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All sourcesNASA NTRSDOE OSTI
NASA NTRS2013

Preparation and Single-Crystal X-Ray Structures of Four Related Mixed-Ligand 4-Methylpyridine Indium Halide Complexes

We describe the structures of four related indium complexes obtained during synthesis of solid-state materials precursors. Indium adducts of halides and 4-methylpyridine, InX3(pic)3 (X = Cl, Br; pic = 4-methylpyridine) consist of octahedral molecules with meridional (mer) geometry. Crystals of mer-InCl3(pic)3 (1) are triclinic, space group P1(bar) (No. 2), with a = 9.3240(3), b = 13.9580(6), c = 16.7268 (7) A, alpha = 84.323(2), beta = 80.938(2), gamma = 78.274(3)Z = 4, R = 0.035 for 8820 unique reflections. Crystals of mer-InBr3(pic)3 (2) are monoclinic, space group P21/n (No. 14), with a = 15.010(2), b = 19.938(2), c = 16.593(3), beta = 116.44(1)Z = 8, R = 0.053 for 4174 unique reflections. The synthesis and structures of related compounds with phenylsulfide (chloride) (3) and a dimeric complex with bridging hydroxide (bromide) (4) coordination is also described. Crystals of trans-In(SC6H5)Cl2(pic)3 (3) are monoclinic, space group P21/n (No. 14), with a = 9.5265(2), b = 17.8729(6), c = 13.8296(4), beta = 99.7640(15)Z = 4, R = 0.048 for 5511 unique reflections. Crystals of [In(mu-OH)Br2(pic)22 (4) are tetragonal, space group = I41cd (No. 110) with a = 19.8560(4), b = 19.8560(4), c = 25.9528(6), Z = 8, R = 0.039 for 5982 unique reflections.

Hepp, Aloysius F.↗
DOE OSTI2019

Structure of lipoprotein lipase in complex with GPIHBP1

Lipoprotein lipase (LPL) plays a central role in triglyceride (TG) metabolism. By catalyzing the hydrolysis of TGs present in TG-rich lipoproteins (TRLs), LPL facilitates TG utilization and regulates circulating TG and TRL concentrations. Until very recently, structural information for LPL was limited to homology models, presumably due to the propensity of LPL to unfold and aggregate. By coexpressing LPL with a soluble variant of its accessory protein glycosylphosphatidylinositol-anchored high-density lipoprotein binding protein 1 (GPIHBP1) and with its chaperone protein lipase maturation factor 1 (LMF1), we obtained a stable and homogenous LPL/GPIHBP1 complex that was suitable for structure determination. We report here X-ray crystal structures of human LPL in complex with human GPIHBP1 at 2.5–3.0 Å resolution, including a structure with a novel inhibitor bound to LPL. Binding of the inhibitor resulted in ordering of the LPL lid and lipid-binding regions and thus enabled determination of the first crystal structure of LPL that includes these important regions of the protein. It was assumed for many years that LPL was only active as a homodimer. The structures and additional biochemical data reported here are consistent with a new report that LPL, in complex with GPIHBP1, can be active as a monomeric 1:1 complex. The crystal structures illuminate the structural basis for LPL-mediated TRL lipolysis as well as LPL stabilization and transport by GPIHBP1.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2018

Streams, cascades, and pools: various water cluster motifs in structurally similar Ni(ii) complexes

Hydrogen bonding (HB) interactions are well known to impact the properties of water in the bulk and within hydrated materials. A series of Ni(II) complexes based on chelates containing N-(2-aminoethyl)-1-methylimidazole-2-carboxamide have been synthesized and fully characterized by single crystal X-ray diffraction, spectroscopic methods, and thermal analysis. The complexes reveal a variety of water cluster motifs dependent on the packing arrangement in the solid state. A key feature is the orientation of the carboxamide moiety, which leads to the formation of void spaces that accommodate water through HB interactions. The water motifs contain 1D water chains (streams), 2D tapes of infused rings (cascades), and isolated water dimers (pools). The HB motifs in the hydrated structures vary as a function of the crystal packing of the host molecules. Thermal analyses show a correlation between the HB motif in the hydrated crystals and the temperature range of the dehydration process. The conductivity of the hydrated crystals varies as a function of the crystal packing interactions between metal complexes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Synthesis of Parent Acetylide and Dicarbide Complexes of Thorium and Uranium and an Examination of Their Electronic Structures

