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Crystal Formation (crystal + formation)
Selected AbstractsCharacterization of the Triacylglycerol Crystal Formation in Adipose Tissue During a Vehicle CollisionJOURNAL OF FORENSIC SCIENCES, Issue 4 2007Barbara H. Stuart Ph.D. Abstract:, The unusual appearance of crystalline fat structures was observed during the postmortem examination of a motor vehicle accident victim. The crystal structures were characterized using Fourier transform infrared spectroscopy and x-ray diffractometry. The structures were found to be made of triacylglycerols, a dominant lipid structure found in human adipose tissue, capable of forming various polymorphic structures. The morphology of the crystalline material was found using both techniques to be predominantly the ,, form of triacylglycerols. The accelerated growth of such triacylglycerol morphology has been observed as a result of shear stresses in other studies involving edible fats. As a result of the findings of this study, it is proposed that increased shear forces may be responsible for the formation of the unusual fat structure found in the victim. An understanding of the effect of forces on the structure of body fat in high-impact collisions can potentially assist in verifying a high-velocity impact. [source] Motif Reconstruction in Clusters and Layers: Benchmarks for the Kawska,Zahn Approach to Model Crystal FormationCHEMPHYSCHEM, Issue 4 2010Theodor Milek Abstract A recently developed atomistic simulation scheme for investigating ion aggregation from solution is transferred to the morphogenesis of metal clusters grown from the vapor and layers deposited on a substrate surface. Both systems are chosen as benchmark models for intense motif reorganization during aggregate/layer growth. The applied simulation method does not necessarily involve global energy minimization after each growth event, but instead describes crystal growth as a series of structurally related configurations which may also include local energy minima. Apart from the particularly favorable high-symmetry configurations known from experiments and global energy minimization, we also demonstrate the investigation of transient structures. In the spirit of Ostwald's step rule, a continuous evolution of the aggregate/layer structure during crystal growth is observed. [source] Growth of YCOB single crystals by flux technique and their characterizationCRYSTAL RESEARCH AND TECHNOLOGY, Issue 5 2008R. Arun Kumar Abstract Nonlinear optical single crystals of YCOB with good optical quality were grown by the flux technique for the first time. Polycrystalline YCOB samples were synthesized by solid state reaction method. The thermal analysis of the sample was performed with lithium carbonate flux in different weight proportions and the growth temperature was optimised. Single crystals of YCOB with dimensions 3 × 3 × 5 mm3 were obtained by the method of ,slow-cooling'. The grown crystals were characterized by XRD, UV-VIS-NIR, EDAX, FTIR and etching studies. The powder XRD pattern revealed the formation of YCOB compound. The lattice parameters were identified through single crystal XRD studies. The UV-VIS-NIR results showed that the crystal has a sharp cutoff at 220 nm and is nearly 55% transparent over a wide wavelength range enabling applications in the UV region. The EDAX measurement revealed the ,flux-free' crystal formation. The presence of the functional groups belonging to the YCOB crystals was identified by the FTIR results. ,Hillock-like' patterns are observed in the etching studies. The primary emphasis in this study is laid to describe ,flux technique' as an alternative method to grow YCOB crystals. The results are presented and discussed. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Sedimentation as a tool for crystallization from protein mixturesCRYSTAL RESEARCH AND TECHNOLOGY, Issue 11 2006I. Dimitrov Abstract Crystals from apoferritin which is an iron-free form of protein ferritin were obtained from protein mixtures lysozyme/apoferritin using sedimentation under high gravity. Solution containing apoferritin at concentration as high as 5mg/ml in the presence of 25mg/ml lysozyme and overlaid on 5%(w/v) CdSO4 in 0,2M/L NaAC, pH=5 still favors apoferritin crystal formation under normal gravity conditions, but at apoferritin concentrations <0,5mg/ml (,1,14µM/L) in 25mg/ml (,1,71mM/L) lysozyme only the sedimentation in a centrifuge appears to be useful for separating the apoferritin molecules from the mixture followed by apoferritin crystallization in the same system. The very high molecule number ratio (,1:103) of two proteins is used to stress on the observed effect. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Gallbladder Na+/H+ exchange activity is up-regulated prior to cholesterol crystal formationEUROPEAN JOURNAL OF CLINICAL INVESTIGATION, Issue 8 2005S. C. Narins Abstract Background, Gallbladder Na+ and H2O absorption are increased prior to gallstone formation and may promote cholesterol nucleation. Na+/H+ exchange (NHE) isoforms NHE2 and NHE3 are involved in gallbladder Na+ transport in prairie dogs. We examined whether increased gallbladder Na+ absorption observed during early gallstone formation is the result of NHE up-regulation. Materials and methods, Native gallbladder and primary cultures of gallbladder epithelial cells (GBECs) harvested from prairie dogs fed nonlithogenic (CON) or 1·2% cholesterol diet for varying lengths of time to induce cholesterol-saturated bile (PreCRYS), cholesterol crystals (CRYS), or gallstones (GS) were used. NHE activity was assessed by measuring dimethylamiloride-inhibitable 22Na+ uptake under H+ gradient in primary GBECs. HOE-694 was used to determine NHE2 and NHE3 contributions. NHE protein and mRNA expression were examined by Western and Northern blots, respectively. Results, Gallbladder total NHE activity was 25·1 ± 1·3 nmol mg protein,1 min,1 in the control and increased during gallstone formation peaking at the PreCRYS stage (98·4 ± 3·9 nmol mg protein,1 min,1). There was a shift in NHE activity from NHE2 to NHE3 as the animals progressed from no stones through the PreCRYS and CRYS stages to gallstones. The increase in NHE activity was partly caused by an increased Vmax without any change in KNam. Both NHE2 and NHE3 protein increased moderately during the PreCRYS stage without increases in mRNA expression. Conclusions, Increased gallbladder Na+ absorption observed prior to crystal formation is in part caused by an increase NHE activity which is not fully accounted for by an increase in NHE proteins and mRNA levels but may be explained by enhanced localization in the membranes and/or altered regulation of NHE. [source] Promoters of crystal protein genes do not control crystal formation inside exosporium of Bacillus thuringiensis ssp. finitimus strain YBT-020FEMS MICROBIOLOGY LETTERS, Issue 1 2009Fang Ji Abstract Most Bacillus thuringiensis parasporal crystals separate from spores after sporulation. A special phenomenon called spore-crystal association (SCA) occurs in a few subspecies (e.g. ssp. finitimus) where enclosed crystals are associated with spores. In this study, the involvement of crystal protein gene promoters in SCA was investigated. Two crystal protein genes, cry26Aa and cry28Aa, were isolated from subspecies finitimus strain YBT-020, and each or both were then transferred to acrystalliferous B. thuringiensis strain BMB171 and the plasmid-cured derivative of strain YBT-020. SCA was not observed with any recombinant strain, implying that the crystal protein genes are not sufficient to cause SCA. When the typical crystal protein gene cry1Ca was introduced into strain YBT-020, free bipyramidal crystals formed in addition to SCA. Recombinant genes containing the promoter of cry26Aa or cry28Aa fused with the coding sequence (CDS) of cry1Ca were introduced into strain YBT-020, and the typical cry1Ca phenotype was observed. Another two fusion genes consisting of the promoter of cry1Ca and the CDS of cry26Aa or cry28Aa were also transferred to strain YBT-020. Only enclosed crystals formed. These results indicate that the promoters of the crystal protein genes are not the key factor determining the crystal location in strain YBT-020. [source] Semiconductor-Dielectric Blends: A Facile All Solution Route to Flexible All-Organic TransistorsADVANCED MATERIALS, Issue 42 2009Wi Hyoung Lee A one-step process for the production of all-organic, all-solution-processed field-effect transistors (FETs) can be achieved using triethylsilylethynyl anthradithiophene (TES-ADT). TES-ADT has a lower surface energy than poly(methyl methacrylate) (PMMA), which results in a segregation and crystal formation of TES-ADT at the air,film interface after spin-casting and subsequent solvent annealing. The resulting FETs comprise vertically phase-separated semiconducting and dielectric layers and exhibit high performances. [source] Formation of Lipid Emulsions and Clear Gels by Liquid Crystal EmulsificationINTERNATIONAL JOURNAL OF COSMETIC SCIENCE, Issue 1 2007T. Suzuki Recently developed emulsion technologies for the formation of fine emulsions, lipid emulsions and clear gels by liquid