High-resolution X-ray Data Research Articles

Photolithographic additive manufacturing of high-entropy perovskite oxides from synthesized multimetallic polymeric precursors

In this work, the synthesis of high-entropy perovskite-type oxides from multimetallic polymeric precursors and their shaping by photolithographic additive manufacturing is investigated. Thermosets with well-controlled complex geometries are produced by digital light processing using the multimetallic organic-inorganic hybrid resin developed in this work and converted into ceramics by thermal debinding and sintering. The high-entropy perovskite-type oxides are produced at 1500 °C, they retain the printed geometry with high shape fidelity. The orthorhombic crystal structure is identified by the Rietveld refinement of high-resolution synchrotron X-ray data; elemental and spectroscopic characterizations suggest the composition Sr(Ti0.22Zr0.22Hf0.23Mn0.15Sn0.18)O2.85. The use of aqueous polyethylene glycol as a binder and porogen greatly reduces the formation of cracks and creates evenly distributed micropores, which leads to improved compressive strength of the specimens. The compressive strength of 0.94 MPa is highest for materials printed from the resins with 3 wt% PEG in the woodpile-like geometries.

Conditional generative adversarial networks for stripe artefact removal in high-resolution X-ray tomography

Tomographic imaging supports a great number of medical and material science applications. The collected projection data usually has different types of imaging artefacts and noise. Various image pre-processing and reconstruction methods are used to obtain volumetric datasets of high quality for further analysis. In order to minimise reconstruction artefacts, one can apply either filtering and/or data completion/inpainting techniques which can recover the data. Deep learning (DL) methods to remove artefacts and noise have been successfully applied in the past. In this paper, we present a novel approach based on conditional generative adversarial networks (cGANs) to remove stripe artefacts. The novelty of the presented technique is in how the training data for DL is extracted from the same tomographic dataset that needs recovery. We also provide new deterministic stripe detection and inpainting algorithms to support the development. The presented methods are compared with other stripe removal algorithms and applied to 3D and 4D high-resolution X-ray data collected at Diamond Light Source synchrotron, UK. The proposed DL method delivers reconstructed images with minimised ring artefacts while being a parameter-free approach. A similar DL strategy can also be applied to remove other types of artefacts in images.

Enhancing hydrogen positions in X-ray structures of transition metal hydride complexes with dynamic quantum crystallography.

Hirshfeld atom refinement (HAR) is a method which enables the user to obtain more accurate positions of hydrogen atoms bonded to light chemical elements using X-ray data. When data quality permits, this method can be extended to hydrogen-bonded transition metals (TMs), as in hydride complexes. However, addressing hydrogen thermal motions with HAR, particularly in TM hydrides, presents a challenge. At the same time, proper description of thermal vibrations can be vital for determining hydrogen positions correctly. In this study, we employ tools such as SHADE3 and Normal Mode Refinement (NoMoRe) to estimate anisotropic displacement parameters (ADPs) for hydrogen atoms during HAR and IAM refinements performed for seven structures of TM (Fe, Ni, Cr, Nb, Rh and Os) and metalloid (Sb) hydride complexes for which both the neutron and the X-ray structures have been determined. A direct comparison between neutron and HAR/SHADE3/NoMoRe ADPs reveals that the similarity between neutron hydrogen ADPs and those estimated with NoMoRe or SHADE3 is significantly higher than when hydrogen ADPs are refined with HAR. Regarding TM-H bond lengths, traditional HAR exhibits a slight advantage over the other methods. However, combining NoMoRe/SHADE3 with HAR results in a minor decrease in agreement with neutron TM-H bond lengths. For the Cr complex, for which high-resolution X-ray data were collected, an investigation of resolution-related effects was possible.

Quantifying weak interactions in ferroelectric and paraelectric phases of phenazine and chloroanilic acid co-crystal using experimental and theoretical electron densities.

