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At least 757 records · Page 42

Redox manipulation of the manganese metal in human manganese superoxide dismutase for neutron diffraction

Human manganese superoxide dismutase (MnSOD) is one of the most significant enzymes in preventing mitochondrial dysfunction and related diseases by combating reactive oxygen species (ROS) in the mitochondrial matrix. Mitochondria are the source of up to 90% of cellular ROS generation, and MnSOD performs its necessary bioprotective role by converting superoxide into oxygen and hydrogen peroxide. This vital catalytic function is conducted via cyclic redox reactions between the substrate and the active-site manganese using proton-coupled electron transfers. Owing to protons being difficult to detect experimentally, the series of proton transfers that compose the catalytic mechanism of MnSOD are unknown. Here, methods are described to discern the proton-based mechanism using chemical treatments to control the redox state of large perdeuterated MnSOD crystals and subsequent neutron diffraction. These methods could be applicable to other crystal systems in which proton information on the molecule in question in specific chemical states is desired.

Azadmanesh, Jahaun↗

Crystal structures of polymerized lithium chloride and dimethyl sulfoxide in the form of {2LiCl·3DMSO} n and {LiCl·DMSO} n

Two novel LiCl·DMSO polymer structures were created by combining dry LiCl salt with dimethyl sulfoxide (DMSO), namely, catena-poly[[chlorido­lithium(I)]-μ-(dimethyl sulfoxide)-κ 2 O:O-[chlorido­lithium(I)]-di-μ-(dimethyl sulfoxide)-κ 4 O:O], [Li 2 Cl 2 (C 2 H 6 OS) 3 ]n, and catena-poly[lithium(I)-μ-chlorido-μ-(dimethyl sulfoxide)-κ 2 O:O], [LiCl(C 2 H 6 OS)]n. The initial synthesized phase had very small block-shaped crystals (<0.08 mm) with monoclinic symmetry and a 2 LiCl: 3 DMSO ratio. As the solution evaporated, a second phase formed with a plate-shaped crystal morphology. After about 20 minutes, large (>0.20 mm) octa­hedron-shaped crystals formed. The plate crystals and the octa­hedron crystals are the same tetra­gonal structure with a 1 LiCl: 1 DMSO ratio. These structures are reported and compared to other known LiCl·solvent compounds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Challenges in solving structures from radiation-damaged tomograms of protein nanocrystals assessed by simulation

Structure-determination methods are needed to resolve the atomic details that underlie protein function. X-ray crystallography has provided most of our knowledge of protein structure, but is constrained by the need for large, well ordered crystals and the loss of phase information. The rapidly developing methods of serial femtosecond crystallography, micro-electron diffraction and single-particle reconstruction circumvent the first of these limitations by enabling data collection from nanocrystals or purified proteins. However, the first two methods also suffer from the phase problem, while many proteins fall below the molecular-weight threshold required for single-particle reconstruction. Cryo-electron tomography of protein nanocrystals has the potential to overcome these obstacles of mainstream structure-determination methods. Here, a data-processing scheme is presented that combines routines from X-ray crystallography and new algorithms that have been developed to solve structures from tomograms of nanocrystals. This pipeline handles image-processing challenges specific to tomographic sampling of periodic specimens and is validated using simulated crystals. The tolerance of this workflow to the effects of radiation damage is also assessed. The simulations indicate a trade-off between a wider tilt range to facilitate merging data from multiple tomograms and a smaller tilt increment to improve phase accuracy. Since phase errors, but not merging errors, can be overcome with additional data sets, these results recommend distributing the dose over a wide angular range rather than using a finer sampling interval to solve the protein structure.