crystal emulsification were reviewed. As a basic information on liquid crystal emulsification, the structures and characteristic behaviours of lyotropic liquid crystals were summarized. Formation of a liquid crystalline phase was often seen in emulsions and biological systems. The significance of liquid crystal formation during emulsification was analysed by comparing the states and stabilities of emulsions prepared by different processes. Then uses of liquid crystals for formation of the characteristic emulsions and gels were also discussed. In liquid crystal emulsification, an oil phase is dispersed directly into the lamellar liquid-crystalline phase composed of surfactant, glycerol and water to prepare a gel-like oil-in-liquid crystal emulsion. This is followed by dilution with the remaining water to produce an emulsion. From the phase behaviour during emulsification and analysis of the local motion of the liquid crystal membrane by fluorometry, it was confirmed that the interaction between surfactant and a polyol molecule such as glycerol promotes hydrogen bonding and enhances the strength of the lamellar liquid crystal membranes, which results in the formation of oil-in-liquid crystal emulsions. The interaction between the liquid crystal and oil was analysed from the changes in molecular motion of the membrane at the oil-liquid crystal interface using the spin label technique of electron spin resonance (ESR). The fluidity of the liquid crystal membrane did not change when oil was added, and therefore oil-in-liquid crystal emulsions of various oils were prepared by the identical process. This lack of dependence of the liquid crystal membrane on oil results in the unique properties of liquid crystal emulsification, which can be used for oils of various polarity and different molecular constituents. When a self-organizing artificial stratum corneum lipid containing pseudo-ceramide was used as a principal component of the oil, a multilamellar emulsion of concentric lamellar structure was formed. The multilamellar emulsion supplements the physiological function of stratum corneum by the identical mechanism as natural intercellular lipids. High-pressure treatment of the lipid emulsion produced a gel-like emulsion crystal, in which the homogeneous nanoemulsion droplets were arranged in a hexagonal array. This review paper was presented at the Conference of the Asian Societies of Cosmetic Scientists 2005 in Bangkok. [source] Editorial Comment to renal tubular epithelial cell injury and oxidative stress induce calcium oxalate crystal formation in mouse kidneyINTERNATIONAL JOURNAL OF UROLOGY, Issue 1 2010Tohru Umekawa md phd No abstract is available for this article. [source] Early stages of protein crystallization as revealed by emerging optical waveguide technologyJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3 2008Attia Boudjemline A highly sensitive method for studying the onset of protein crystallization in real time using an optical-waveguide-based technique is reported. Dual polarization interferometry uses light from sensing and reference waveguides to produce an interference pattern, which when the sensing waveguide is immersed in a protein solution supplies information on the thickness and density of any protein adlayer on the sensing waveguide's surface. This technique provides evidence that crystallization proceeds via large protein aggregates but, more strikingly, shows dramatic light loss from the sensing waveguide at a very early stage during crystallization. The technique proves relatively insensitive to the crystallization of small molecules or poorly formed protein crystals and affords a method of distinguishing crystal formation from the formation of other protein aggregates or salt crystals. The experimental setup currently necessitates crystallization using the batch method, and precipitant mixing at high supersaturation is known to introduce a greater variability compared with methods such as vapour diffusion or dialysis, but first results promise to bridge the paucity of real-time methods available to distinguish the onset of protein crystallization from other forms of aggregation. [source] Small and wide-angle X-ray scattering study of metallocene isotactic poly(propylene)JOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3-1 2000P.S. Dai We report a study of metallocene isotactic poly(propylene) (m-iPP) which crystallizes into , and , crystal modifications. Simultaneous in-situ small- and wide-angle X-ray scattering (SAXS and WAXS) were used to study kinetics during crystallization. Both techniques provide