The co-crystal of phenazine and chloroanilic acid is known to display paraelectric properties at room temperature. It shows a paraelectric to ferroelectric phase transition at 253 K and has an incommensurately modulated ferroelectric phase below 137 K. High-resolution synchrotron X-ray data were collected at 160 K to model the experimental electron-density distributions, and derived topological properties from the electron density were used to quantify the weak interactions responsible for the origin of the ferroelectric phase. The structure and non-covalent interactions are analysed using Hirshfeld surfaces and energy frameworks. The topological properties, energies, atomic charges and molecular electrostatic potential surfaces are determined from the experimental data, further supported by theoretical calculations. The results from the ferroelectric phase are compared with the paraelectric phase. Although the structural descriptions indicate neutral phenazine and chloroanilic acid molecules in the ferroelectric phase, the topological properties of the electron density indicate a considerable amount of proton transfer in the O-H...O hydrogen bond. Indeed, the displaced H atom in the O-H...O hydrogen bond suggests a mixed covalent/polar nature of chemical bonding. Subtle changes in the chemical bonding and proton-transfer pathways could be detected from the high-resolution electron-density studies.

Three-dimensional mineral dendrites reveal a nonclassical crystallization pathway

Abstract Manganese (Mn) dendrites are a common type of mineral dendrite that typically forms two-dimensional structures on rock surfaces. Three-dimensional (3-D) Mn dendrites in rocks have rarely been reported, and so their growth implications have largely escaped attention. Here, we combined high-resolution X-ray and electron-based data with numerical modeling to give the first detailed description of natural 3-D Mn dendrites (in clinoptilolite tuffs) and elucidate their growth dynamics. Our data show that 3-D dendrite growth occurred by accretion of Mn-oxide nanoparticles formed when Mn-bearing fluids mixed with oxygenated pore water. The geometry of the resulting structures is sensitive to ion concentrations, the volume of infiltrating fluid, and the number of fluid pulses; thus, 3-D dendrites record the hydrogeochemical rock history.

Structure of the gel phase of diC22:1PC lipid bilayers determined by x-ray diffraction

High-resolution x-ray data are reported for the ordered phases of long-chain di-monounsaturated C22:1 phosphocholine lipid bilayers. Similar to PC lipids that have saturated chains, diC22:1PC has a subgel phase and a gel phase, but dissimilarly, we find no ripple phase. Our quantitative focus is on the structure of the gel phase. We have recorded 17 lamellar orders, indicating a very well-ordered structure. Fitting to a model provides the phases of the orders. The Fourier construction of the electron density profile has two well-defined headgroup peaks and a very sharp and deep methyl trough. The wide-angle scattering exhibits two Bragg rods that provide the area per molecule. They have an intensity pattern quite different than that of lipids with saturated chains. Models of chain packing indicate that ground state chain configurations are tilted primarily toward next nearest neighbors with an angle that is also consistent with the modeling of the electron density profile. Wide-angle modeling also indicates broken mirror symmetry between the monolayers. Our wide-angle results and our electron density profile together leads to the hypothesis that the sn-1 and sn-2 chains have equivalent penetration depths in contrast to the gel phase structure of lipids with saturated hydrocarbon chains.

Experimental X-ray Charge-Density Studies─A Suitable Probe for Superconductivity? A Case Study on MgB2.

Case studies of 1T-TiSe2 and YBa2Cu3O7-δ have demonstrated that X-ray diffraction (XRD) studies can be used to trace even subtle structural phase transitions which are inherently connected with the onset of superconductivity in these benchmark systems. However, the utility of XRD in the investigation of superconductors like MgB2 lacking an additional symmetry-breaking structural phase transition is not immediately evident. Nevertheless, high-resolution powder XRD experiments on MgB2 in combination with maximum entropy method analyses hinted at differences between the electron density distributions at room temperature and 15 K, that is, below the Tc of approx. 39 K. The high-resolution single-crystal XRD experiments in combination with multipolar refinements presented here can reproduce these results but show that the observed temperature-dependent density changes are almost entirely due to a decrease of atomic displacement parameters as a natural consequence of a reduced thermal vibration amplitude with decreasing temperature. Our investigations also shed new light on the presence or absence of magnesium vacancies in MgB2 samples─a defect type claimed to control the superconducting properties of the compound. We propose that previous reports on the tendency of MgB2 to form non-stoichiometric Mg1-xB2 phases (1 - x ∼ 0.95) during high-temperature (HT) synthesis might result from the interpretation of XRD data of insufficient resolution and/or usage of inflexible refinement models. Indeed, advanced refinements based on an Extended Hansen-Coppens multipolar model and high-resolution X-ray data, which consider explicitly the contraction of core and valence shells of the magnesium cations, do not provide any significant evidence for the formation of non-stoichiometric Mg1-xB2 phases during HT synthesis.

