin sealant foam (FSF) into a body cavity via trocar would spread throughout the cavity, bind to damaged tissue, and stop bleeding from inaccessible...liver hemorrhage model in anticoagulated rabbits. We then compared pressurized FSF with liq- uid and a powdered form of fibrin sealant. MATERIALS AND

  13. Capture rate and neutron helicity asymmetry for ordinary muon capture on hydrogen

    CERN Document Server

    Ando, S; Kubodera, K; Ando, Shung-ichi; Myhrer, Fred; Kubodera, Kuniharu

    2001-01-01

    Applying heavy-baryon chiral perturbation theory to ordinary muon capture (OMC) on a proton, we calculate the capture rate and neutron helicity asymmetry up to next-to-next-to-leading order. For the singlet hyperfine state, we obtain the capture rate Gamma_0 = 695 sec^{-1} while, for the triplet hyperfine state, we obtain the capture rate Gamma_1 = 11.9 sec^{-1} and the neutron asymmetry alpha_1 = 0.93. If the existing formalism is used to relate these atomic capture rate to Gamma_{liq}, the OMC rate in liquid hydrogen, then Gamma_{liq} corresponding to our improved values of Gamma_0 and Gamma_1 is found to be significantly larger than the experimental value. We argue that this apparent difficulity may be correlated to the specious anomaly recently reported for mu^- + p to n + nu_mu + gamma, and we suggest a possibility to remove these two "problems" simply and simultaneously by reexamining the molecular physics input that underlies the conventional analysis of Gamma_{liq}.

  14. Mesial Temporal Lobe and Memory Function in Autism Spectrum Disorder: An Exploration of Volumetric Findings

    Science.gov (United States)

    Trontel, Haley G.; Duffield, Tyler C.; Bigler, Erin D.; Abildskov, Tracy J.; Froehlich, Alyson; Prigge, Molly B.D.; Travers, Brittany G.; Anderson, Jeffrey S.; Zielinski, Brandon A.; Alexander, Andrew; Lange, Nicholas; Lainhart, Janet E.

    2015-01-01

    Studies have shown that individuals with autism spectrum disorder (ASD) tend to perform significantly below typical developing individuals on standardized measures of memory, even when not significantly different on measures of IQ. The current study sought to examine within ASD whether anatomical correlates of memory performance differed between those with average-to-above-average IQ (AIQ Group) compared to those with low average to borderline ability (LIQ group) as well as in relations to typically-developing comparisons (TDC). Using automated volumetric analyses, we examined regional volume of classic memory areas including the hippocampus, parahippocampal gyrus, entorhinal cortex, and amygdala in an all-male sample AIQ (n = 38) and LIQ (n = 18) individuals with ASD along with 30 typically-developing comparisons (TDC). Memory performance was assessed using the Test of Memory and Learning (TOMAL) compared among the groups and then correlated with regional brain volumes. Analyses revealed group differences on almost all facets of memory and learning as assessed by the various subtests of the TOMAL. The three groups did not differ on any ROI memory-related brain volumes. However, significant size-memory function interactions were observed. Negative correlations were found between the volume of the amygdala and composite, verbal, and delayed memory indices for the LIQ ASD group indicating larger volume related to poorer performance. Implications for general memory functioning and dysfunctional neural connectivity in ASD are discussed. PMID:25749302

  15. 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

  16. The effect of liquid composition on the partitioning of Ni between olivine and silicate melt

    Science.gov (United States)

    Matzen, Andrew K.; Baker, Michael B.; Beckett, John R.; Wood, Bernard J.; Stolper, Edward M.

    2017-01-01

    We report the results of experiments designed to separate the effects of temperature and pressure from liquid composition on the partitioning of Ni between olivine and liquid, D_{{Ni}}^{{ol/liq}}. Experiments were performed from 1300 to 1600 °C and 1 atm to 3.0 GPa, using mid-ocean ridge basalt (MORB) glass surrounded by powdered olivine in graphite-Pt double capsules at high pressure and powdered MORB in crucibles fabricated from single crystals of San Carlos olivine at one atmosphere. In these experiments, pressure and temperature were varied in such a way that we produced a series of liquids, each with an approximately constant composition ( 12, 15, and 21 wt% MgO). Previously, we used a similar approach to show that D_{{Ni}}^{{ol/liq}} for a liquid with 18 wt% MgO is a strong function of temperature. Combining the new data presented here with our previous results allows us to separate the effects of temperature from composition. We fit our data based on a Ni-Mg exchange reaction, which yields ln ( {D_{{Ni}}^{{molar}} } ) = { -Δ _{r(1)} H_{{T_{{ref}} ,P_{{ref}} }}°}/RT + {Δ _{r(1)} S_{{T_{{ref}} ,P_{{ref}} }}°}/R - ln ( {{X_{{MgO}}^{{liq}} }/{X_{{{{MgSi}_{ 0. 5} {{O}}_{ 2} }}^{{ol}} }}} ). Each subset of constant composition experiments displays roughly the same temperature dependence of D_{{Ni}}^{{ol/liq}} (i.e.,-Δ _{r(1)} H_{{T_{{ref}} ,P_{{ref}} }}°/R) as previously reported for liquids with 18 wt% MgO. Fitting new data presented here (15 experiments) in conjunction with our 13 previously published experiments (those with 18 wt% MgO in the silicate liquid) to the above expression gives -Δ _{r(1)} H_{{T_{{ref}} ,P_{{ref}} }}°/R = 3641 ± 396 (K) and Δ _{r(1)} S_{{T_{{ref}} ,P_{{ref}} }}° /R = - 1.597 ± 0.229. Adding data from the literature yields -Δ _{r(1)} H_{{T_{{ref}} ,P_{{ref}} }}° /R = 4505 ± 196 (K) and Δ _{r(1)} S_{{T_{{ref}} ,P_{{ref}} }}° /R = - 2.075 ± 0.120, a set of coefficients that leads to a predictive equation for D_{{Ni}}^{{ol/liq

  17. Paracoccus niistensis sp. nov., isolated from forest soil, India

    Digital Repository Service at National Institute of Oceanography (India)

    Dastager, S.G.; Deepa, C.K.; Li, Wen-Jun; Tang, Shu-Kun; Pandey, A.

    stream_size 21756 stream_content_type text/plain stream_name Antonie van Leeuwenhoek_99_501a.pdf.txt stream_source_info Antonie van Leeuwenhoek_99_501a.pdf.txt Content-Encoding UTF-8 Content-Type text/plain; charset=UTF-8... loaded ion exchange as stationary phases. J Liq Chromatogr 5 : 2359-2387 La H-J, Im W-T, Ten LN, Kang MS, Shin D-Y, Lee S-T (2005) Paracoccus koreensis sp. nov., isolated from anaerobic granules in an up flow anaerobic sludge blanket (UASB) reactor. Int...

  18. Convenient synthesis of volatile streptomyces lactones

    Digital Repository Service at National Institute of Oceanography (India)

    Amonkar, C.P.; Tilve, S.G.; Parameswaran, P.S.

    mixture was washed with benzene (2 × 20 mL). Benzene (50 mL) and phenolphthalein (2 drops) were added to the aqueous layer and 2 N NaOH was added dropwise with vigorous shaking till a pink colour persisted. The benzene layer was separated, washed with H 2... O (20 mL), brine (10 mL), dried over Na 2 SO 4 and concentrated to get a thick syrupy liq- uid which on scratching after addition of anhyd hexane (15 mL) re- sulted in a solid product. The solid, on recrystallisation (benzene– hexane), yielded...

  19. 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......) , and the std. molar enthalpy of formation, Delta form H (o,m)(EuBr2, s, 298.15 K), the thermodn. functions of europium dibromide were calcd. up to T = 1300 K. Preliminary structural investigations were conducted both by reflectometry and Raman spectroscopy....