information about time development of crystallinity, while WAXS gives also kinetics of formation of , and , crystals. During the earliest stages of crystal formation, the SAXS Bragg peak occurs simultaneously, or slightly lags, the appearance of crystalline WAXS reflections. We conclude crystallization occurs by a nucleation and growth process in this m-iPP. [source] Effect of monomer composition on crystal growth by resin containing bioglassJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 1 2010Masanori Hashimoto Abstract This study evaluated the effect of resin monomer composition on crystal growth at the interface between the resin/bioglass composites and water. Light-cured resin that contained 2-bis[4(2-hydroxy-3-methacryloyloxy-propyloxy)-phenyl], 2-hydroxyethyl methacrylate, and triethylene glycol dimethacrylate with different compositions were used. Resin/bioglass composites were prepared with 40 mass% bioglass and 60 mass% resin. The resin/bioglass composites were stored in deionized distilled water for 24 h (control group) or 3,12 months (experimental groups). After water storage, the disk surfaces were examined by light- and scanning electron microscopy. Chemical states of the crystals were analyzed by laser-Raman spectroscopy and micro-X-ray diffractometry. The microscopic analysis showed crystal on the resin disks surface after six months of water storage for hydrophilic resins. However, there was no crystal formation in the control and the experimental groups of specimens of hydrophobic resins. Raman analysis showed the chemical states of the crystals formed on the resin matrix and bioglass to be different. The micro-X-ray analysis of crystals on resin disks identified them to be calcium carbonate. This crystal formation occurred in water instead of simulated body fluid. In conclusion, the resin monomer compositions affected the ability to induce crystal growth on the surfaces of disks containing bioglass. © 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2010 [source] Characterization of Ice Crystals in Pork Muscle Formed by Pressure-shift Freezing as Compared with Classical Freezing MethodsJOURNAL OF FOOD SCIENCE, Issue 4 2004S. Zhu ABSTRACT: Cylindrical specimens of fresh pork muscle packed in plastic bags were frozen by air blaster freezing (ABF), liquid immersion freezing (LIF), and pressure-shift freezing (PSF) (100 to 200 MPa). Sample internal temperature and phase transformations were monitored at center, midway, and surface locations. ABF and LIF resulted in large irregular ice crystals, causing serious muscle structure deformation. PSF ice crystals were generally small and regular, but differed along the radial direction. Near the surface, there were many fine and regular intracellular ice crystals with well-preserved muscle tissue. From midway to the center, ice crystals were larger in size and located extracellularly. Ice crystal formation was affected by super-cooling during/after depressurization and subsequent freezing. [source] Effect of pH on synthesis and properties of perovskite oxide via a citrate processAICHE JOURNAL, Issue 2 2006Zhentao Wu Abstract A series of La0.6Sr0.4Co0.4Fe0.6O3-, (LSCF) perovskite-type oxides were synthesized using a modified citrate process under various pH conditions (pH =1, 3, 5, 7, and 9, respectively). The effect of pH on the chelate process, crystal development, morphology, and oxygen permeability of LSCF oxides were investigated. FT-IR analysis showed that the chelate processes for pH = 1 and 3 were different from those for pH = 5, 7, and 9. XRD and SEM observations revealed that the crystal formation and morphology of LSCF oxides were dependent on the precursors with different pH conditions. The LSCF membranes derived from the precursors with lower pH values (pH = 1 and 3) exhibited larger apparent activation energy for oxygen permeation than the other samples (pH = 5, 7, and 9) in the range of 1073-1123K. This study indicated that properties such as crystallinity and oxygen permeability of LSCF oxide could be tailored by controlling the pH values in the synthesis process. © 2005 American Institute of Chemical Engineers AIChE J, 2006 [source] Self-association of cromolyn sodium in aqueous solution characterized by nuclear magnetic resonance spectroscopyJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 5 2004Xuan Ding Abstract The major objective of this study was to investigate and characterize the solution properties of cromolyn sodium (in D2O or D2O/H2O phosphate buffer at pH 7.5) using nuclear magnetic resonance (NMR) spectroscopy. The self-association of cromolyn