Unveiling the Merger Dynamics of the Most Massive MaDCoWS Cluster at z = 1.2 from a Multiwavelength Mapping of Its Intracluster Medium Properties

Abstract The characterization of the Intracluster Medium (ICM) properties of high-redshift galaxy clusters is fundamental to our understanding of large-scale structure formation processes. We present the results of a multiwavelength analysis of the very massive cluster MOO J1142+1527 at a redshift z = 1.2 discovered as part of the Massive and Distant Clusters of WISE Survey. This analysis is based on high angular resolution Chandra X-ray and NIKA2 Sunyaev–Zel’dovich (SZ) data. The cluster thermodynamic radial profiles have been obtained with unprecedented precision at this redshift and up to 0.7R 500, thanks to the combination of high-resolution X-ray and SZ data. The comparison between the galaxy distribution mapped in infrared by Spitzer and the morphological properties of the ICM derived from the combined analysis of the Chandra and NIKA2 data leads us to the conclusion that the cluster is an ongoing merger. We have estimated a systematic uncertainty on the cluster total mass that characterizes both the impact of the observed deviations from spherical symmetry and of the core dynamics on the mass profile. We further combine the X-ray and SZ data at the pixel level to obtain maps of the temperature and entropy distributions. We find a relatively low-entropy core at the position of the X-ray peak and high-temperature regions located on its south and west sides. This work demonstrates that the addition of spatially resolved SZ observations to low signal-to-noise X-ray data brings a high information gain on the characterization of the evolution of ICM thermodynamic properties at z > 1.

Hot WHIM counterparts of FUV O VI absorbers: Evidence in the line-of-sight towards quasar 3C 273

Aims. We explore the high spectral resolution X-ray data towards the quasar 3C 273 to search for signals of hot (∼106−7 K) X-ray-absorbing gas co-located with two established intergalactic far-ultraviolet (FUV) O VI absorbers. Methods. We analyze the soft X-ray band grating data of all XMM-Newton and Chandra instruments to search for the hot phase absorption lines at the FUV predicted redshifts. The viability of potential line detections is examined by adopting the constraints of a physically justified absorption model. The WHIM hypothesis is investigated with a complementary 3D galaxy distribution analysis and by detailed comparison of the measurement results to the WHIM properties in the EAGLE cosmological, hydrodynamical simulation. Results. At one of the examined FUV redshifts, z = 0.09017 ± 0.00003, we measured signals of two hot ion species, O VIII and Ne IX, with a 3.9σ combined significance level. While the absorption signal is only marginally detected in individual co-added spectra, considering the line features in all instruments collectively and assuming collisional equilibrium for absorbing gas, we were able to constrain the temperature (kT = 0.26 ± 0.03 keV) and the column density (NH × Z⊙/Z = 1.3−0.5+0.6 × 1019 cm−2) of the absorber. Thermal analysis indicates that FUV and X-ray absorption relate to different phases, with estimated temperatures, TFUV ≈ 3 × 105, and, TX − ray ≈ 3 × 106 K. These temperatures match the EAGLE predictions for WHIM at the FUV/X-ray measured Nion-ranges. We detected a large scale galactic filament crossing the sight-line at the redshift of the absorption, linking the absorption to this structure. Conclusions. This study provides observational insights into co-existing warm and hot gas within a WHIM filament and estimates the ratio of the hot and warm phases. Because the hot phase is thermally distinct from the O VI gas, the estimated baryon content of the absorber is increased, conveying the promise of X-ray follow-up studies of FUV detected WHIM in refining the picture of the missing baryons.