  20. 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...

  1. Quenching and Tempering for 42 CrMo4 Steel Forged Gear Ring%42 CrM o4钢锻辗齿圈的调质处理

    Institute of Scientific and Technical Information of China (English)

    王松林; 任秀凤; 张永庆; 刘守峰; 银伟; 王聪

    2014-01-01

    通过改进调质工艺,使用8%~10%的无机水基淬火液,改进淬火冷却工艺参数,解决了42CrMo4钢齿圈淬火开裂的问题。%By improving the tempering and quenching process , 8%~10%of inorganic water-based quenching liq-uid is used to improve the quench cooling process parameters and solve the crack problem during 42CrMo4 steel gear ring quenching .

  2. Análise ultra-estrutural do líquido cefalorraquiano de parkinsonianos

    Directory of Open Access Journals (Sweden)

    James Pitágoras de Mattos

    1990-03-01

    Full Text Available Pelo método da coloração negativa, o estudo ultra-estrutural do liqüido cefalorraquiano, em 20 casos de parkinsonismo, mostrou presença de estruturas não-identificadas, com configurações geométricas, em 30%. Consideradas como suspeitas de conterem partículas virais, por questão de método, não levaram a dados estatisticamente significativos se comparados à incidência de mortalidade entre os animais de experimentação. Artefatos ou não, estas estruturas merecem registro.

  3. A novel family of green ionic liquids with surface activities

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Ionic liquids have many unique properties as a new and remarkable class of environmental benign solvents,which promises widespread applications in industry and other areas. However,the ionic liq-uids with surface activity are rarely reported. In this work,a series of novel ionic liquids was synthe-sized by using N-methyl-2-pyrrolidone and alkyl bromide. The physical properties of this family of ionic liquids have been characterized,which shows that these compounds have ionic liquids characteristics,surface activity and biocompatibility.

  4. Hydrotrope-Solubilization Action of Urea in CTAB/n-C5H11-OH/H2 O System

    Institute of Scientific and Technical Information of China (English)

    GUO Rong; ZOU Ai-Hua; YANG Han-Min

    2001-01-01

    Urea can enhance the aqueous solubility of surfactant CTAB (hexadecyltrimethylammonium bromide) when it shows the hydrotrope action.It will show the hydrotrope-solubilization action when the solubilized amount microemulsion and that of n-C5H11OH in O/W increased The mechanism of the hydrotrope-solubilization ac-tion of urea is the increase of the stability of W/O and O/Wmicroemulsion and structural transition from the lamellar liq-uid crystalline phase to the bicontinuous structure.

  5. 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.

  6. Characterization of chemical speciation of titanyl sulfate solutions for production of titanium dioxide precipitates.

    Science.gov (United States)

    Szilágyi, István; Königsberger, Erich; May, Peter M

    2009-03-02

    Ion association in concentrated aqueous solutions of titanyl sulfate in sulfuric acid has been investigated at 25 degrees C by Raman spectroscopy under conditions like those used in the preparation of titania nanoparticles. Systematic variation of titanyl (M), sulfate (L), and hydrogen ion concentrations and a detailed quantitative analysis of the spectra reveal that two weak titanyl sulfato complexes (ML and ML(2)) are formed, with ML predominating. This assignment conflicts with the recent results of Baillon et al. (J. Mol. Liq. 2008, 143, 8-12).

  7. 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.

  8. Stability of Tranexamic Acid after 12-Week Storage at Temperatures from -20 deg C to 50 deg C

    Science.gov (United States)

    2013-07-01

    by thromboelastography (to measure the units/mL of SK needed to get 100% fibri- nolysis at 60 minutes [LY60]), and by high -performance liq- uid...Prescribed by ANSI Std Z39-18 de Guzman et al. TXA STABILITY AT DIFFERENT TEMPERATURES 395 in Afghanistan.7 Because of this survival benefit and the low ... fibrinogen , DD, protein C, von Willebrand’s factor, antithrombin III, and factors II, V, VII, VIII, IX, X, XI, XII, and XIII at 1, 2, 4, and 12 weeks

  9. Empirical valence bond model of an SN2 reaction in polar and nonpolar solvents

    Science.gov (United States)

    Benjamin, Ilan

    2008-08-01

    A new model for the substitution nucleophilic reaction (SN2) in solution is described using the empirical valence bond (EVB) method. The model includes a generalization to three dimensions of a collinear gas phase EVB model developed by Mathis et al. [J. Mol. Liq. 61, 81 (1994)] and a parametrization of solute-solvent interactions of four different solvents (water, ethanol, chloroform, and carbon tetrachloride). The model is used to compute (in these four solvents) reaction free energy profiles, reaction and solvent dynamics, a two-dimensional reaction/solvent free energy map, as well as a number of other properties that in the past have mostly been estimated.

  10. Thermal Engineering Issues in Hydrogen Storage for Mobile and Portable Applications

    Science.gov (United States)

    2010-09-01

    liq. • Ca(BH4)2 AB/cat. 0 + AIH3 Mg(BH,.b(NRJh • ~ 10 I I L iBHJ MgH2 LiBH,./CA 0 1 M-8-N-H O MgH2 • MD C-foam : • Li~gN • ILi~Hs/LiNH2...Hapke (1994) 15 Mg- MgH2 0.1 to 50 523 to 653 2 to 8 Oscillating heating technique Kapischke and Hapke (1998) Effective thermal conductivity of metal

  11. Room-temperature switching of magnetic hysteresis by reversible single-crystal-to-single-crystal solvent exchange in imidazole-inspired Fe(ii) complexes.

    Science.gov (United States)

    Huang, Wei; Shen, Fuxing; Zhang, Ming; Wu, Dayu; Pan, Feifei; Sato, Osamu

    2016-10-14

    The recent upsurge in molecular magnetism reflects its application in the areas of sensors and molecular switches. Thermal hysteresis is crucial to the molecular bistability and information storage, a wide hysteresis near room temperature is expected to be of practical sense for the molecular compound. In this work, spin crossover iron(ii) complexes [Fe(Liq)2](BF4)2·(CH3CH2)2O (1-Et2O) and [Fe(Liq)2](BF4)2·3H2O (1-3H2O) were prepared and structurally and magnetically analysed. The single-crystal-to-single-crystal (SCSC) solvation transformation and the influence on the crystal structures and magnetic hysteresis were investigated in an etherification-hydration cycle. At room temperature, X-ray diffraction experiments indicated a transformation from one crystal (1-Et2O, P21212) to another crystal (1-3H2O, P212121) upon humidity exposure and reversible recovery of its crystallinity upon exposure to ether vapor. The etherified phase 1-Et2O exhibits room temperature spin crossover (T1/2 = 305 K) but negligible thermal hysteresis, however the hydrated phase 1-3H2O exhibits the apparent hysteresis loop (T1/2↑ = 346 K, T1/2↓ = 326 K) which expands to room temperature. This effect is associated with the change of intermolecular cooperativity in the etherification-hydration recyclability.

