Seeding from silica-reinforced lysozyme crystals for neutron crystallography

2018 ◽  
Vol 74 (12) ◽  
pp. 1200-1207 ◽  
Author(s):  
Jose A. Gavira ◽  
Mayte Conejero-Muriel ◽  
José Manuel Delgado-López

The fragility of protein crystals plays an important role in the final quality of the diffraction data and therefore that of the derived three-dimensional structural model. The growth of protein crystals in gels of various natures has been shown to overcome this problem, facilitating the manipulation of the crystals; this is probably owing, amongst other factors, to the incorporation of the gel fibres within the body of the crystal. In this study, lysozyme crystals were grown in silica gel at a wide range of concentrations of up to 22%(v/v) to quantitatively determine the amount of gel incorporated into the crystal structure by means of thermogravimetric analysis. The interaction between the silica fibres and the lysozyme molecules within the crystals was also investigated using Raman spectroscopy and the direct influence on the crystalline protein stability was analysed using differential scanning calorimetry. Finally, the benefits of the use of gel-grown crystals to overgrow protein crystals intended for neutron diffraction are highlighted.


2017 ◽  
Vol 474 (24) ◽  
pp. 4253-4268 ◽  
Author(s):  
Alessia Leonetti ◽  
Laura Cervoni ◽  
Fabio Polticelli ◽  
Yuta Kanamori ◽  
Zuleyha Nihan Yurtsever ◽  
...  

Spermine oxidase (SMOX) is a flavin-containing enzyme that oxidizes spermine to produce spermidine, 3-aminopropanaldehyde, and hydrogen peroxide. SMOX has been shown to play key roles in inflammation and carcinogenesis; indeed, it is differentially expressed in several human cancer types. Our previous investigation has revealed that SMOX purified after heterologous expression in Escherichia coli actually consists of monomers, covalent homodimers, and other higher-order forms. All association forms oxidize spermine and, after treatment with dithiothreitol, revert to SMOX monomer. Here, we report a detailed investigation on the thermal denaturation of SMOX and its association forms in native and reducing conditions. By combining spectroscopic methods (circular dichroism, fluorescence) and thermal methods (differential scanning calorimetry), we provide new insights into the structure, the transformation, and the stability of SMOX. While the crystal structure of this protein is not available yet, experimental results are interpreted also on the basis of a novel SMOX structural model, obtained in silico exploiting the recently solved acetylspermine oxidase crystal structure. We conclude that while at least one specific intermolecular disulfide bond links two SMOX molecules to form the homodimer, the thermal denaturation profiles can be justified by the presence of at least one intramolecular disulfide bond, which also plays a critical role in the stabilization of the overall three-dimensional SMOX structure, and in particular of its flavin adenine dinucleotide-containing active site.



2018 ◽  
Vol 860 ◽  
pp. 739-766 ◽  
Author(s):  
Rémi Bourguet

The flow-induced vibrations of an elastically mounted circular cylinder, free to oscillate in an arbitrary direction and forced to rotate about its axis, are examined via two- and three-dimensional simulations, at a Reynolds number equal to 100, based on the body diameter and inflow velocity. The behaviour of the flow–structure system is investigated over the entire range of vibration directions, defined by the angle $\unicode[STIX]{x1D703}$ between the direction of the current and the direction of motion, a wide range of values of the reduced velocity $U^{\star }$ (inverse of the oscillator natural frequency) and three values of the rotation rate (ratio between the cylinder surface and inflow velocities), $\unicode[STIX]{x1D6FC}\in \{0,1,3\}$, in order to cover the reference non-rotating cylinder case, as well as typical slow and fast rotation cases. The oscillations of the non-rotating cylinder ($\unicode[STIX]{x1D6FC}=0$) develop under wake-body synchronization or lock-in, and their amplitude exhibits a bell-shaped evolution, typical of vortex-induced vibrations (VIV), as a function of $U^{\star }$. When $\unicode[STIX]{x1D703}$ is increased from $0^{\circ }$ to $90^{\circ }$ (or decreased from $180^{\circ }$ to $90^{\circ }$), the bell-shaped curve tends to monotonically increase in width and magnitude. For all angles, the flow past the non-rotating body is two-dimensional with formation of two counter-rotating spanwise vortices per cycle. The behaviour of the system remains globally the same for $\unicode[STIX]{x1D6FC}=1$. The principal effects of the slow rotation are a slight amplification of the VIV-like responses and widening of the vibration windows, as well as a limited asymmetry of the responses and forces about the symmetrical configuration $\unicode[STIX]{x1D703}=90^{\circ }$. The impact of the fast rotation ($\unicode[STIX]{x1D6FC}=3$) is more pronounced: VIV-like responses persist over a range of $\unicode[STIX]{x1D703}$ but, outside this range, the system is found to undergo a transition towards galloping-like oscillations characterised by amplitudes growing unboundedly with $U^{\star }$. A quasi-steady modelling of fluid forcing predicts the emergence of galloping-like responses as $\unicode[STIX]{x1D703}$ is varied, which suggests that they could be mainly driven by the mean flow. It, however, appears that flow unsteadiness and body motion remain synchronised in this vibration regime where a variety of multi-vortex wake patterns are uncovered. The interaction with flow dynamics results in deviations from the quasi-steady prediction. The successive steps in the evolution of the vibration amplitude versus $U^{\star }$, linked to wake pattern switch, are not captured by the quasi-steady approach. The flow past the rapidly-rotating, vibrating cylinder becomes three-dimensional over an interval of $\unicode[STIX]{x1D703}$ including the in-line oscillation configuration, with only a minor effect on the system behaviour.