molecules was examined primarily via one-dimensional 1H and 13C, and two-dimensional homonuclear NOESY NMR. Significant spectral shifts were observed for a majority of cromolyn 1H and 13C resonances, and are attributed to inter-molecular ring-stacking association accompanied by intra-molecular conformational changes. The critical self-association concentration was determined to be 10 mg/mL at pH 7.5 and 25°C by measuring the chemical shift of a specific cromolyn 1H resonance. The observed magnitude and sign changes of NOESY correlations indicate the formation of cromolyn aggregates with restricted molecular mobility. Mesomorphic liquid crystal formation is suggested by uniformly pronounced line broadening in concentrated cromolyn solutions; the transition concentration was approximately 60 mg/mL at 25°C, which is consistent with literature findings based on other techniques. A stronger tendency toward association was observed at lower temperature but aggregation appeared to be independent of pH. Lastly, it was concluded that self-association of cromolyn is promoted by the presence of monovalent cations as a result of reduced electrostatic repulsive forces. © 2004 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 93:1351,1358, 2004 [source] Improvement of Mechanical Properties of Self Setting Calcium Phosphate Bone Cements Mixed With Different Metal OxidesMATERIALWISSENSCHAFT UND WERKSTOFFTECHNIK, Issue 12 2003U. Gbureck Calciumphosphat Zemente; Metalloxide; Mechanische Eigenschaften Abstract Calcium phosphate cements (CPC), based on multicomponent powder mixtures of calcium orthophosphates with medium particle sizes in the region of 1 - 20 ,m, set isothermally in an aqueous environment to form hydroxyapatite (HA). HA cement reactants include tetracalcium phosphate (TTCP), tricalcium phosphate (TCP), dicalcium phosphate anhydrate (DCPA), dicalcium phosphate dihydrate (DCPD), monocalcium phosphate (MCPA) or octacalcium phosphate (OCP). The aim of this study was to improve the mechanical performance of TTCP / DCPA cement by adding several metal oxides to tetracalcium phosphate during the fabrication process. Cements based on tetracalcium phosphate mixed with silica or titanium oxide showed significant increases in compressive strength, approximately 80 - 100 MPa, whilst no change in the mechanical behavior of CPC was observed if zirconia was added. X-ray diffraction measurement confirmed the setting reaction of doped cements was similar to that of pure CPC. Low crystalline HA was found to be the main constituant of set cement; additional phases, such as calcium titanate or calcium zirconate, were not involved in the reaction. A mechanical reinforcement effect was thought to result from changes in the thermodynamic or kinetic solubilities of doped tetracalcium phosphates, this would lead to slower HA crystal formation and a more cross-linked cement structure. Verbesserung der mechanischen Eigenschaften von Calciumphosphat-Zementen durch Modifikation mit verschiedenen Metalloxiden Calciumphosphat-Zemente, CPC, bestehen aus Pulvermischungen verschiedener Calcium orthophophate, beispielsweise Tetracalciumphosphat (TTCP), Tricalciumphosphat (TCP), Dicalciumphosphatanhydrid (DCPA), Dicalciumphosphatdihydrat (DCPD), Monocalcium phosphatanhydrid (MCPA) oder Octacalciumphosphat (OCP) mit durchschnittlichen Partikelgrößen im Bereich von 1 , 20 ,m. Die Zemente binden in wässriger Umgebung isotherm zu Hydroxylapatit ab. Das Ziel dieser Arbeit war die Verbesserung materialspezifischer Eigenschaften , wie die mechanische Festigkeit - eines TTCP / DCPA-Zementes durch die Verwendung von Metalloxiden im Syntheseprozess von Tetracalciumphosphat. Zemente, die aus mit Silicium- oder Titandioxid versetzten Tetracalciumphosphaten hergestellt wurden, zeigten eine deutliche Steigerung der Druckfestigkeit auf Werte von 80 , 100 MPa, während im Falle von Zirkoniumdioxid keine Änderung der mechanischen Stabilität erreicht werden konnte. Röntgendiffraktometrische Untersuchungen ergaben, dass die Abbindereaktion dieser Zemente ähnlich der eines reinen TTCP / DCPA-Zements verläuft. Jeweiliges Hauptprodukt war niedrigkristalliner Hydroxylapatit, die im Herstellungsprozess von Tetracalciumphosphat entstandenen Nebenprodukte Calciumtitanat bzw. ,zirkonat waren nicht an der Abbindereaktion beteiligt. Ein Grund für die Steigerung der mechanischen Stabilität ist offensichtlich die Veränderung der kinetischen und thermodynamischen Löslichkeit der synthetisierten Tetracalciumphosphate, die zu einer langsameren Abbindereaktion und somit einer besseren Vernetzung in der