  12. Effects of Acmella oleracea methanolic extract and fractions on the tyrosinase enzyme

    Directory of Open Access Journals (Sweden)

    Alan F. Barbosa

    2016-06-01

    Full Text Available Abstract The aim of the current study is to evaluate the effect of Acmella oleracea (L. R.K. Jansen, Asteraceae, methanolic extract, hexane (84.28% spilanthol and dichloromethane (approximately 100% spilanthol fractions on the tyrosinase enzyme. The dehydrated jambu extract was obtained through maceration using methanol. The extract residue was solubilized in MeOH/H2O (8:2 and subjected to liq.–liq. partition in organic solvents. Both the extraction and the partition procedures were conducted with three replicates. The analyses were performed using GC–MS, 1H and 13C NMR. The hexane fraction provided samples containing 84.28, 82.91 and 62.83% spilanthol in repetitions 1, 2 and 3, respectively. The dichloromethane fraction showed 88.55% spilanthol in repetition 1, and approximately 100% spilanthol in repetitions 2 and 3. The jambu extract as well as the hexane fraction (84.28% spilanthol were able to activate the oxidizing activity of the tyrosinase enzyme for L-DOPA. The dichloromethane fraction (approximately 100% spilanthol showed stronger inhibition effect on the tyrosinase enzyme in the first 10 min. The results raise the interest in study in spilanthol formulations for topical use, since it may prevent and/or slow skin hyperpigmentation or depigmentation processes. Furthermore, spilanthol may be used to control the enzymatic browning in fruits and vegetables.

  13. A Method for Estimating the Activity of Titania in Magmatic Liquids From the Compositions of Coexisting Rhombohedral and Cubic Iron-Titanium Oxides

    Science.gov (United States)

    Ghiorso, M. S.; Gualda, G. A.

    2011-12-01

    If the compositions of rhombohedral (hematite-ilmenite) and cubic (magnetite-ulvöspinel) oxide solid solutions found as phenocryst pairs in volcanic rocks are interpreted as reflecting pre-eruptive equilibrium growth conditions, then they may be utilized to estimate the temperature (T), oxygen fugacity (fO2), and the activity of titania (TiO2) in the liquid phase of the parental magma prior to eruption. The T and fO2 are obtained from the oxide compositions in the usual manner (e.g. Ghiorso and Evans, 2008, AJS, 308, 957-1039: GE2008). An internally consistent value for the activity of titania is obtained by evaluating two equilibria: [1] 2FeTiO3 (rhm) ↔ Fe2TiO4 (cubic) + TiO2 (liquid), and [2] TiO2 (liquid) ↔ TiO2 (rutile). Equilibria [1] implies the thermodynamic relation {aTiO2liquid = K[1] ( aFeTiO3rhm)2/aFe{2}TiO_4cubic, while [2] gives (aTiO2}liquid){sat = K[2], the latter referring to the activity of TiO2 in a liquid saturated with pure rutile. The ratio {aTiO2liquid/(aTiO2}liquid){sat ≡ aTiO2liq,rutile is the activity of titania in the liquid referenced to a standard state of rutile saturation (e.g., TitaniQ, Wark and Watson, CMP, 152, 743-754). It follows that K[3] = (K[1]/K[2]) = aTiO2liq,rutileaFe{2}TiO_4cubic/(aFeTiO3rhm)2, where K[3] corresponds to a new equilibrium constant for the combined reaction: 2FeTiO3 (rhm) ↔ Fe2TiO4 (cubic) + TiO2 (rutile). K[3] is independent of any assumption regarding the thermodynamic properties of liquid titania. Consequently, its value at specified T and pressure (P), may be obtained from GE2008 and Berman (for rutile, 1988, J.Petrol., 29, 445-522). From GE2008, the activities of the oxide endmembers may be estimated from their compositions. Taken together the aTiO2liq,rutile is obtained, along with T and fO2 from the compositions of coexisting Fe-Ti oxides. We have estimated aTiO2liq,rutile in 729 Fe-Ti oxide pairs from dacitic and rhyolitic volcanic rocks as previously tabulated by GE2008. Calculated values

  14. 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

  15. Particle processing technology

    Science.gov (United States)

    Yoshio, Sakka

    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

  16. 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

    2013-05-01

    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.

  17. Fabrication of ZnO nanorods in ionic liquids and their photoluminescent properties

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A novel and simple approach is reported to fabricate uniform single-crystal ZnO nanorods in ionic liq-uids. The as-obtained ZnO nanorods have been characterized by XRD,TEM,HRTEM,SAED,XPS,EDXA,PL and UV-vis absorption spectra. The rod diameters of the nanostructures can be controlled by tuning the amount of sodium hydroxide in the synthesis. Photoluminescence results show that the nanos-tructural ZnO exhibits better optical properties than bulk ZnO does and interestingly,the smaller the rod diameters are,the better optical property 1D nanostructural ZnO exhibits. The possible growth mechanism of ZnO nanorods is also investigated.

  18. 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

  19. Breve comentário sobre a patogenia da cisticercose espinhal

    Directory of Open Access Journals (Sweden)

    A. Sperlescu

    1989-03-01

    Full Text Available A hipótese de que embriões cisticercóticos possam alcançar os espaços suba-racnóideos espinhais por migração descendente a partir de espaços intracranianos previamente infestados não é compatível ao acometimento leptomeníngeo espinhal primário, que observamos em duas pacientes. É sugerido que nesses casos os embriões invadem o sistema nervoso central através do fluxo sangüíneo retrógrado pelo plexo venoso vertebral interno e veias intervertebrais, e que o compartimento intracraniano do liqüido cefalorraqueano possa ser secundariamente invadido pelos cisticercos.

  20. Changes in molar volume and heat capacity of actin upon polymerization.

    Science.gov (United States)

    Quirion, F; Gicquaud, C

    1993-11-01

    We have used densimetry and microcalorimetry to measure the changes in molar volume and heat capacity of the actin molecule during Mg(2+)-induced polymerization. Molar volume is decreased by 720 ml/mol. This result is in contradiction with previous measurements by Ikkai and Ooi [(1966) Science 152, 1756-1757], and by Swezey and Somero [(1985) Biochemistry 24, 852-860]: both of these groups reported increases in actin volume during polymerization, of 391 ml/mol and 63 ml/mol respectively. We also observed a decrease in heat capacity of about 69.5 kJ.K-1.mol-1 during polymerization. This is in agreement with the concept of conformational fluctuation of proteins proposed by Lumry and Gregory [(1989) J.Mol. Liq. 42, 113-144]whereby either ligand binding by a protein or monomer-monomer interaction decreases the protein's conformational flexibility.

  1. Criptococose do sistema nervoso central. Registro de um caso

    Directory of Open Access Journals (Sweden)

    Adherbal Tolosa

    1956-06-01

    Full Text Available Registro de caso de criptococose do sistema nervoso central, cujo diagnóstico foi estabelecido pelo exame do liqüido cefalorraquidiano. A presença do criptococo, verificada no exame direto, foi confirmada por culturas. O paciente apresentava quadro irritativo meníngeo, ao qual se associaram, ulteriormente, distúrbios encefálicos difusos e síndrome de hipertensão intracraniana. Evolução fatal após 4 meses de doença; foi tentada a sulfamido-terapia, sem resultado. O exame necroscópico confirmou a existência de leptomeningite difusa e micro-abscessos disseminados no córtex cerebral; o óbito foi relacionado à compressão bulbar por hérnia das tonsilas cerebelares.

  2. Optimization for microwave-assisted direct liquefaction of bamboo residue in glycerol/methanol mixtures

    Institute of Scientific and Technical Information of China (English)

    Jiulong Xie; Jinqiu Qi; Chungyun Hse; Todd F. Shupe

    2015-01-01

    Bamboo residues were liquefied in a mixture of glycerol and methanol in the presence of sulfuric acid using microwave energy. We investigated the effects of lique-faction conditions, including glycerol/methanol ratio, liq-uefaction temperature, and reaction time on the conversion yield. The optimal liquefaction conditions were under the temperature of 120 °C, the reaction time of 7 min, the glycerol–methanol–bamboo ratio of 8/0/2 (W/W), and the microwave power of 300 W. Maximum conversion yield was 96.7%. The liquid products were separated into two contents (water soluble part and precipitate part) by addi-tion of a sufficient amount of water. By Fourier transform infrared (FT-IR), the water soluble content mainly con-tained glycerol and its derivate and carbohydrate degra-dation products, and the precipitate content was mainly lignin derivatives.