59 BASIC BIOLOGICAL SCIENCES↗

Understanding Function and Performance of Carbon Additives in Lead-Acid Batteries

While the low cost and strong safety record of lead-acid batteries make them an appealing option compared to lithium-ion technologies for stationary storage, they can be rapidly degraded by the extended periods of high rate, partial state-of-charge operation required in such applications. Degradation occurs primarily through a process called hard sulfation, where large PbSO 4 crystals are formed on the negative battery plates, hindering charge acceptance and reducing battery capacity. Various researchers have found that the addition of some forms of excess carbon to the negative active mass in lead-acid batteries can mitigate hard sulfation, but the mechanism through which this is accomplished is unclear. In this work, the effect of carbon composition and morphology was explored by characterizing four discrete types of carbon additives, then evaluating their effect when added to the negative electrodes within a traditional valve-regulated lead-acid battery design. The cycle life for the carbon modified cells was significantly larger than an unmodified control, with cells containing a mixture of graphitic carbon and carbon black yielding the greatest improvement. The carbons also impacted other electrochemical aspects of the battery (e.g., float current, capacity, etc.) as well as physical characteristics of the negative active mass, such as the specific surface area.

25 ENERGY STORAGE↗

Czochralski Growth of Indium Iodide and other Wide Bandgap Semiconductor Compounds

The Czochralski pulling process is the most valuable and cost efficient method for producing large oriented single crystals of the group IV and III-V semiconductors. However, there have been only a small number of reported attempts to use the Czochralski process for growing the wide bandgap compound semiconductors, needed for the room temperature operated gamma-ray detectors. The main difficulty is in the low chemical stability and high vapor pressure of the group II, V and VI elements, leading to off-stoichiometric composition, and various related defects. Among the heavy metal halides, indium iodide and indium bromide present an interesting exception. InI has a high molecular disassociation energy and a low vapor pressure, allowing for Czochralski pulling. Finally, we will describe the procedures used and the results obtained by Czochralski growth and characterization of indium iodide and the related ternary compounds that appear to be quite encouraging.

36 MATERIALS SCIENCE↗

Measurement of the energy and time resolution of a undoped CsI + MPPC array for the Mu2e experiment

This paper describes the measurements of energy and time response and resolution of a 3 x 3 array made of undoped CsI crystals coupled to large area Hamamatsu Multi Pixel Photon Counters. The measurements have been performed using the electron beam of the Beam Test Facility in Frascati (Rome, Italy) in the energy range 80-120 MeV. The measured energy resolution, estimated with the FWHM, at 100 MeV is 16.4%. This resolution is dominated by the energy leakage due to the small dimensions of the prototype. The time is reconstructed by fitting the leading edge of the digitized signals and applying a digital constant fraction discrimination technique. A time resolution of about 110 ps at 100 MeV is achieved.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Stilbene Scintillator Detector Array and Data-Acquisition System for Active Interrogation

A large area Stilbene crystal detector array has been assembled and calibrated for use in active interrogation measurements. The array consists of 10 high-efficiency 4”x2” stilbene cells. The cells were grown by Inrad Optics using LLNL developed technology. The array can be used to detect multiple signatures of SNM items, both actively and passively. Prompt and delayed gamma rays as well as prompt and delay neutrons can be detected and counted separately. The array is coupled to the Mesytec MDPP-16 VME-based digitizer module for data acquisition. This module performs on-board pulse-shape discrimination of signals from the Stilbene crystal detectors. This data-acquisition module allows separation of neutron and gamma-ray events with a low demand on data transfer rates. In addition, the high-resolution timing (<100 ps) is suitable for correlated gamma-ray and neutron multiplicity counting. This report describes the construction and calibration of the system. We also discuss applications of the system as well as how the system is currently being utilized by end users.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

Synthesis and Observation of Emergent Phenomena in Epitaxial Heusler Compound Heterostructures