Hydroxylapatitstruktur führt. [source] Predictable close-packing similarities between cis - and trans -2-hydroxy-1-cyclooctanecarboxylic acids and trans -2-hydroxy-1-cyclooctanecarboxamideACTA CRYSTALLOGRAPHICA SECTION B, Issue 5 2002Alajos Kálmán In order to extend the experimental data already available on the close packing of cyclopentanes substituted with vicinal COX (X,=,OH, NH2) and OH groups to the analogous cyclohexanes, cycloheptanes and cyclooctanes, (1R*,2S*) -cis- 2-hydroxy-1-cyclooctanecarboxylic acid (8C), (1R*,2R*)- trans -2-hydroxy-1-cyclooctanecarboxylic acid (8T) and (1R*,2R*)- trans -2-hydroxy-1-cyclooctanecarboxamide (8T*) were subjected to X-ray crystal structure analysis. In 8T and 8T*, the hydrogen bonds form infinite ribbons of dimers joined by (12) rings with Ci symmetry. Two types of dimer alternate along each ribbon. The dimers differ in the donor and acceptor roles of the functional groups. This pattern was previously deduced topologically among the possible forms of association for heterochiral dimers [Kálmán et al. (2002). Acta Cryst. B58, 494,501]. As they have the same pattern of hydrogen bonds, 8T and 8T* are isostructural. The additional donor (i.e. the second hydrogen of the NH2 group) present in 8T* links the adjacent ribbons so as to form smaller (8) rings between them. The crystals of the cis stereoisomer 8C are built up from antiparallel hydrogen-bonded helices. The topology and symmetry of this structure are the same as for the close packing of (1R*,2R*,4S*)-4- tert -butyl-2-hydroxy-1-cyclopentanecarboxamide [Kálmán et al. (2001). Acta Cryst. B57, 539,550]; only the hydrogen-bond donors and acceptors are interchanged, in the same way as in the two dimer types of 8T and 8T* ribbons. This analogy suggests that helices may originate as homochiral dimers with C2 symmetry and polymerize into helices during crystal formation. The conformational characteristics of the heterochiral dimers observed in the title compounds and in closely related structures are discussed. [source] Improved conception rates in sows inseminated with cryopreserved boar spermatozoa prepared with a more optimal combination of osmolality and glycerol in the freezing extenderANIMAL SCIENCE JOURNAL, Issue 2 2009Tetsuji OKAZAKI ABSTRACT Cryoprotectant agents (CPAs) are added in freezing extenders to prevent intracellular ice crystal formation. However, it has been reported that high dose of CPAs confer toxicity on spermatozoa. Recently, the reduction of intracellular water by a high osmolality solution has also resulted in the suppression of ice crystal formation in spermatozoa, suggesting that the optimal combination of glycerol concentration and freezing extender osmolality could contribute to the development of effective sperm cryopreservation techniques. In this study, we investigated the motility, membrane and acrosomal integrity of frozen-thawed boar spermatozoa treated with freezing extender (NSF) of varying osmolalities (300, 400, 500 mOsm/kg) and final concentrations of glycerol (0.5, 1, 2, 3%). The spermatozoa that were treated at 400 mOsm/kg and 2% glycerol showed significantly higher rates of motility and membrane integrity compared with those in other treatment groups. In addition, the conception and implantation rates of swine artificially inseminated with spermatozoa frozen by the novel freezing extender (conception; 79%, implantation; 57.5%) were significantly higher than those of frozen-thawed spermatozoa treated in the conventional NSF (300 mOsm/kg, 3% glycerol) (conception; 29%, implantation; 33.8%). From these results, we concluded that the novel hyperosmotic (400 mOsm/kg) and low-glycerol (final concentration 2%) freezing extender is beneficial for the cryopreservation of boar spermatozoa. [source] Structure of the ribosomal protein L1,mRNA complex at 2.1,Å resolution: common features of crystal packing of L1,RNA complexesACTA CRYSTALLOGRAPHICA SECTION D, Issue 12 2006S. Tishchenko The crystal structure of a hybrid complex between the bacterial ribosomal protein L1 from Thermus thermophilus and a Methanococcus vannielii mRNA fragment containing an L1-binding site was determined at 2.1,Å resolution. It was found that all polar atoms involved in conserved protein,RNA hydrogen bonds have high values of density in the electron-density map and that their hydrogen-bonding capacity is fully realised through interactions with protein atoms, water molecules and K+ ions. Intermolecular contacts were thoroughly analyzed in the present crystals and in crystals of previously determined L1,RNA complexes. It was shown that extension of