  3. 某涉氨制冷企业液氨储罐泄漏事故的后果分析%Analysis of An Ammonia Refrigeration Enterprise Involved in Liquid Ammonia Storage Tank Leakage Accident Consequence

    Institute of Scientific and Technical Information of China (English)

    周峰

    2014-01-01

    以某涉氨制冷企业液氨储罐为例,选用蒸气云爆炸、沸腾液体扩展蒸气爆炸和中毒模型对液氨储罐泄漏事故进行后果分析,定量地得出各类伤害半径,为企业制定应急救援预案和政府进行安全监管提供科学依据。%Taking the liquid ammonia tank of a refrigeration enterprise as example, the consequences of liquid ammonia storage tank leakage accident were analyzed using vapor cloud explosion model, boiling liq-uid expanding vapor explosion model and poisoning model. The various damage radiuses were calculated. It provided the scientific basis for enterprises to formulate emergency rescue plans and for safety supervision of government.

  4. Accurate level set method for simulations of liquid atomization☆

    Institute of Scientific and Technical Information of China (English)

    Changxiao Shao; Kun Luo; Jianshan Yang; Song Chen; Jianren Fan

    2015-01-01

    Computational fluid dynamics is an efficient numerical approach for spray atomization study, but it is chal enging to accurately capture the gas–liquid interface. In this work, an accurate conservative level set method is intro-duced to accurately track the gas–liquid interfaces in liquid atomization. To validate the capability of this method, binary drop collision and drop impacting on liquid film are investigated. The results are in good agreement with experiment observations. In addition, primary atomization (swirling sheet atomization) is studied using this method. To the swirling sheet atomization, it is found that Rayleigh–Taylor instability in the azimuthal direction causes the primary breakup of liquid sheet and complex vortex structures are clustered around the rim of the liq-uid sheet. The effects of central gas velocity and liquid–gas density ratio on atomization are also investigated. This work lays a solid foundation for further studying the mechanism of spray atomization.

  5. Infrared spectrophotometric analysis of acidified aqueous sodium oleate solutions

    Science.gov (United States)

    Drzymala, Jan; Kielkowska, M. M.

    Infrared spectroscopy was applied to the analysis of 10 -3 M aqueous sodium oleate solutions titrated with 0.2 M HCl. From characteristic absorption bands of sodium oleate at 1560 cm -1 and oleic acid at 1710 cm -1 the degree of oleate ion neutralization in the titrated system at varying pH was calculated.It was found that the pH-metric titration curve of oleate ions differs considerably from the theoretical curve calculated for the reaction Ol -aq + H + = HOl liq, taking the solubility product of oleic acid equal to 12.5. Most likely aggregates of oleate ons (micelles) are formed during titration and account for the deviation of the titration curves from theory.

  6. Centrifugal experimental study of suction bucket foundations under dynamic loading

    Institute of Scientific and Technical Information of China (English)

    Xiaobing Lu; Yongren Wu; Bintian Jiao; Shuyun Wang

    2007-01-01

    Centrifugal experiments were carded out to investigate the responses of suction bucket foundations under horizontal and vertical dynamic loading. It is shown that when the loading amplitude is over a critical value, the sand at the upper part around the bucket is softened or even liq-uefied. The excess pore pressure decreases from the upper part to the lower part of the sand layer in the vertical direc-tion and decreases radially from the bucket's side wall in the horizontal direction. Large settlements of the bucket and the sand layer around the bucket are induced by dynamic load-ing. The dynamic responses of the bucket with smaller height (the same diameter) are heavier.

  7. La Génesis desde el Babel de Emociones

    OpenAIRE

    Sagasti Aurrecoechea, Joseba Josu

    2012-01-01

    Duración (en horas): De 21 a 30 horas. Destinatario: Estudiante y Docente Dña. Sonia Losada, empadronada en Getxo desde el día 20 de Septiembre de 1990, acudió en el mes de Julio de 2010 al despacho de abogados S&J a solicitar asesoramiento sobre diversos hechos y problemas que le habían surgido. De una parte, había problemas de naturaleza personal, pero con implicaciones económicas, ya que, quien había sido su pareja de hecho durante diez años, le exigía en el año 2009 la disolución y liq...

  8. Granuloma paracoccidióidico cerebral: a propósito de um caso operado

    Directory of Open Access Journals (Sweden)

    Octavio Lemmi

    1960-03-01

    Full Text Available Os autores fazem rápida revisão da literatura, referindo-se aos casos de blastomicose sulamericana do sistema nervoso comprovados seja pelo exame bacteriológico do liqüido cefalorraqueano, seja pelo exame bacteriológico ou histopatológico de material cirúrgico ou de necropsia. Apresentam em seguida um caso operado de tumor cerebral granulomatoso, de localização frontal, produzido pelo Paracoccidioides brasiliensis. Houve suspeita clinica da etiologia através da anamnese e confirmação pelos exames bacteriológico e histopatológico do material cirúrgico.

  9. Investigation of many-body forces in krypton and xenon

    Science.gov (United States)

    Salacuse, J. J.; Egelstaff, P. A.

    1988-10-01

    The simplicity of the state dependence at relatively high temperatures of the many-body potential contribution to the pressure and energy has been pointed out previously [J. Ram and P. A. Egelstaff, J. Phys. Chem. Liq. 14, 29 (1984); A. Teitsima and P. A. Egelstaff, Phys. Rev. A 21, 367 (1980)]. In this paper, we investigate how far these many-body potential terms may be represented by simple models in the case of krypton on the 423-, 273-, 190-, and 150-K isotherms, and xenon on the 170-, 210-, and 270-K isotherms. At the higher temperatures the best agreement is found for the mean-field type of theory, and some consequences are pointed out. On the lower isotherms a state point is found where the many-body energy vanishes, and large departures from mean-field behavior are observed. This is attributed to the influence of short-ranged many-body forces.

  10. 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.

  11. Variación de la mineralogía del residuo y fraccionación de los elementos traza durante la fusión parcial incongruente

    Directory of Open Access Journals (Sweden)

    López Ruiz, J.

    1989-04-01

    Full Text Available Some minerals of the crust and mantle melt incongruently. During incongruent melting, the trace element Cractionation can't be modelled by the mathematical expressions derived by Shaw (1970. In this case, the equations of Hanson (1978 should be used, when the mineralogy of residual solid is known, or the expressions obtained by Hertogen and Gijbels (1976, when the composition of the initial solid is known. In this paper, the mathematical expressions presented by these last authors to treat incongruent melting processes, are extended to a more general case when the breakdown of one phase (α takes the form α + β + γ = δ + ε + Liq.Algunas fases minerales de las que constituyen las rocas de la corteza y del manto superior funden incongruentemente. En estas condiciones; la fraccionación de los elementos traza no puede ser modelada mediante las clásicas ecuaciones de Shaw (1970; sino que tienen que utilizarse las ecuaciones de Hanson (1978 o las de Hertogen y Gijbels (1976. La elección de unas u otras ecuaciones; dependerá de que se desee calcular el valor de la concentración en el líquido para un momento dado de la fusión o a lo largo del proceso. En este trabajo se modifican las ecuaciones propuestas por Hertogen y Gijbels (1976; extendiéndolas al caso más general en el que la reacción y fusión incongruente de una fase (α tiene lugar según la reacción α + β + γ = δ + ε + Liq.