The reaction of [AnCl(NR 2 ) 3 ] (An = U or Th; R = SiMe 3 ) with NaCCH and tetramethylethylenediamine (TMEDA) results in the formation of [An(C≡CH)(NR 2 ) 3 ] (1, An = U; 2, An = Th), which can be isolated in good yields after workup. Similarly, the reaction of 3 equiv of NaCCH and TMEDA with [AnCl(NR 2 ) 3 ] results in the formation of [Na(TMEDA)][An(C≡CH) 2 (NR 2 ) 3 ] (4, An = U; 5, An = Th), which can be isolated in fair yields after workup. The reaction of 1 with 2 equiv of KC 8 and 1 equiv of 2.2.2-cryptand in tetrahydrofuran results in formation of the uranium(III) acetylide complex [K(2.2.2-cryptand)][U(C≡CH)(NR 2 ) 3 ] (3). Thermolysis of 1 or 2 results in formation of the bimetallic dicarbide complexes [{An(NR 2 ) 3 } 2 (μ,η 1 :η 1 -C 2 )] (6, An = U; 7, An = Th), whereas the reaction of 1 with [Th{N(R)(SiMe 2 CH 2 )}(NR 2 ) 2 ] results in the formation of [U(NR 2 ) 3 (μ,η 1 :η 1 -C 2 )Th(NR 2 ) 3 ] (8). The 13 C NMR chemical shifts of the α-acetylide carbon atoms in 2, 5, and 7 exhibit a characteristic spin–orbit-induced downfield shift, due to participation of the 5f orbitals in the Th–C bonds. Furthermore, magnetism measurements demonstrate that 6 displays weak ferromagnetic coupling between the uranium(IV) centers (J = 1.78 cm –1 ).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Preferential Paths of Air-water Two-phase Flow in Porous Structures with Special Consideration of Channel Thickness Effects

Accurate understanding and predicting the flow paths of immiscible two-phase flow in rocky porous structures are of critical importance for the evaluation of oil or gas recovery and prediction of rock slides caused by gas-liquid flow. A 2D phase field model was established for compressible air-water two-phase flow in heterogenous porous structures. The dynamic characteristics of air-water two-phase interface and preferential paths in porous structures were simulated. The factors affecting the path selection of two-phase flow in porous structures were analyzed. Transparent physical models of complex porous structures were prepared using 3D printing technology. Tracer dye was used to visually observe the flow characteristics and path selection in air-water two-phase displacement experiments. The experimental observations agree with the numerical results used to validate the accuracy of phase field model. The effects of channel thickness on the air-water two-phase flow behavior and paths in porous structures were also analyzed. The results indicate that thick channels can induce secondary air flow paths due to the increase in flow resistance; consequently, the flow distribution is different from that in narrow channels. This study provides a new reference for quantitatively analyzing multi-phase flow and predicting the preferential paths of immiscible fluids in porous structures.

42 ENGINEERING↗
NASA NTRS1973

Infrared photography of OH airglow structures.

Results of high-angular-resolution photography of the complex airglow structures present in the infrared sky. The photographs obtained all show bright cloud-like structures which moved on the sky and varied in brightness. It is concluded that these structures are due to varying airglow emission and not to any type of modulation of a uniform background by atmospheric clouds, dust, or haze. It is also concluded that observations of a bright spot from two widely separated sites will yield parallax determinations of the height of the OH emitting layer, so that it is no longer necessary to rely on infrequent rocket measurements at a few places.