2015 ◽  
Vol 1117 ◽  
pp. 283-286
Author(s):  
Inga Dāboliņa ◽  
Ausma Viļumsone ◽  
Jānis Dāboliņš ◽  
Dana Beļakova

Computer aided designing software not only the possibility to speed up the process of putting a new model into production and improve the quality of the products, but also reduces material costs and labour intensity, ensuring an elastic change of the assortment. The designing of clothes includes a row of processes and one of the most time and labour consuming is constructing. A construction displays the layout (pattern) of the surface of the body (garment). As it depends on correct anthropometric data, it is very important to get ones right. The use of 3D surface scanning technologies to produce digitized representations of the human anatomy has the potential to help change the way a wide range of products are designed and produced. Every scanning device is equipped with optic (light) appliances to ensure non-contact measuring. Measurements acquired by 3D scanning device should be checked out for compliance with CAD systems for automatized pattern making procedure. The paper introduces the experiment with scanned data usage in CAD pattern making. The project aims to implement scanned data values in the CAD/CAM individual measurement list for acquiring individualized pattern blocks.



Author(s):  
A. J. Perrotta ◽  
J. V. Smith

SummaryA full-matrix, three-dimensional refinement of kalsilite, KAlSi04 (hexagonal, a 5·16, c 8.69 Å, P6a), shows that the silicon and aluminium atoms are ordered. The respective tetrahedral distances of 1·61 and 1·74 Å agree with values of 1·61 and 1·75 Å taken to be typical of framework structures. As in nepheline, an oxygen atom is statistically distributed over three sites displaced 0·25 Å from the ideal position on a triad axis. This decreases the bond angle from 180° to 163° in conformity with observations on some other crystal structures. The potassiumoxygen distances of 2·77, 2·93, and 2·99 Å are consistent with the wide range normally found for this weakly bonded atom.



2016 ◽  
Vol 71 (5) ◽  
pp. 611-619 ◽  
Author(s):  
Yurii Prots ◽  
Felix Lange ◽  
Christina Drathen ◽  
Marcus Schmidt ◽  
Yuri Grin

AbstractCombining laboratory X-ray powder diffraction with in-situ high-temperature synchrotron experiments and differential scanning calorimetry, it has been shown that Ba21Al40, Ba3Al5, Ba7Al10 and Ba4Al5 decompose peritectically at 914, 826, 756, and 732°C, respectively. In addition, a new binary compound with the composition Ba4Al7+x (x = 0.17) and the formation temperature of 841°C was found. The initial structural model (space group P63/mmc, a = 6.0807(1), c = 39.2828(8) Å) with four Ba and five Al crystallographic positions was developed. It is based on the intergrowth concept involving the neighboring Ba21Al40 and Ba3Al5 phases and the derived atomic arrangement is subsequently refined using X-ray diffraction data. The crystal structures of all phases in the Ba–Al system, except BaAl4, exhibit Kagomé nets of aluminum atoms resembling those observed for the B atoms in the Laves phases AB2. In the crystal structure of Ba4Al7+x, single Kagomé layers alternate with double slabs (MgZn2 motif) along [001] and are separated by Ba cations. Intergrowth features of Ba4Al7+x are discussed together with the neighboring Ba–Al compounds and Sr5Al9.



2020 ◽  
Vol 26 (10) ◽  
pp. 1789-1795
Author(s):  
Mattia Mele ◽  
Giampaolo Campana ◽  
Gregorio Pisaneschi ◽  
Gian Luca Monti

Purpose Multi jet fusion is an industrial additive manufacturing technology characterised by high building speed and considerable properties of the parts. The cooling phase represents a crucial step to determine productivity, since it can take up to 4.5 times the building time. The purpose of this paper is to investigate into effects of cooling rate on parts manufactured by multi jet fusion. Crystallinity, density, distortions and mechanical properties of specimens produced through an HP multi jet fusion 4200 are examined. Design/methodology/approach An experimental activity is carried out on specimens cooled down at three different rates. Properties of the parts are analysed by means of differential scanning calorimetry, optical microscopy, three-dimensional scanning and tensile testing. Originality/value The present work makes a contribution to the body of knowledge providing correlations between the cooling phase of multi jet fusion and part properties. These results can be used to choose the right balance between production time and product quality.