  12. Evidences of the existence of SiTe2 crystalline phase and a proposed new Si-Te phase diagram

    Science.gov (United States)

    Mishra, R.; Mishra, P. K.; Phapale, S.; Babu, P. D.; Sastry, P. U.; Ravikumar, G.; Yadav, A. K.

    2016-05-01

    The existence of two distinct crystalline phases viz., Si2Te3 and SiTe2, in the Si-Te system is established from differential thermal analysis (DTA) studies. Thermo-gravimetric (TG) data on SiTe2 indicate that the compound decomposes to Si in multiple steps via intermediate Si2Te3 phase. X-ray diffraction (XRD) reveals that SiTe2 crystallizes in P 3 ̅m1 space group with CdI2 trigonal structure, whereas Si2Te3 crystallizes in trigonal structure with space group P 3 ̅1c with varying occupation of octahedral voids. Single Si atoms fill only 1/2 of the octahedral voids in SiTe2 structure whereas in Si2Te3, Si atoms are arranged in pairs occupying 2/3 of the octahedral voids in alternating planes along c-axis. Further, X-ray absorption near edge structure (XANES) and X-ray photoelectron spectroscopy (XPS) confirm the distinctness of the chemical environment in the two crystalline structures confirming the uniqueness of both the phases. DTA results on the two compounds indicate the presence of one crystallographic phase-transition in each of the compound with transition temperatures at 441 °C for Si2Te3 and 392 °C for SiTe2. At the same time both Si2Te3 and SiTe2 undergo peritectic decomposition at 683 °C and 432 °C forming [Si(s)+Te(liq)] and [α-Si2Te3(s)+Te(liq)], respectively. The system revealed eutectic reaction between β-SiTe2 and Te at 398 °C [L=Te+SiTe2]. Consequently, the phase diagram in the Si-Te system has been delineated.

  13. Which way will the circulation shift in a changing climate? Possible nonlinearity of extratropical cloud feedbacks

    Science.gov (United States)

    Tandon, Neil F.; Cane, Mark A.

    2017-06-01

    In a suite of idealized experiments with the Community Atmospheric Model version 3 coupled to a slab ocean, we show that the atmospheric circulation response to CO2 increase is sensitive to extratropical cloud feedback that is potentially nonlinear. Doubling CO2 produces a poleward shift of the Southern Hemisphere (SH) midlatitude jet that is driven primarily by cloud shortwave feedback and modulated by ice albedo feedback, in agreement with earlier studies. More surprisingly, for CO2 increases smaller than 25 %, the SH jet shifts equatorward. Nonlinearities are also apparent in the Northern Hemisphere, but with less zonal symmetry. Baroclinic instability theory and climate feedback analysis suggest that as the CO2 forcing amplitude is reduced, there is a transition from a regime in which cloud and circulation changes are largely decoupled to a regime in which they are highly coupled. In the dynamically coupled regime, there is an apparent cancellation between cloud feedback due to warming and cloud feedback due to the shifting jet, and this allows the ice albedo feedback to dominate in the high latitudes. The extent to which dynamical coupling effects exceed thermodynamic forcing effects is strongly influenced by cloud microphysics: an alternate model configuration with slightly increased cloud liquid (LIQ) produces poleward jet shifts regardless of the amplitude of CO2 forcing. Altering the cloud microphysics also produces substantial spread in the circulation response to CO2 doubling: the LIQ configuration produces a poleward SH jet shift approximately twice that produced under the default configuration. Analysis of large ensembles of the Canadian Earth System Model version 2 demonstrates that nonlinear, cloud-coupled jet shifts are also possible in comprehensive models. We still expect a poleward trend in SH jet latitude for timescales on which CO2 increases by more than 25 %. But on shorter timescales, our results give good reason to expect significant

  14. 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.

  15. Importância do exame do liquor de controle em meningite bacteriana como critério de alta Importance of cerebrospinal fluid control tests in bacterial meningitis cases as a discharge criterion

    Directory of Open Access Journals (Sweden)

    Diogo Buarque Cordeiro Cabral

    2008-04-01

    Full Text Available Há controvérsias sobre indicação do exame do liquor de controle em pacientes recuperados clinicamente de meningite bacteriana como critério de cura. Alguns autores defendem alta hospitalar após normalização clínica e liqüórica, outros que a análise do liquor não se justifica em todos os pacientes. Esta série de casos com comparação de grupos investiga alterações no exame liqüórico de controle e avalia a importância do exame na decisão da alta. De 297 pacientes estudados, em 89,9%, o liquor de controle não mudou a intenção de alta (liquor resolutivo, já em 10,1% a alta foi suspensa (liquor não-resolutivo. Destes, o esquema antibiótico foi trocado em 30%. Entre as variáveis que pudessem ser preditivas de liquor não-resolutivo, à admissão, proteinorraquia maior que 100mg/dL (p=0,04 e glicorraquia menor ou igual a 20mg/dL (p=0,03 associaram-se a chance 2,5 vezes maior, podendo ser úteis como critérios para indicar exame do liquor como controle de cura para alta.There is controversy regarding indications for cerebrospinal fluid control tests on patients who have clinically recovered from bacterial meningitis, as a cure criterion. Some authors advocate discharge after confirmation of clinical and cerebrospinal fluid normalization, while others maintain that cerebrospinal fluid analysis is not justified in all cases. This case series with group comparisons investigated changes seen in cerebrospinal fluid control tests and evaluated the importance of this for the discharge decision. Out of 297 patients studied, the cerebrospinal fluid control test did not change the discharge intention in 89.9% of the cases (healed cerebrospinal fluid, while in 10.1%, the discharge was suspended (non-healed cerebrospinal fluid. Of these, the antibiotic scheme was changed in 30%. Among the variables that might predict the presence of non-healed cerebrospinal fluid on admission, cerebrospinal fluid protein levels higher than 100mg/dl (p

  16. Petrology of the zoned calcalkaline magma chamber of Mount Mazama, Crater Lake, Oregon

    Science.gov (United States)

    Druitt, T.H.; Bacon, C.R.

    1989-01-01

    Evolution of the magma chamber at Mount Mazama involved repeated recharge by two types of andesite (high-Sr and low-Sr), crystal fractionation, crystal accumulation, assimilation, and magma mixing (Bacon and Druitt 1988). This paper addresses the modal compositions, textures, mineral chemistry and magmatic temperatures of (i) products of the 6845??50 BP climactic eruption, (ii) blocks of partially fused granitoid wallrock found in the ejecta, and (iii) preclimactic rhyodacitic lavas leaked from the chamber in late Pleistocene and early Holocene time. Immediately prior to the climactic eruption the chamber contained ??? 40 km3 of rhyodacite (10 vol% plag + opx + aug + hb + mt + ilm, ???880?? C) overlying high-Sr andesite and cumulus-crystal mush (28-51 vol% plag + hb ?? opx ?? aug + mt ?? ilm, 880?? to ???950?? C), which in turn overlay low-Sr crystal mush (50-66 vol% plag + opx + aug ?? hb ?? ol + mt + ilm, 890?? to ???950??? C). Despite the well known compositional gap in the ejecta, no thermal discontinuity existed in the chamber. Pre-eruptive water contents of pore liquids in most high-Sr and low-Sr mushes were 4-6 wt%, but on average the high-Sr mushes were slightly richer in water. Although parental magmas of the crystal mushes were andesitic, xenocrysts of bytownite and Ni-rich magnesian olivine in some scoriae record the one-time injection of basalt into the chamber. Textures in ol-bearing scoriae preserve evidence for the reactions ol + liq = opx and ol + aug + liq(+ plag?) = hb, which occurred in andesitic liquids at Mount Mazama. Strontium abundances in plagioclase phenocrysts constrain the petrogenesis of preclimactic and climactic rhyodacites. Phenocryst cores derived from high-Sr and low-Sr magmas have different Sr contents which can be resolved by microprobe. Partition coefficients for plagioclase in andesitic to rhyolitic glasses range from 2 to 7, and increase as glass %SiO2 increases. Evolved Pleistocene rhyodacites (???30-25,000 BP) and

  17. Aircraft-Measured Indirect Cloud Effects from Biomass Burning Smoke in the Arctic and Subarctic

    Science.gov (United States)

    Zamora, L. M.; Kahn, R. A.; Cubison, M. J.; Diskin, G. S.; Jimenez, J. L.; Kondo, Y.; McFarquhar, G. M.; Nenes, A.; Thornhill, K. L.; Wisthaler, A.; Zelenyuk, A.; Ziemba, L. D.