the RNA helices providing canonical helix stacking between open,open or open,closed ends of RNA fragments is a common feature of these and all known crystals of complexes between ribosomal proteins and RNAs. In addition, the overwhelming majority of complexes between ribosomal proteins and RNA molecules display crystal contacts formed by the central parts of the RNA fragments. These contacts are often very extensive and strong and it is proposed that they are formed in the saturated solution prior to crystal formation. [source] A method for screening the temperature dependence of three-dimensional crystal formationACTA CRYSTALLOGRAPHICA SECTION D, Issue 5 2006Michael J. Landsberg Temperature is an important parameter controlling protein crystal growth. A new temperature-screening system (Thermo-screen) is described consisting of a gradient thermocycler fitted with a special crystallization-plate adapter onto which a 192-well sitting-drop crystallization plate can be mounted (temperature range 277,372,K; maximum temperature gradient 20,K; interval precision 0.3,K). The system allows 16 different conditions to be monitored simultaneously over a range of 12 temperatures and is well suited to conduct wide (,20,K) and fine (,3,K) temperature-optimization screens. It can potentially aid in the determination of temperature phase diagrams and run more complex temperature-cycling experiments for seeding and crystal growth. [source] Mutation of surface residues to promote crystallization of activated factor XI as a complex with benzamidine: an essential step for the iterative structure-based design of factor XI inhibitorsACTA CRYSTALLOGRAPHICA SECTION D, Issue 10 2005Pramod Pandey Activated factor XI (FXIa) is a key enzyme in the amplification phase of the blood-coagulation cascade. Thus, a selective FXIa inhibitor may have lesser bleeding liabilities and provide a safe alternative for antithrombosis therapy to available drugs on the market. In a previous report, the crystal structures of the catalytic domain of FXIa (rhFXI370,607) in complex with various ecotin mutants have been described [Jin et al. (2005), J. Biol. Chem.280, 4704,4712]. However, ecotin forms a matrix-like interaction with rhFXI370,607 and is impossible to displace with small-molecule inhibitors; ecotin crystals are therefore not suitable for iterative structure-based ligand design. In addition, rhFXI370,607 did not crystallize in the presence of small-molecule ligands. In order to obtain the crystal structure of rhFXI370,607 with a weak small-molecule ligand, namely benzamidine, several rounds of surface-residue mutation were implemented to promote crystal formation of rhFXI370,607. A quadruple mutant of rhFXI370,607 (rhFXI370,607 -S434A,T475A,C482S,K437A) readily crystallized in the presence of benzamidine. The benzamidine in the preformed crystals was easily exchanged with other FXIa small-molecule inhibitors. These crystals have facilitated the structure-based design of small-molecule FXIa inhibitors. [source] The Corynebacterium glutamicum aconitase repressor: scratching around for crystalsACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 9 2010Javier García-Nafría Imperfections on the surfaces of crystallization containers are known to influence crystal formation and are thought to do so by helping to overcome the nucleation barrier. The intentional creation of imperfections has been widely applied to induce crystallization of small molecules, but has not been reported for protein crystallization. Here, the crystallization and preliminary X-ray analysis of the TetR-type aconitase repressor are reported. This regulator was the first transcription factor to be identified in the regulation of the tricarboxylic acid cycle in Corynebacterium glutamicum, an organism that is of special industrial interest and is an emerging model organism for Corynebacterineae. Successful crystallization involved introducing manual scratches on the surface of standard commercial plates, which led to a substantial improvement in crystal nucleation and quality. [source] Enzyme-assisted physicochemical enantioseparation processes,Part III: Overcoming yield limitations by dynamic kinetic resolution of asparagine via preferential crystallization and enzymatic racemizationBIOTECHNOLOGY & BIOENGINEERING, Issue 6 2009Kerstin Würges Abstract The application of enantioseparation methods alone can only yield up to 50% of the desired chiral product. Thus enantioseparation becomes more attractive when accompanied by the racemization of the counter-enantiomer. Here we present first results of dynamic