Peterson, A. W.↗
NASA NTRS2004

Particle Acceleration and Magnetic Field Generation in Electron-Positron Relativistic Shocks

Shock acceleration is an ubiquitous phenomenon in astrophysical plasmas. Plasma waves and their associated instabilities (e.g., Buneman, Weibel and other two-stream instabilities) created in collisionless shocks are responsible for particle (electron, positron, and ion) acceleration. Using a 3-D relativistic electromagnetic particle (REMP) code, we have investigated particle acceleration associated with a relativistic electron-positron jet front propagating into an ambient electron-positron plasma with and without initial magnetic fields. We find small differences in the results for no ambient and modest ambient magnetic fields. Simulations show that the Weibel instability created in the collisionless shock front accelerates jet and ambient particles both perpendicular and parallel to the jet propagation direction. The non-linear fluctuation amplitudes of densities, currents, electric, and magnetic fields in the electron-positron shock are larger than those found in the electron-ion shock studied in a previous paper. This comes from the fact that both electrons and positrons contribute to generation of the Weibel instability. Additionally, we have performed simulations with different electron skin depths. We find that growth times scale inversely with the plasma frequency, and the sizes of structures created by the Weibel instability scale proportional to the electron skin depth. This is the expected result and indicates that the simulations have sufficient grid resolution. While some Fermi acceleration may occur at the jet front, the majority of electron and positron acceleration takes place behind the jet front and cannot be characterized as Fermi acceleration. The simulation results show that the Weibel instability is responsible for generating and amplifying nonuniform, small-scale magnetic fields which contribute to the electron's (positron's) transverse deflection behind the jet head. This small scale magnetic field structure is appropriate to the generation of "jitter" radiation from deflected electrons (positrons) as opposed to synchrotron radiation. The jitter radiation has different properties than synchrotron radiation calculated assuming a a uniform magnetic field. The jitter radiation resulting from small scale magnetic field structures may be important for understanding the complex time structure and spectral evolution observed in gamma-ray bursts or other astrophysical sources containing relativistic jets and relativistic collisionless shocks.

Nishikawa, K.-I.↗
NASA NTRS2004

Particle Acceleration and Magnetic Field Generation in Electron-Positron Relativistic Shocks

Shock acceleration is an ubiquitous phenomenon in astrophysical plasmas. Plasma waves and their associated instabilities (e.g., Buneman, Weibel and other two-stream instabilities) created in collisionless shocks are responsible for particle (electron, positron, and ion) acceleration. Using a 3-D relativistic electromagnetic particle (REMP) code, we have investigated particle acceleration associated with a relativistic electron-positron jet front propagating into an ambient electron-positron plasma with and without initial magnetic fields. We find small differences in the results for no ambient and modest ambient magnetic fields. Simulations show that the Weibel instability created in the collisionless shock front accelerates jet and ambient particles both perpendicular and parallel to the jet propagation direction. The non-linear fluctuation amplitudes of densities, currents, electric, and magnetic fields in the electron-positron shock are larger than those found in the electron-ion shock studied in a previous paper at the comparable simulation time. This comes from the fact that both electrons and positrons contribute to generation of the Weibel instability. Additionally, we have performed simulations with different electron skin depths. We find that growth times scale inversely with the plasma frequency, and the sizes of structures created by the Weibel instability scale proportional to the electron skin depth. This is the expected result and indicates that the simulations have sufficient grid resolution. While some Fermi acceleration may occur at the jet front, the majority of electron and positron acceleration takes place behind the jet front and cannot be characterized as Fermi acceleration. The simulation results show that the Weibel instability is responsible for generating and amplifying nonuniform: small-scale magnetic fields which contribute to the electron's (positron's) transverse deflection behind the jet head. This small scale magnetic field structure is appropriate to the generation of jitter radiation from deflected electrons (positrons) as opposed to synchrotron radiation. The jitter radiation has different properties than synchrotron radiation calculated assuming a a uniform magnetic field. The jitter radiation resulting from small scale magnetic field structures may be important for understanding the complex time structure and spectral evolution observed in gamma-ray bursts or other astrophysical sources containing relativistic jets and relativistic collisionless shocks.