Comparison of different strategies for modelling hydrogen atoms in charge-density analyses

The quality of various approximation methods for modelling anisotropic displacement parameters (ADPs) for hydrogen atoms was investigated in a comparative study. A multipole refinement was performed against high-resolution single crystal X-ray data of 9-diphenylthiophosphoranylanthracene (SPAnH) and 9,10-bis-diphenylthiophosphoranylanthracene·toluene (SPAnPS). Hydrogen-atom parameters and structural properties derived from our collected neutron data sets were compared with those obtained from the SHADE-server, the software APD-Toolkit based on the invariom database, the results from Hirshfeld atom refinement conducted in the OLEX2 GUI (HARt), and the results of anisotropic hydrogen refinement within XD2016. Additionally, a free refinement of H-atom positions against X-ray data was performed with fixed ADPs from various methods. The resulting C-H bond distances were compared with distances from neutron diffraction experiments and the HARt results. Surprisingly, the refinement of anisotropic hydrogen displacement parameters against the X-ray data yielded the smallest deviations from the neutron values. However, the refinement of bond-directed quadrupole parameters turned out to be vital for the quality of the resulting ADPs. In both model structures, SHADE and, to a lesser extent, APD-Toolkit showed problems in dealing with atoms bonded to carbon atoms with refined Gram-Charlier parameters for anharmonic motion. The HARt method yields the most accurate C-H bond distances compared to neutron data results. Unconstrained refinement of hydrogen atom positions using ADPs derived from all other used approximation methods showed that even with well approximated hydrogen ADPs, the resulting distances were still significantly underestimated.

What Shapes the Absorption Measure Distribution in AGN Outflows?

The Absorption Measure Distribution (AMD) in the X-ray outflows of Seyfert active galactic nuclei (AGN) describes the distribution of absorbing column density as a function of ionization parameter. Up to now, AMD has been measured only for seven objects with high-resolution X-ray data that contain absorption lines from ionized heavy elements. Even though the number of measured AMDs is not large, they display a universal broad shape containing a prominent dip, for which the absorbing column drops by around two orders of magnitude. In this paper, we tested a range of photoionization models against the overall shape of the AMD as observed in Seyferts. In particular, we demonstrate that the shape of the AMD depends both on the spectral energy distribution (SED) of radiation which enters the outflow, and the density of the warm absorber (WA). The model that best reproduces the observed shape of the AMD is one wherein the gas density of the WA is of the order of $10^{12}$ cm$^{-3}$, irradiated by an SED whose optical/UV luminosity is 100 times higher than the X-ray luminosity. When the cloud density is higher than $\sim 10^{11}$ cm$^{-3}$, free-free heating dominates the entire absorber, and only one instability zone occurs, which is in agreement with observations.

Energetics of interactions in the solid state of 2-hydroxy-8-X-quinoline derivatives (X = Cl, Br, I, S-Ph): comparison of Hirshfeld atom, X-ray wavefunction and multipole refinements.

In this work, two methods of high-resolution X-ray data refinement: multipole refinement (MM) and Hirshfeld atom refinement (HAR) - together with X-ray wavefunction refinement (XWR) - are applied to investigate the refinement of positions and anisotropic thermal motion of hydrogen atoms, experiment-based reconstruction of electron density, refinement of anharmonic thermal vibrations, as well as the effects of excluding the weakest reflections in the refinement. The study is based on X-ray data sets of varying quality collected for the crystals of four quinoline derivatives with Cl, Br, I atoms and the -S-Ph group as substituents. Energetic investigations are performed, comprising the calculation of the energy of intermolecular interactions, cohesive and geometrical relaxation energy. The results obtained for experimentally derived structures are verified against the values calculated for structures optimized using dispersion-corrected periodic density functional theory. For the high-quality data sets (the Cl and -S-Ph compounds), both MM and XWR could be successfully used to refine the atomic displacement parameters and the positions of hydrogen atoms; however, the bond lengths obtained with XWR were more precise and closer to the theoretical values. In the application to the more challenging data sets (the Br and I compounds), only XWR enabled free refinement of hydrogen atom geometrical parameters, nevertheless, the results clearly showed poor data quality. For both refinement methods, the energy values (intermolecular interactions, cohesive and relaxation) calculated for the experimental structures were in similar agreement with the values associated with the optimized structures - the most significant divergences were observed when experimental geometries were biased by poor data quality. XWR was found to be more robust in avoiding incorrect distortions of the reconstructed electron density as a result of data quality issues. Based on the problem of anharmonic thermal motion refinement, this study reveals that for the most correct interpretation of the obtained results, it is necessary to use the complete data set, including the weak reflections in order to draw conclusions.