    2016-01-01

    The incidence of wildfires in the Arctic and subarctic is increasing; in boreal North America, for example, the burned area is expected to increase by 200-300% over the next 50-100 years, which previous studies suggest could have a large effect on cloud microphysics, lifetime, albedo, and precipitation. However, the interactions between smoke particles and clouds remain poorly quantified due to confounding meteorological influences and remote sensing limitations. Here, we use data from several aircraft campaigns in the Arctic and subarctic to explore cloud microphysics in liquid-phase clouds influenced by biomass burning. Median cloud droplet radii in smoky clouds were approx. 40- 60% smaller than in background clouds. Based on the relationship between cloud droplet number (N(liq)/ and various biomass burning tracers (BBt/ across the multi-campaign data set, we calculated the magnitude of subarctic and Arctic smoke aerosol-cloud interactions (ACIs, where ACI = (1/3) x dln(N(liq))/dln(BBt)) to be approx. 0.16 out of a maximum possible value of 0.33 that would be obtained if all aerosols were to nucleate cloud droplets. Interestingly, in a separate subarctic case study with low liquid water content (0.02 gm/cu m and very high aerosol concentrations (2000- 3000/ cu cm in the most polluted clouds, the estimated ACI value was only 0.05. In this case, competition for water vapor by the high concentration of cloud condensation nuclei (CCN) strongly limited the formation of droplets and reduced the cloud albedo effect, which highlights the importance of cloud feedbacks across scales. Using our calculated ACI values, we estimate that the smoke-driven cloud albedo effect may decrease local summertime short-wave radiative flux by between 2 and 4 W/sq m or more under some low and homogeneous cloud cover conditions in the subarctic, although the changes should be smaller in high surface albedo regions of the Arctic.We lastly explore evidence suggesting that numerous northern

  18. Aspectos electrencefalográficos da cisticercose encefálica

    Directory of Open Access Journals (Sweden)

    Paulino W. Longo

    1959-12-01

    Full Text Available Com a finalidade de conhecer os elementos úteis que o EEG poderia trazer para o diagnóstico da forma clínica da cisticercose encefálica, foram reunidos 118 casos desta afecção, com diagnóstico confirmado pela verificação cirúrgica, pelo exame do liqüido cefalorraqueano (presença de leucocitose, eosinofilia e reação de desvio de complemento positiva ou pela verificação radiológica de cisticercos calcificados. Os resultados electrencefalográficos foram analisados particularmente visando os dados que pudessem informar sôbre existência de processo difuso envolvendo o parênquima nervoso dos hemisférios cerebrais, ou a existência de focos epileptógenos ativos, ou ainda, sinais de sofrimento do parênquima em conseqüência da hipertensão intracraniana. Êstes resultados foram estudados separadamente no grupo dos casos com síndrome clínica da convexidade cerebral, com a presença ou não de síndrome convulsiva e no grupo dos casos com síndrome clínica de base e fossa posterior. Além disso os resultados electrencefalográficos foram estudados comparativamente no grupo de pacientes com cisticercos não calcificados, assim como também foram estudados, comparativamente, em grupos de pacientes com síndrome inflamatória verificável pelo exame do líqüido cefalorraqueano e no de pacientes com o liqüido cefalorraqueano normal. Êstes resultados, projetados nos quadros 1 e 2, permitiram conclusões de algum interêsse clínico, significativas para a importância do exame electrencefalográfico na avaliação dos processos patológicos encefálicos decorrentes da neurocisticercose.

  19. 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

  20. Magma storage before large and small explosive eruption at Grímsvötn volcano, Iceland, constrained by thermobarometry and volatiles in melt inclusions

    Science.gov (United States)

    Haddadi, Baptiste; Sigmarsson, Olgeir; Larsen, Gudrun

    2017-04-01

    Basaltic eruptions at Grímsvötn occur every decade on average. These are normally phreatomagmatic of a low intensity whereas occasionally larger eruptions with an initial plinian phase take place. The last eruption in May 2011 reached into the stratosphere with heavy ash fall over south Iceland. What causes the difference in eruption intensity at Grímsvötn is not understood. In order to discuss this difference, the crystallization conditions of the eruptive magma were determined through thermobarometry and volatile concentration measured on melt inclusion (MI) and groundmass glasses. Tephra of the two largest historical eruptions (2011 and 1873) and two small eruptions (2004 and 1823) were investigated. Pressure and temperature estimates of crystallization are obtained through equilibrium clinopyroxene-glass (cpx-liq) pairs, where both adjacent groundmass glass and that of melt inclusions (MI) were measured. Most cpx-liq equilibria give pressure of 4 ±1 kbar corresponding to approximately 15 km depth. The cpx crystallization occurred over a considerable temperature range, 1065-1175 °C that correlates with the estimated pressure in products of the 19th century eruptions. Sulfur and chlorine concentrations are highest in MI of the larger eruptions (1974-1789 ppm and 339-266 ppm, respectively) together with lowest groundmass glass concentrations (908-766 ppm and 208-180 ppm, respectively). Quenching with glacial water explains higher groundmass values for the smaller phreatomagmatic eruptions. The differences in volatile concentrations between MI and groundmass glass (S) and the average sulfur concentration in the degassed groundmass correlate with known eruptive volume for the 21st century eruptions and that of the Laki eruption. This suggests water/magma ratio control of S degassing efficiency and allows crude estimates of unknown volumes for older eruptions. The higher volatile concentrations of MI in the larger eruptions are likely to reflect recharge of

  1. Liquidus temperatures of komatiites and the effect of cooling rate on element partitioning between olivine and komatiitic melt

    Science.gov (United States)

    Sossi, Paolo A.; O'Neill, Hugh St. C.

    2016-05-01

    Archean komatiites are the hottest magmas preserved on Earth and are thus unique probes of its thermal evolution. Estimating their eruption temperatures remains problematic, however, because the uppermost (A1, A2) zones of komatiite flows contain randomly oriented spinifex-textured olivines, indicative of rapid cooling and growth. Fe-Mg partitioning between olivine and assumed komatiitic liquid typically shows departures from equilibrium, extending towards higher K_{{D}}^{{{{Fe}}^{2 + } - {{Mg}}}}. If these higher values are a disequilibrium effect, using them to calculate parental magma composition would lead to errors in estimated liquidus temperatures. In order to investigate this possibility, we have performed experiments on two komatiite compositions, the classic Barberton Aluminium Undepleted Komatiite (AUK) sample 49J (32.2 % MgO) and Munro AUK sample 422/95 (23 % MgO). Isothermal experiments to constrain phase equilibria on 49J at atmospheric pressure, between 1360 and 1600 °C at 1.7 log units below and 1.1 above the fayalite-magnetite-quartz (FMQ) buffer reveal a liquidus temperature ( T liq) of 1616 °C, 40 °C lower than a previous estimate. The K_{{D}}^{{Σ {{Fe}}{-}{{Mg}}}} ranges between 0.320 and 0.295 at FMQ - 1.7, with a slight negative dependence on temperature. To replicate the conditions that prevailed during the quenching of komatiites in their upper chill zones, experiments with a constant cooling rate at FMQ - 1.7 were performed on 422/95 ( T liq = 1450 °C) at 0.5, 1.5, 2.5, 6.5 and 16 °C/min. Olivine morphology changes from euhedral to tabular at low cooling rates, hopper at intermediate, and skeletal and chain structures at high rates. Concurrently, the K_{{D}}^{{Σ {{Fe}}{-}{{Mg}}}} increases monotonically from an equilibrium value of 0.305 to 0.376 at 16 °C/min, reflecting the inability of unwanted cations to diffuse away from the growing olivine. The high K_{{D}}^{{Σ {{Fe}}{-}{{Mg}}}} between olivine and komatiitic liquid caused by