Nishikawa, K.-L.↗
NASA NTRS2004

Particle Acceleration, Magnetic Field Generation, and Emission in Relativistic Pair Jets

Shock acceleration is a ubiquitous phenomenon in astrophysical plasmas. Plasma waves and their associated instabilities (e.g., Buneman, Weibel and other two-stream instabilities) created in collisionless shocks are responsible for particle (electron, positron, and ion) acceleration. Using a 3-D relativistic electromagnetic particle (REMP) code, we have investigated particle acceleration associated with a relativistic jet front propagating into an ambient plasma. We find that the growth times depend on the Lorenz factors of jets. The jets with larger Lorenz factors grow slower. Simulations show that the Weibel instability created in the collisionless shock front accelerates jet and ambient particles both perpendicular and parallel to the jet propagation direction. The small scale magnetic field structure generated by the Weibel instability is appropriate to the generation of "jitter" radiation from deflected electrons (positrons) as opposed to synchrotron radiation. The jitter radiation resulting from small scale magnetic field structures may be important for understanding the complex time structure and spectral evolution observed in gamma-ray bursts or other astrophysical sources containing relativistic jets and relativistic collisionless shocks.

Nishikawa, K. I.↗
NASA NTRS2005

Particle Acceleration and Magnetic Field Generation in Electron-Positron Relativistic Shocks

Shock acceleration is a ubiquitous phenomenon in astrophysical plasmas. Plasma waves and their associated instabilities (e.g., Buneman, Weibel, and other two-stream instabilities) created in collisionless shocks are responsible for particle (electron, positron, and ion) acceleration. Using a three-dimensional relativistic electromagnetic particle (REMP) code, we have investigated particle acceleration associated with a relativistic electron-positron jet front propagating into an ambient electron-positron plasma with and without initial magnetic fields. We find small differences in the results for no ambient and modest ambient magnetic fields. New simulations show that the Weibel instability created in the collisionless shock front accelerates jet and ambient particles both perpendicular and parallel to the jet propagation direction. Furthermore, the nonlinear fluctuation amplitudes of densities, currents, and electric and magnetic fields in the electron-positron shock are larger than those found in the electron-ion shock studied in a previous paper at a comparable simulation time. This comes from the fact that both electrons and positrons contribute to generation of the Weibel instability. In addition, we have performed simulations with different electron skin depths. We find that growth times scale inversely with the plasma frequency, and the sizes of structures created by tine Weibel instability scale proportionally to the electron skin depth. This is the expected result and indicates that the simulations have sufficient grid resolution. While some Fermi acceleration may occur at the jet front, the majority of electron and positron acceleration takes place behind the jet front and cannot be characterized as Fermi acceleration. The simulation results show that the Weibel instability is responsible for generating and amplifying nonuniform, small-scale magnetic fields, which contribute to the electron s (positron s) transverse deflection behind the jet head. This small- scale magnetic field structure is appropriate to the generation of "jitter" radiation from deflected electrons (positrons) as opposed to synchrotron radiation. The jitter radiation has different properties than synchrotron radiation calculated assuming a uniform magnetic field. The jitter radiation resulting from small-scale magnetic field structures may be important for understanding the complex time structure and spectral evolution observed in gamma-ray bursts or other astrophysical sources containing relativistic jets and relativistic collisionless shocks.

Nishikawa, K.-I.↗
DOE OSTI2023

Structure of metallochaperone in complex with the cobalamin-binding domain of its target mutase provides insight into cofactor delivery