kinetic resolution of L -asparagine (L -Asn) via preferential crystallization and enzymatic racemization from a racemic, supersaturated solution on a 20,mL scale. An enzyme lyophilisate (WT amino acid racemase from P. putida KT2440 (E.C. 5.1.1.10), overexpressed in E. coli BL21(DE3)) was used for in situ racemization (enzyme concentrations varying from 0 to 1,mg/mL). When preferential crystallization was applied without any enzyme, a total of 31,mg of L -Asn monohydrate could be crystallized, before crystal formation of d -Asn started. Crystallization experiments accompanied by enzymatic racemization led to a significant increase of crystallized L -Asn (198,mg L -Asn monohydrate; >92%ee) giving the first experimental proof for this new process concept of dynamic kinetic resolution via preferential crystallization and enzymatic racemization. Measurements of the racemase activity before and after the crystallization process showed no significant differences, which would allow for enzyme recovery and recycling. Biotechnol. Bioeng. 2009; 104: 1235,1239. © 2009 Wiley Periodicals, Inc. [source] Dipole Moment Enhancement in Molecular Crystals from X-ray Diffraction DataCHEMPHYSCHEM, Issue 14 2007Mark A. Spackman Prof. Abstract Although reliable determination of the molecular dipole moment from experimental charge density analyses on molecular crystals is a challenging undertaking, these values are becoming increasingly common experimental results. We collate all known experimental determinations and use this database to identify broad trends in the dipole moment enhancements implied by these measurements as well as outliers for which enhancements are pronounced. Compelling evidence emerges that molecular dipole moments from X-ray diffraction data can provide a wealth of information on the change in the molecular charge distribution that results from crystal formation. Most importantly, these experiments are unrivalled in their potential to provide this information in such detail and deserve to be exploited to a much greater extent. The considerable number of experimental determinations now available has enabled us to pinpoint those studies that merit further attention, either because they point unequivocally to a considerable enhancement in the crystal (of 50,% or more), or because the experimental determinations suggest enhancements of 100,% or more,much larger than independent theoretical estimates. In both cases further detailed experimental and theoretical studies are indicated. [source] Adsorption behaviour of azo disperse dyes on polyurethane fibreCOLORATION TECHNOLOGY, Issue 3 2009Hong-Fei Qian Adsorption isotherms of disperse dyes were measured and the surfaces of dyed polyurethane, cellulose diacetate and polylactic acid fibres were observed using a scanning electron microscope and compared. Obvious crystal growth of the dyes occurred on the surface of the polyurethane fibres. The maximum dye uptake on polyurethane fibres and the degree of crystal growth varied greatly with the dye type. Factors such as the dye affinity for the fibre, crystallisation properties and dye solubility in the dyebath affect the sorbed state of the dye on the fibre surface. A mechanism is proposed for crystal formation on the fibre surface during dyeing of polyurethane fibre with disperse dyes. [source] Effect of citric acid and 1,2-dihydroxybenzene 3,5-disulfonic acid on crystallization of calcium sulfate dihydrate under simulated conditions of phosphoric acid productionCRYSTAL RESEARCH AND TECHNOLOGY, Issue 8 2005M. M. Rashad Abstract The effect of citric acid and 1,2-dihydroxybenzene 3,5-disulfonic acid (DHBDSA), as additives, on the crystallization of gypsum was studied under simulated conditions of the of phosphoric acid production. Calcium hydrogen phosphate and sulfuric acid were mixed with dilute phosphoric acid at 80 °C, and the turbidity of the reaction mixture was measured at different time periods to calculate the induction time of gypsum crystals formation. Addition of citric acid increased the induction time and decreased the growth efficiency while addition of DHBDSA decreased the induction time and increased the growth efficiency compared with in absence of additives. The crystals mean and median diameters were found to decrease in the presence of citric acid and increased in the presence of DHBDSA. The surface energy decreased with citric acid and increased with DHBDSA compared to the baseline (without additives). Interestingly, the majority of the formed crystals are tabular with DHBDSA and needle-like type with citric acid and baseline [source] |