The synthesis and preliminary cytotoxicity evaluation of hexahydrodispiro[indole-3,3′-indolizine-2′,3″-piperidine]-2(1H),4″-dione compounds

Seven hexahydrodispiro[indole-3,3′-indolizine-2′,3″-piperidine]-2(1 H),4″-dione compounds were synthesized by a catalyst-free 1,3-dipolar cycloaddition reaction in a one-pot three-component system containing 3,5-diarylidene-1-benzylpiperidin-4-one, isatin and l-pipecolic acid. The structures of these compounds were characterized by nuclear magnetic resonance, high-resolution mass spectrometry and X-ray data analysis. These chemical entities were evaluated for their cytotoxicity (brine shrimp assay), and five compounds were found potential in this bioassay. Compound 2e was the most prominent target against Artemia salina with an LC50 value of 7.27 μg/mL.

Comparison of different strategies for modelling hydrogen atoms in charge density analyses.

The quality of various approximation methods for modelling anisotropic displacement parameters (ADPs) for hydrogen atoms was investigated in a comparative study. A multipole refinement was performed against high-resolution single crystal X-ray data of 9-diphenylthiophosphoranylanthracene (SPAnH) and 9,10-bis-diphenylthiophosphoranylanthracene·toluene (SPAnPS). Hydrogen-atom parameters and structural properties derived from our collected neutron data sets were compared with those obtained from the SHADE-server, the software APD-Toolkit based on the invariom database, the results from Hirshfeld atom refinement conducted in the OLEX2 GUI (HARt), and the results of anisotropic hydrogen refinement within XD2016. Additionally, a free refinement of H-atom positions against X-ray data was performed with fixed ADPs from various methods. The resulting C-H bond distances were compared with distances from neutron diffraction experiments and the HARt results. Surprisingly, the refinement of anisotropic hydrogen displacement parameters against the X-ray data yielded the smallest deviations from the neutron values. However, the refinement of bond-directed quadrupole parameters turned out to be vital for the quality of the resulting ADPs. In both model structures, SHADE and, to a lesser extent, APD-Toolkit showed problems in dealing with atoms bonded to carbon atoms with refined Gram-Charlier parameters for anharmonic motion. The HARt method yields the most accurate C-H bond distances compared to neutron data results. Unconstrained refinement of hydrogen atom positions using ADPs derived from all other used approximation methods showed that even with well approximated hydrogen ADPs, the resulting distances were still significantly underestimated.

Determination of the miscibility gap in the solid solutions series of methylammonium lead iodide/chloride.

Perovskites are widely known for their enormous possibility of elemental substitution, which leads to a large variety of physical properties. Hybrid perovskites such as CH3NH3PbI3 (MAPbI3) and CH3NH3PbCl3 (MAPbCl3) are perovskites with an A[XII]B[VI]X[II]3-structure, where A is an organic molecule, B is a lead(II) cation and X is a halide anion of iodine or chlorine. Whereas MAPbCl3 crystallizes in the cubic space group Pm{\overline 3}m, MAPbI3 is in the tetragonal space group I4/mcm. The substitution of I by Cl leads to an increased tolerance against humidity but is challenging or even impossible due to their large difference in ionic radii. Here, the influence of an increasing Cl content in the reaction solution on the miscibility of the solid solution members is examined systematically. Powders were synthesized by two different routes depending on the I:Cl ratio. High-resolution synchrotron X-ray data are used to establish values for the limits of the miscibility gap which are 3.1 (1.1) mol% MAPbCl3 in MAPI and 1.0 (1) mol% MAPbI3 in MAPCl. The establishment of relations between average pseudo-cubic lattice parameters for both phases allows a determination of the degree of substitution from the observed lattice parameters.

Investigating the Many Roles of Internal Water in Cytochrome c Oxidase.