  2. The single-electrode Peltier heats of Li-Al alloy electrodes in LiCl-KCl eutectic system

    Energy Technology Data Exchange (ETDEWEB)

    Amezawa, Koji; Ito, Yasuhiko; Tomii, Yoichi (Kyoto Univ. (Japan))

    1994-11-01

    This paper presents the single-electrode Peltier heat of cathodic (or anodic) reaction of Li-Al alloy electrode in a coexisting phase state, or an intermetallic compound phase state estimated by thermoelectric-power measurement. The thermoelectric-power measurements of Li-Al alloys in various coexisting phase states were carried out with both potentiometric and potential-sweep methods in the LiCl-KCl eutectic system between 673 and 843 K. The values of the thermoelectric power of Li-Al alloys calculated by using thermodynamic literature data were in good agreement with those obtained by experiment. The single-electrode Peltier heat changes drastically with change of its phase state, and it was found that the formation reactions of [beta] (Li[sub 0.5]Al[sub 0.5]) and [gamma] (Li[sub 0.6]Al[sub 0.4]) phases are exothermic, and those of liquid phase from [beta] and [gamma] phase are endothermic. The single-electrode Peltier heat for the cathodic formation reaction of Li-Al alloy in intermetallic compound [gamma] phase is estimated to be exothermic by using the measured values of thermoelectric powers of Li-Al alloys in ([beta] + [gamma]) and ([gamma] + liq.) regions.

  3. 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.

  4. From ab initio quantum chemistry to molecular dynamics: The delicate case of hydrogen bonding in ammonia

    CERN Document Server

    Boese, A D; Martin, J M L; Marx, D; Chandra, Amalendu; Martin, Jan M.L.; Marx, Dominik

    2003-01-01

    The ammonia dimer (NH3)2 has been investigated using high--level ab initio quantum chemistry methods and density functional theory (DFT). The structure and energetics of important isomers is obtained to unprecedented accuracy without resorting to experiment. The global minimum of eclipsed C_s symmetry is characterized by a significantly bent hydrogen bond which deviates from linearity by about 20 degrees. In addition, the so-called cyclic C_{2h} structure is extremely close in energy on an overall flat potential energy surface. It is demonstrated that none of the currently available (GGA, meta--GGA, and hybrid) density functionals satisfactorily describe the structure and relative energies of this nonlinear hydrogen bond. We present a novel density functional, HCTH/407+, designed to describe this sort of hydrogen bond quantitatively on the level of the dimer, contrary to e.g. the widely used BLYP functional. This improved functional is employed in Car-Parrinello ab initio molecular dynamics simulations of liq...

  5. 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.)

  6. Thermodynamic description of Sn-Y and Mg-Sn-Y systems

    Institute of Scientific and Technical Information of China (English)

    吕东显; 郭翠萍; 李长荣; 杜振民

    2014-01-01

    The thermodynamic optimization of the Sn-Y and Mg-Sn-Y systems was critically carried out by means of the CALPHAD (CALculation of PHAse Diagram) technique. In the Sn-Y system, the solution phases (liquid, bcc, bct and hcp) were described by the substitutional solution model. The compound Sn3Y5, which has a homogeneity range, was treated as the formula (Sn, Y)3(Sn, Y)2Y3 by a three-sublattice model in accordance with the site occupancies. In the Mg-Sn-Y system, the liquid phase was treated as the for-mula (Mg, Sn, Y, Mg2Sn) using an associated solution model, and bcc, bct and hcp were treated as the formula (Mg, Sn, Y). The compound Sn3Y5 was treated as the formula (Sn, Y, Mg)3(Sn, Y, Mg)2Y3. The ternary compound MgSnY was treated as stoichiomet-ric compound. A set of self-consistent thermodynamic parameters of the Mg-Sn-Y system was obtained. The projection of the liq-uidus surfaces and the reaction scheme of the Mg-Sn-Y system were predicted.

  7. 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.

  8. Thermodynamic design of a cascade refrigeration system of liquefied natural gas by applying mixed integer non-linear programming

    Institute of Scientific and Technical Information of China (English)

    Meysam Kamalinejad; Majid Amidpour; S.M. Mousavi Naeynian

    2015-01-01

    Liquefied natural gas (LNG) is the most economical way of transporting natural gas (NG) over long distances. Liq-uefaction of NG using vapor compression refrigeration system requires high operating and capital cost. Due to lack of systematic design methods for multistage refrigeration cycles, conventional approaches to determine op-timal cycle are largely trial-and-error. In this paper a novel mixed integer non-linear programming (MINLP) model is introduced to select optimal synthesis of refrigeration systems to reduce both operating and capital costs of an LNG plant. Better conceptual understanding of design improvement is illustrated on composite curve (CC) and exergetic grand composite curve (EGCC) of pinch analysis diagrams. In this method a superstruc-ture representation of complex refrigeration system is developed to select and optimize key decision variables in refrigeration cycles (i.e. partition temperature, compression configuration, refrigeration features, refrigerant flow rate and economic trade-off). Based on this method a program (LNG-Pro) is developed which integrates VBA, Refprop and Excel MINLP Solver to automate the methodology. Design procedure is applied on a sample LNG plant to illustrate advantages of using this method which shows a 3.3% reduction in total shaft work consumption.

  9. 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.

  10. Studies of Commercial Banks' Liquidity Creation%商业银行流动性创造研究

    Institute of Scientific and Technical Information of China (English)

    刘志洋; 宋玉颖

    2015-01-01

    The amount of China's on-listed bank liquidity creation has increased a lot from 2006 to 2013. The more liq-uidity creates, the more liquidity risk that banks face. Empirical studies on China's on-listed bank shows that higher capital ratio means lower liquidity creation, and this will lower the liquidity risk that banks face, in other words, financial fragility-crowding out effect dominance China's on-listed bank. The higher credit risk, the more liquidity creates, and banks will face more liquidity risk.%2006—2013年中国上市商业银行流动性创造总量大幅增长。流动性创造越多,商业银行流动性风险会越大。运用中国上市商业银行数据实证分析表明,中国上市商业银行资本充足率越高,银行流动性创造越低,越会降低银行流动性风险,即金融脆弱挤出效应占据主导地位。中国上市商业银行信用风险越高,银行流动性创造量越多,银行流动性风险越大。

  11. Fabrication and electroluminescence properties of white organic light-emitting diode with a new yellow fluorescent dopant.