The proposal was on the synthesis and observation of emergent phenomena in epitaxial Heusler compound heterostructures. The large range of properties and number of Heusler compounds opens up a wide number of potential compounds that will exhibit emergent phenomena. The similarity, large range of relatively inexpensive, large area, high crystal quality, III-V bulk substrates, lattice parameters and the ability to tune the lattice parameters through ternary or quaternary III-V compound semiconductor epitaxial growth, makes III-V semiconductors an ideal choice for substrates for epitaxial growth of Heusler compounds. A number of half Heusler compounds have been predicted to exhibit band inversion, making them topological and are therefore expected to exhibit spin-momentum locked topological surface states with linear dispersion. Others are predicted to be semimetals with Weyl points and others semiconducting and magnetic. During the course of this grant, emphasis has been on investigating Heusler compounds with emergent phenomena and demonstrating the ability to tune their properties through alloying and strain. We have grown toplogical semimetal (PtLuSb, PtMnBi), Weyl (Co 2 MnAl, Co 2 TiGe), half metal (PtMnSb, Co 2 MnSi, Co 2 MnAl x Si 1-x , Co2FeAl), and semiconducting (CoTiSb, NiTiSn) and tuned their properties through alloying and epitaxial strain. We also investigated the closely related materials of rare-earth monopnictide, some of which have also been predicted to be topological. During the attempts to grow the PtMnBi, it was discovered that Bi, another predicted topological material when ultrathin, could be grown epitaxially on InSb, results for which are also reported here. The main focus for this effort has been on using variable photon energy and spin-dependent angle resolved photoemission (ARPES) to determine bulk band structure and surface states of pristine epitaxial films grown on III-V semiconductor and MgO substrates and correlate results with theory and transport measurements. Theory has been critical to interpretation of experimental results and has been essential in guiding experiments. The research benefited from several strong collaborations between the PIs and the beamline scientists at the Advanced Light Source at Lawrence Berkeley Laboratory, the Stanford Linear Accelerator Center (SLAC) at Stanford and at the Max Lab at Lund University in Sweden. The strong experiment - theory collaboration between the PI’s groups, the Palmstrøm group at UCSB and the Janotti group at the University of Delaware, has been critical for interpreting the experimental ARPES and magnetotransport measurements results and making predictions to guide experiments. Weekly interactive Zoom meetings made this work well. A collaboration between the Palmstrøm group and Dr. Alexei Fedorov at the Advanced Light Source (ALS) resulted in significant modifications to his end chamber to accommodate the vacuum suitcase that was designed and constructed in the Palmstrøm group at UCSB. In collaboration with beamline scientists, Drs. Makoto Hashimoto and Donghui Lu at SLAC, Palmstrøm made modifications to the vacuum suitcase and developed special sample holders that allowed samples to be grown in the Palmstrøm MBE systems at UCSB and transported in the UHV vacuum suitcase to SLAC for ARPES measurements. The development of the vacuum suitcase was essential for this grant as it has allowed variable photon energies to be used to identify surface versus bulk states on samples that could not be capped and decapped using As- or Sb-capping layers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

High average current HVDC electron gun for EIC hadron cooling

A critical R&D initiative for the Electron Ion Collider (EIC) involves the design of an electron gun capable of gen erating a high average current and high-brightness electron beam for the hadron cooler. This is essential to preserve hadron beam quality and achieve the collider’s luminosity target of 1 × 10 34 s −1 cm −2 . For an energy recovery linac (ERL)-based hadron cooler, the gun must deliver a high average current of 98.5 mA, a normalized transverse emittance of less than 2 mm−mrad, and a bunch charge of up to 2.5 nC. This proceeding outlines the high-voltage design of a DC gun operating at 500 kV, with conditioning capability up to 600 kV. The design incorporates several unique fea tures, including the use of inverted ceramic at this voltage level, active cooling for the cathode, and large single-crystal multi-alkali cathodes grown on a silicon carbide substrate. High-brightness electron sources are also pivotal for other ad vanced applications, such as high-intensity gamma sources, future 𝑒 + 𝑒 − colliders, and ultra-deep UV sources for the semiconductor industry. Additionally, this paper provides an overview of the hadron cooling approaches planned or proposed for the EIC.

43 PARTICLE ACCELERATORS↗

Investigation of experimental signatures of spin glass transition temperature

We present a series of temperature and field-dependent magnetization studies of large single-crystal spin glass samples, focusing on both field-cooled (FC) and zero-field-cooled (ZFC) magnetization studies, as well as ac susceptibility measurements. Using the above experimental techniques we aim to understand the nature of spin glass transition in presence of a field, a key factor in understanding the properties of these systems. Building on previous studies that have explored magnetic signatures indicative of spin glass transitions, our research employs a systematic approach to refine the identification of this transition temperature. Through static and dynamic measurements, we aim to shed light on the open issues regarding the key markers of spin glass transitions, enhancing our understanding of these complex systems.