Cytochrome c oxidase (C cO) is the terminal enzyme in the respiratory electron transport chain. As part of its catalytic cycle, C cO transfers protons to its Fe-Cu binuclear center (BNC) to reduce oxygen, and in addition, it pumps protons across the mitochondrial inner, or bacterial, membrane where it is located. It is believed that this proton transport is facilitated by a network of water chains inside the enzyme. Here we present an analysis of the hydration of C cO, including the BNC region, using a semi-empirical hydration program, Dowser++, recently developed in our group. Using high-resolution X-ray data, we show that Dowser++ predictions match very accurately the water molecules seen in the D- and K-channels of C cO, as well as in the vicinity of its BNC. Moreover, Dowser++ predicts many more internal water molecules than is typically seen in the experiment. However, no significant hydration of the catalytic cavity in C cO described recently in the literature is observed. As Dowser++ itself does not account for structural changes of the protein, this result supports the earlier assessment that the proposed wetting transition in the catalytic cavity can only either be due to structural rearrangements of BNC, possibly induced by the charges during the catalytic cycle, or occur transiently, in concert with the proton transfer. Molecular dynamics simulations were performed to investigate the global dynamic nature of Dowser++ waters in C cO, and the results suggest a consistent explanation as to why some predicted water molecules would be missing in the experimental structures. Furthermore, in light of the significant protein hydration predicted by Dowser++, the dielectric constant of the hydrated cavities in C cO was also investigated using the Fröhlich-Kirkwood model; the results indicate that in the cavities where water is packed sufficiently densely the dielectric constant can approach values comparable even to that of bulk water.

Infrared and X-ray study of the Galactic SNR G15.9+0.2

G15.9+0.2 is a Galactic shell-type supernova remnant (SNR), which was detected in radio and has been confirmed in X-rays based on Chandra observations. An X-ray point source CXOUJ181852.0-150213 has been detected and suggested to be an associated neutron star. In a recent study, we have confirmed the source to be a central compact object (CCO). We have studied the SNR using high-resolution X-ray data taken with Chandra in combination with infrared (IR) data in order to understand its emission and to derive its physical parameters. This will also help to constrain, e.g., the age of the CCO and the environment in which it was born. The spectral analysis of the X-ray emission using the new Chandra data and the comparison to the IR data have shown that the SNR is relatively young with an age of a few thousand years and that its emission is dominated by that of shocked interstellar medium (ISM). However, the analysis of the spectrum of the bright eastern shell shows that there is an additional emission component with enhanced abundances of {\alpha} elements and Fe, suggesting ejecta emission. The multi-wavelength emission is consistent with SNR G15.9+0.2 expanding in an ISM with a density gradient, while there is also colder material located in front of the SNR, which absorbs its thermal X-ray emission in the softer bands.

Using cryo-electron microscopy maps for X-ray structure determination.

X-ray crystallography and cryo-electron microscopy (cryo-EM) are complementary techniques for structure determination. Crystallography usually reveals more detailed information, while cryo-EM is an extremely useful technique for studying large-sized macromolecules. As the gap between the resolution of crystallography and cryo-EM data narrows, the cryo-EM map of a macromolecule could serve as an initial model to solve the phase problem of crystal diffraction for high-resolution structure determination. FSEARCH is a procedure to utilize the low-resolution molecular shape for crystallographic phasing. The IPCAS (Iterative Protein Crystal structure Automatic Solution) pipeline is an automatic direct-methods-aided dual-space iterative phasing and model-building procedure. When only an electron-density map is available as the starting point, IPCAS is capable of generating a completed model from the phases of the input map automatically, without the requirement of an initial model. In this study, a hybrid method integrating X-ray crystallography with cryo-EM to help with structure determination is presented. With a cryo-EM map as the starting point, the workflow of the method involves three steps. (1) Cryo-EM map replacement: FSEARCH is utilized to find the correct translation and orientation of the cryo-EM map in the crystallographic unit cell and generates the initial low-resolution map. (2) Phase extension: the phases calculated from the correctly placed cryo-EM map are extended to high-resolution X-ray data by non-crystallographic symmetry averaging with phenix.resolve. (3) Model building: IPCAS is used to generate an initial model using the phase-extended map and perform model completion by iteration. Four cases (the lowest cryo-EM map resolution being 6.9 Å) have been tested for the general applicability of the hybrid method, and almost complete models have been generated for all test cases with reasonable Rwork/Rfree. The hybrid method therefore provides an automated tool for X-ray structure determination using a cryo-EM map as the starting point.