2017 ◽  
Vol 73 (11) ◽  
pp. 896-904 ◽  
Author(s):  
Ridha Ben Smail ◽  
Mohamed Faouzi Zid

Since the discovery of electrochemically active LiFePO4, materials with tunnel and layered structures built up of transition metals and polyanions have become the subject of much research. A new quaternary arsenate, sodium calcium trinickel aluminium triarsenate, NaCa1–x Ni3–2x Al2x (AsO4)3 (x = 0.23), was synthesized using the flux method in air at 1023 K and its crystal structure was determined from single-crystal X-ray diffraction (XRD) data. This material was also characterized by qualitative energy-dispersive X-ray spectroscopy (EDS) analysis and IR spectroscopy. The crystal structure belongs to the α-CrPO4 type with the space group Imma. The structure is described as a three-dimensional framework built up of corner-edge-sharing NiO6, (Ni,Al)O6 and AsO4 polyhedra, with channels running along the [100] and [010] directions, in which the sodium and calcium cations are located. The proposed structural model has been validated by bond-valence-sum (BVS) and charge-distribution (CHARDI) tools. The sodium ionic conduction pathways in the anionic framework were investigated by means of the bond-valence site energy (BVSE) model, which predicted that the studied material will probably be a very poor Na+ ion conductor (bond-valence activation energy ∼7 eV).



Author(s):  
Christoph Krebs ◽  
Inke Jess ◽  
Christian Näther

The reaction of Co(NCS)2 with 3-(aminomethyl)pyridine as coligand leads to the formation of crystals of the title compound, [Co(NCS)2(C6H8N2)2] n , that were characterized by single-crystal X-ray analysis. In the crystal structure, the CoII cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions as well as two pyridine and two amino N atoms of four symmetry-equivalent 3-(aminomethyl)pyridine coligands with all pairs of equivalent atoms in a trans position. The CoII cations are linked by the 3-(aminomethyl)pyridine coligands into layers parallel to the ac plane. These layers are further linked by intermolecular N—H...S hydrogen bonding into a three-dimensional network. The purity of the title compound was determined by X-ray powder diffraction and its thermal behavior was investigated by differential scanning calorimetry and thermogravimetry.



Author(s):  
Hayley Worth ◽  
Daniel O'Hara ◽  
Neeru Agarwal ◽  
David Collister ◽  
Frank Brennan ◽  
...  

People with kidney failure can experience a range of symptoms that lead to suffering and poor quality of life. Available therapies are limited, and evidence for new treatment options is sparse, often resulting in incomplete relief of symptoms. There is growing interest in the potential for cannabinoids, including cannabidiol and tetrahydrocannabinol, to treat symptoms across a wide range of chronic diseases. As legal prohibitions are withdrawn or minimized in many jurisdictions, patients are increasingly able to access these agents. Cannabinoid receptors, CB1 and CB2, are widely expressed in the body, including within the nervous and immune systems, and exogenous cannabinoids can have anxiolytic, anti-emetic, analgesic and anti-inflammatory effects. Considering their known physiological actions and successful studies in other patient populations, cannabinoids may be viewed as potential therapies for a variety of common symptoms affecting those with kidney failure, including pruritus, nausea, insomnia, chronic neuropathic pain, anorexia, and restless legs syndrome. In this review, we summarize the pharmacology and pharmacokinetics of cannabinoids, along with what is known about the use of cannabinoids for symptom relief in those with kidney disease, and the evidence available concerning their role in management of common symptoms. Presently, while these agents show varying efficacy with a reasonable safety profile in other patient populations, evidence-based prescribing of cannabinoids for people with symptomatic kidney failure is not possible. Given the symptom burden experienced by individuals with kidney failure, there is an urgent need to understand the tolerability and safety of these agents in this population, which must ultimately be followed by robust, randomized controlled trials to determine if they are effective for symptom relief.



2014 ◽  
Vol 47 (6) ◽  
pp. 2030-2037 ◽  
Author(s):  
Mojmír Meduňa ◽  
Claudiu V. Falub ◽  
Fabio Isa ◽  
Daniel Chrastina ◽  
Thomas Kreiliger ◽  
...  

Quantitative nondestructive imaging of structural properties of semiconductor layer stacks at the nanoscale is essential for tailoring the device characteristics of many low-dimensional quantum structures, such as ultrafast transistors, solid state lasers and detectors. Here it is shown that scanning nanodiffraction of synchrotron X-ray radiation can unravel the three-dimensional structure of epitaxial crystals containing a periodic superlattice underneath their faceted surface. By mapping reciprocal space in all three dimensions, the superlattice period is determined across the various crystal facets and the very high crystalline quality of the structures is demonstrated. It is shown that the presence of the superlattice allows the reconstruction of the crystal shape without the need of any structural model.



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