G-protein metallochaperone MeaB in bacteria [methylmalonic aciduria type A (MMAA) in humans] is responsible for facilitating the delivery of adenosylcobalamin (AdoCbl) to methylmalonyl-CoA mutase (MCM), the only AdoCbl-dependent enzyme in humans. Genetic defects in the switch III region of MMAA lead to the genetic disorder methylmalonic aciduria in which the body is unable to process certain lipids. Here, we present a crystal structure of Methylobacterium extorquens MeaB bound to a nonhydrolyzable guanosine triphosphate (GTP) analog guanosine-5'-[(β,γ)-methyleno]triphosphate (GMPPCP) with the Cbl-binding domain of its target mutase enzyme (MeMCM cbl ). This structure provides an explanation for the stimulation of the GTP hydrolyase activity of MeaB afforded by target protein binding. We find that upon MCM cbl association, one protomer of the MeaB dimer rotates ~180°, such that the inactive state of MeaB is converted to an active state in which the nucleotide substrate is now surrounded by catalytic residues. Importantly, it is the switch III region that undergoes the largest change, rearranging to make direct contacts with the terminal phosphate of GMPPCP. These structural data additionally provide insights into the molecular basis by which this metallochaperone contributes to AdoCbl delivery without directly binding the cofactor. Our data suggest a model in which GTP-bound MeaB stabilizes a conformation of MCM that is open for AdoCbl insertion, and GTP hydrolysis, as signaled by switch III residues, allows MCM to close and trap its cofactor. Substitutions of switch III residues destabilize the active state of MeaB through loss of protein:nucleotide and protein:protein interactions at the dimer interface, thus uncoupling GTP hydrolysis from AdoCbl delivery.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2021

CHARGED POINT DEFECTS AND DEFECT COMPLEXES IN PHOSPHORENE AND STRUCTURAL PREDICTION OF TAU-11, A DENSITY FUNCTIONAL THEORY APPROACH

With the advent of powerful computers, first principle calculations have become a robust and reliable tool to complement experiments in the study of materials. First principle calculations such as density functional theory can be used to guide experiments to save time and effort when it comes to new and advanced materials discovery. Study of charge defects in materials and crystal structure prediction are such areas in which density functional theory calculations facilitate the prediction of defect formation energy, charge transition levels and elemental site occupations. Experimentally, studying charge defects requires inferring results from various techniques. Likewise, determining site occupancies for similar elements using experimental techniques is challenging and sometimes impossible. In this work, we study the charged intrinsic and extrinsic defects and defect complexes in phosphorene and determine the site occupancies of Al, Fe and Si in the τ11 phase using density functional theory. In the defect work, we calculate the defect formation energy, charge transition level, binding energies and Stokes shift for vacancy, dopant substitution and dopant-vacancy defect complexes in phosphorene. We found that vacancy defect in phosphorene becomes negatively charged in n-type doping and may passivate the dopants and reduce carrier concentration and mobility. For non-metal dopants in phosphorene, we predict that O, S and Si prefer to form dopant-vacancy complexes removing the vacancy defect states from the band gap. Mn dopant-vacancy defect complex exhibits possibility of switching between two magnetic spin states. Lastly, using density functional theory, we complement the results from neutron powder diffraction to determine the site occupancies of Al and Si in τ11 phase which was used to determine the alloying element to develop a high temperature and low density alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Driving macro-scale transformations in three-dimensional-printed biopolymers through controlled induction of molecular anisotropy at the nanoscale

Motivated by the need to harness the properties of renewable and biodegradable polymers for the design and manufacturing of multi-scale structures with complex geometries, we have employed our additive manufacturing platform that leverages molecular self-assembly for the production of metre-scale structures characterized by complex geometries and heterogeneous material composition. As a precursor material, we used chitosan, a chemically modified form of chitin, an abundant and sustainable structural polysaccharide. We demonstrate the ability to control concentration-dependent crystallization as well as the induction of the preferred orientation of the polymer chains through the combination of extrusion-based robotic fabrication and directional toolpathing. Anisotropy is demonstrated and assessed through high-resolution micro-X-ray diffraction in conjunction with finite element simulations. Using this approach, we can leverage controlled and user-defined small-scale propagation of residual stresses to induce large-scale folding of the resulting structures.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Structural Modeling Using "Scanning and Mapping" Technique