    Science.gov (United States)

    Lee, Sung Nam; Lee, Seok Jae; Kim, Young Kwan; Shin, Dong Myung

    2014-08-01

    A new yellow fluorescent material, (2Z)-3-[4,4"-bis(dimethylamino)-1,1':4',1"-terphenyl-2'-yl]-2-phenylacrylonitrile (BDAT-P), have been synthesized for use in organic light-emitting diodes. Opto-electronic properties of device with the structure of ITO (180 nm)/NPB (50 nm)/MADN:PFVtPh (SYB-41) 8% (17 nm)/CBP (5 nm)/CBP:Ir(pq)2acac 8% (3 nm)/CBP (5 nm)/MADN:BDAT-P 8% (3 nm)/CBP (5 nm)/MADN:SYB-41 8% (17 nm)/TPBi (40 nm)/Liq (2 nm)/Al (100 nm) was measured and revealed that BDAT-P was sufficiently applicable as a dopant of one of emitting layers in white light-emitting diodes. Maximum luminance of device was measured to be 26,950 cd/m2. Maximum luminous and quantum efficiency were observed to be 14.22 cd/A and 6.58%, respectively. The device emitted warm white light corresponding to Commission Internationale de l'Eclairage (CIExy) coordinates of (0.372, 0.424) at 11 V, (0.375,0.417) at 12 V, (0.372,0.409) at 13 V, (0.366, 0.401) at 14 V, and (0.360, 0.393) at 15 V, respectively.

  12. 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.

  13. Field-lysimeter and Column Studies As Complementary Survey Tools For Monitored Natural Attenuation (mna)

    Science.gov (United States)

    Totsche, K. U.; Hensel, D.; Jann, S.; Jaesche, P.; Kögel-Knabner, I.; Scheibke, R.

    The contamination of the unsaturated soil zone with organic pollutants (PAH, BTEX, PCB, Phenols, etc.) and pollutant mixtures, e.g. light/dense non-aqueous phase liq- uids (L/D-NAPLs), represents a specific challenge for sanitation and remediation of contaminated sites. Monitored natural attenuation as an alternative option for remedi- ation of such sites requires (1) the proof of an effective pollutant reduction potential and (2) the proof that a further spreading of the contaminants and their potentially toxic metabolites is minimized to an acceptable minimum concentration level. These demands apply equally likely to contaminated soil and groundwater environments. However, a major problem arises when the task is to monitor the release and transport of contaminants within the unsaturated soil zone over a longer period (> 10 years) of time at an expenditure as small as possible. The aim of our presentation is to employ and test a survey technique to monitor pollutant release and redistribution within the unsaturated soil zone in the context of MNA. The proposed technique is based on the combination of laboratory-column and field-lysimeter studies. The first is used to ac- quire knowledge on the governing processes, the latter is used to monitor release and transport of the contaminants.

  14. 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

    2016-12-23

    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.

  15. 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...

  16. A Clinopyroxene-Plagioclase Geobarometer for A-type Silicic Volcanic Rocks

    Science.gov (United States)

    Wolff, J.; Iveson, A. A.; Davis, K.; Johnson, T. A.; Gahagan, S.; Ellis, B. S.

    2015-12-01

    Constraining the crustal storage depths of magmas is important in understanding volcanism. The reaction: anorthite (pl) = Ca-Tschermak's (cpx) + silica (Q or liq) has a large volume change and hence offers potential as a geobarometer, but has not been extensively exploited as such. One of the chief barriers to its wide application is consistent estimation of melt silica activity for assemblages that lack quartz. We have skirted this problem by confining attention to metaluminous silicic compositions (SiO2 > 60% by weight), for which silica activity during crystallization is presumed to be close to 1, and calibrated the barometer for the range 0 - 2 GPa using the LEPR database and additional experiments from the literature. Additional improvement is obtained by excluding hydrous phase-bearing assemblages. Despite the analytical uncertainties present in older experimental investigations, with knowledge of temperature, and clinopyroxene, plagioclase and host melt compositions, pressures for amphibole- and biotite-free dacites and rhyolites can be estimated to ±0.17 GPa (1 sigma). The limitations of the barometer render it most applicable to intraplate, A-type rhyolites. Application to one such system, the Snake River Plain rhyolites, indicate that both melt-hosted phenocrysts and clinopyroxene-plagioclase aggregate grains found in these rhyolites formed at low pressures, <0.5 GPa. This is consistent with isotopic evidence for a shallow crustal origin for Snake River Plain rhyolites.

  17. Synthesis, structure, and properties of Li2In2MQ6 (M = Si, Ge; Q = S, Se): a new series of IR nonlinear optical materials.

    Science.gov (United States)

    Yin, Wenlong; Feng, Kai; Hao, Wenyu; Yao, Jiyong; Wu, Yicheng

    2012-05-21

    The four isostructural compounds Li(2)In(2)MQ(6) (M = Si, Ge; Q = S, Se) have been synthesized for the first time. They crystallize in the noncentrosymmetric monoclinic space group Cc with the three-dimensional framework composed of corner-sharing LiQ(4), InQ(4), and MQ(4) tetrahedra. The second-harmonic-generation signal intensities of the two sulfides and two selenides were close to those of AgGaS(2) and AgGaSe(2), respectively, when probed with a laser with 2090 nm as the fundamental wavelength. They possess large band gaps of 3.61(2) eV for Li(2)In(2)SiS(6), 3.45(2) eV for Li(2)In(2)GeS(6), 2.54(2) eV for Li(2)In(2)SiSe(6), and 2.30(2) eV for Li(2)In(2)GeSe(6), respectively. Moreover, these four compounds all melt congruently at relatively low temperatures, which makes it feasible to grow bulk crystals needed for practical application by the Bridgman-Stockbarger method.

  18. Ground-based Remote Sensing of Cloud Liquid Water Path

    Science.gov (United States)

    Crewell, S.; Loehnert, U.

    Within the BALTEX Cloud LIquid WAter NETwork (CLIWA-NET) measurements of cloud parameters were performed to improve/evaluate cloud parameterizations in numerical weather prediction and climate models. The key variable is the cloud liq- uid water path (LWP) which is measured by passive microwave radiometry from the ground during three two-month CLIWA-NET observational periods. Additionally to the high temporal resolution time series from the ground, LWP fields are derived from satellite measurements. During the first two campaigns a continental scale network consisting of 12 stations was established. Most stations included further cloud sen- sitive instruments like infrared radiometer and lidar ceilometer. The third campaign started with a two-week long microwave intercomparison campaign (MICAM) in Cabauw, The Netherlands, and proceeded with a regional network within a 100 by 100 km area. The presentation will focus on the accuracy of LWP derived from the ground by in- vestigating the accuracy of the microwave brightness temperature measurement and examining the LWP retrieval uncertainty. Up to now microwave radiometer are no standard instruments and the seven radiometer involved in MICAM differ in frequen- cies, bandwidths, angular resolution, integration time etc. The influence of this instru- ment specifications on the LWP retrieval will be discussed.

  19. Evaluation of a Novel Rapid Test System for the Detection of Specific IgE to Hymenoptera Venoms

    Directory of Open Access Journals (Sweden)

    Nikolai Pfender

    2012-01-01

    Full Text Available Background. The Allergy Lateral Flow Assay (ALFA is a novel rapid assay for the detection of sIgE to allergens. The objective of this study is the evaluation of ALFA for the detection of sIgE to bee venom (BV and wasp venom (WV in insect venom allergic patients. Methods. Specific IgE to BV and WV was analyzed by ALFA, ALLERG-O-LIQ, and ImmunoCAP in 80 insect venom allergic patients and 60 control sera. Sensitivity and specificity of ALFA and correlation of ALFA and ImmunoCAP results were calculated. Results. The sensitivity/specificity of ALFA to the diagnosis was 100%/83% for BV and 82%/97% for WV. For insect venom allergic patients, the Spearman correlation coefficient for ALFA versus ImmunoCAP was 0.79 for BV and 0.80 for WV. However, significant differences in the negative control groups were observed. Conclusion. ALFA represents a simple, robust, and reliable tool for the rapid detection of sIgE to insect venoms.

  20. 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.