36 MATERIALS SCIENCE↗

Serial Femtosecond X-Ray Diffraction of HIV-1 Gag MA-IP6 Microcrystals at Ambient Temperature

The Human immunodeficiency virus-1 (HIV-1) matrix (MA) domain is involved in the highly regulated assembly process of the virus particles that occur at the host cell’s plasma membrane. High-resolution structures of the MA domain determined using cryo X-ray crystallography have provided initial insights into the possible steps in the viral assembly process. However, these structural studies have relied on large and frozen crystals in order to reduce radiation damage caused by the intense X-rays. Here, we report the first X-ray free-electron laser (XFEL) study of the HIV-1 MA domain’s interaction with inositol hexaphosphate (IP6), a phospholipid headgroup mimic. We also describe the purification, characterization and microcrystallization of two MA crystal forms obtained in the presence of IP6. In addition, we describe the capabilities of serial femtosecond X-ray crystallography (SFX) using an XFEL to elucidate the diffraction data of MA-IP6 complex microcrystals in liquid suspension at ambient temperature. Two different microcrystal forms of the MA-IP6 complex both diffracted to beyond 3.5 Å resolution, demonstrating the feasibility of using SFX to study the complexes of MA domain of HIV-1 Gag polyprotein with IP6 at near-physiological temperatures. Further optimization of the experimental and data analysis procedures will lead to better understanding of the MA domain of HIV-1 Gag and IP6 interaction at high resolution and will provide basis for optimization of the lead compounds for efficient inhibition of the Gag protein recruitment to the plasma membrane prior to virion formation.

59 BASIC BIOLOGICAL SCIENCES↗

FM oscillator uses tetrode transistor

Tetrode-driven crystal oscillator achieves large frequency variations for a given input signal. Frequency control is obtained by variation of the second base current of the tetrode.

Boensel, D. W.↗

Measurements of the spectrum of galactic electrons at very high energies

A counter telescope has been exposed in three balloon flights in 1970 to measure the flux and energy spectrum of cosmic ray electrons between 10 and 1000 GeV. This instrument has been modified by incorporating a large area CsI crystal as well as highly efficient time of flight circuitry, and was flown again twice during 1972. The methods of data analysis are based on extensive accelerator calibrations at SLAC. The resulting electron spectrum fits well to a single power law with an index (gamma) equal to 2.66 over the whole energy region. No obvious steepening can be observed, although statistical uncertainties prohibit definite claims beyond 250 GeV.

Mueller, D.↗

Search for thermal X-ray line emission from the Crab Nebula

Observations of the Crab Nebula from 1.85 to 8 keV obtained with the large-area graphite crystal spectrometer on OSO-8 show a smooth featureless continuum with an absence of X-ray emission lines from highly ionized Si and S. Upper limits on the line emission are used to derive an upper limit to the emission measure for a thermal source associated with the Crab Nebula. Existing evidence for an extended thermal source is discussed, and it is shown that the evidence is not contradicted by the upper limits set with the spectrometer data.

Kestenbaum, H. L.↗

Search for X-ray line emission from Cassiopeia A

The large area graphite crystal spectrometer aboard OSO 8 has been used to search for X-ray line emission from Cas A from ions of Si, S, and Fe over the energy band 1.865 to 8 keV. No evidence was obtained for line emission. The upper limits for the Si and S line fluxes are used to establish upper limits on the abundances of these elements. The limit on the Fe line flux is consistent with the strength of the emission feature reported in proportional counter experiments. Questions of nonequilibrium in ionization in Cas A and the effects on X-ray line emission are considered.

Kestenbaum, H. L.↗

New limits on gamma-ray bursts

Two balloon flights of large-area scintillation crystal detector arrays indicate that the rate of weak gamma-ray bursts is significantly below that expected from a uniform distribution of burst sources. This result, combined with the data from stronger bursts, gives strong evidence for a galactic confinement of burst sources. Reasonable models of confinement limit the intrinsic radiated energy per burst to the order of 10 to the (39th to 41st power) ergs.

Fishman, G. J.↗