Improved Purification and Crystal Formation of Native Muscle-Type nAChR Using mAbs

The nicotinic acetylcholine receptors (nAChR) are part of the Cys-loop ligand-gated ion channel family and one of the most widely studied, but their molecular structure is still unknown. These receptors are important as the biological target for the development of therapies for a great number of diseases, including Myasthenia gravis, Parkinson's disease, and nicotine addiction. Our aim is to obtain high-quality protein crystals and determine the structure of the native nAChR via X-ray crystallography. We extracted muscle-type nAChRs from the tissue of Torpedo californica, using LFC-16 as a detergent, followed by several steps of purification. Four monoclonal antibodies (mAbs) with a high affinity against the receptor and the impurities were assayed via western blot, and BioLayer interferometry on the Octet platform for kinetic characterization. One of these mAbs yielded a KD <10−12 which suggests strong mAbs-nAChR interactions with no dissociation occurring. Furthermore, we developed a method of immunodepletion to remove impurities from the nAChR-detergent complex, increasing sample purity. Fluorescence recovery after photobleaching (FRAP) assays displayed a lower mobile fraction with mAbs incorporation compared to control, suggesting significant protein-protein interactions. Our next goal is to identify by western blot and protein fingerprinting which proteins are identified by the mAbs. These mAbs will be used to obtain high-quality nAChR crystals and also high-resolution X-ray data. This research was supported by the NIH NIGMS grants 1R01GM098343 (JALD); COBRE NIEF 1P20GM103642 (J.R and JALD) and Research Initiative for Scientific Enhancement (RISE) program.

Chandra and ALMA observations of the nuclear activity in two strongly lensed star-forming galaxies

Aim. According to coevolutionary scenarios, nuclear activity and star formation play relevant roles in the early stages of galaxy formation. We aim at identifying them in high-redshift galaxies by exploiting high-resolution and high-sensitivity X-ray and millimeter-wavelength data to confirm the presence or absence of star formation and nuclear activity and describe their relative roles in shaping the spectral energy distributions and in contributing to the energy budgets of the galaxies. Methods. We present the data, model, and analysis in the X-ray and millimeter (mm) bands for two strongly lensed galaxies, SDP.9 (HATLAS J090740.0-004200) and SDP.11 (HATLAS J091043.1-000322), which we selected in the Herschel-ATLAS catalogs for their excess emission in the mid-IR regime at redshift ≳1.5. This emission suggests nuclear activity in the early stages of galaxy formation. We observed both of them with Chandra ACIS-S in the X-ray regime and analyzed the high-resolution mm data that are available in the ALMA Science Archive for SDP.9. By combining the information available in mm, optical, and X-ray bands, we reconstructed the source morphology. Results. Both targets were detected in the X-ray, which strongly indicates highly obscured nuclear activity. ALMA observations for SDP.9 for the continuum and CO(6-5) spectral line with high resolution (0.02 arcsec corresponding to ~65 pc at the distance of the galaxy) allowed us to estimate the lensed galaxy redshift to a better accuracy than pre-ALMA estimates (1.5753 ± 0.0003) and to model the emission of the optical, millimetric, and X-ray band for this galaxy. We demonstrate that the X-ray emission is generated in the nuclear environment, which strongly supports that this object has nuclear activity. On the basis of the X-ray data, we attempt an estimate of the black hole properties in these galaxies. Conclusions. By taking advantage of the lensing magnification, we identify weak nuclear activity associated with high-z galaxies with high star formation rates. This is useful to extend the investigation of the relationship between star formation and nuclear activity to two intrinsically less luminous high-z star-forming galaxies than was possible so far. Given our results for only two objects, they alone cannot constrain the evolutionary models, but provide us with interesting hints and set an observational path toward addressing the role of star formation and nuclear activity in forming galaxies.