Supported by NASA Glenn Center, we are in the process developing a structural damage diagnostic and monitoring system for rocket engines, which consists of five modules: Structural Modeling, Measurement Data Pre-Processor, Structural System Identification, Damage Detection Criterion, and Computer Visualization. The function of the system is to detect damage as it is incurred by the engine structures. The scientific principle to identify damage is to utilize the changes in the vibrational properties between the pre-damaged and post-damaged structures. The vibrational properties of the pre-damaged structure can be obtained based on an analytic computer model of the structure. Thus, as the first stage of the whole research plan, we currently focus on the first module - Structural Modeling. Three computer software packages are selected, and will be integrated for this purpose. They are PhotoModeler-Pro, AutoCAD-R14, and MSC/NASTRAN. AutoCAD is the most popular PC-CAD system currently available in the market. For our purpose, it plays like an interface to generate structural models of any particular engine parts or assembly, which is then passed to MSC/NASTRAN for extracting structural dynamic properties. Although AutoCAD is a powerful structural modeling tool, the complexity of engine components requires a further improvement in structural modeling techniques. We are working on a so-called "scanning and mapping" technique, which is a relatively new technique. The basic idea is to producing a full and accurate 3D structural model by tracing on multiple overlapping photographs taken from different angles. There is no need to input point positions, angles, distances or axes. Photographs can be taken by any types of cameras with different lenses. With the integration of such a modeling technique, the capability of structural modeling will be enhanced. The prototypes of any complex structural components will be produced by PhotoModeler first based on existing similar components, then passed to AutoCAD for modification and correction of any discrepancies seen in the Photomodeler version of the 3Dmodel. These three software packages are fully compatible. The DXF file can be used to transfer drawings among those packages. To begin this entire process, we are using a small replica of an actual engine blade as a test object. This paper introduces the accomplishment of our recent work.

Amos, Courtney L.↗
NASA NTRS2017

A Network-Based Algorithm for Clustering Multivariate Repeated Measures Data

The National Aeronautics and Space Administration (NASA) Astronaut Corps is a unique occupational cohort for which vast amounts of measures data have been collected repeatedly in research or operational studies pre-, in-, and post-flight, as well as during multiple clinical care visits. In exploratory analyses aimed at generating hypotheses regarding physiological changes associated with spaceflight exposure, such as impaired vision, it is of interest to identify anomalies and trends across these expansive datasets. Multivariate clustering algorithms for repeated measures data may help parse the data to identify homogeneous groups of astronauts that have higher risks for a particular physiological change. However, available clustering methods may not be able to accommodate the complex data structures found in NASA data, since the methods often rely on strict model assumptions, require equally-spaced and balanced assessment times, cannot accommodate missing data or differing time scales across variables, and cannot process continuous and discrete data simultaneously. To fill this gap, we propose a network-based, multivariate clustering algorithm for repeated measures data that can be tailored to fit various research settings. Using simulated data, we demonstrate how our method can be used to identify patterns in complex data structures found in practice.

Koslovsky, Matthew↗
DOE OSTI2018

Aromatic 3,5-Di(2′,4′-dicarboxylphenyl)benozoic acid based coordination polymers as luminescent sensor for the sensitive detection of chromate anions in aqueous solution

Highlights: • The novel pentacarboxylate of 3,5-di(2′,4′-dicarboxylphenyl)benozoic acid were firstly introduced here. • Topology analyses reveal that complex 1 is a 2D {6"3}{sub 2}{6"4.8.10}{6"4.8"2}{sub 2} trilayer structure, and complex 2 is a 3D {6.8"2}{sub 2}{6"4.8"2}{sub 2}{8.10"4.12} network. • Two coordination polymers both show highly sensitive sensing of Cr(VI) anions in aqueous solution. - Abstract: Based on the mixed ligands of aromatic pentacarboxylate of 3,5-di(2′,4′-dicarboxylphenyl)benozoic acid (H{sub 5}L) and 1,4-bis(imidazol-1-yl) benzene (bib), two novel coordination polymers, namely, [Ni{sub 1.5}(H{sub 2}L)(bib){sub 1.5}(H{sub 2}O){sub 2}]{sub n} (1), and {[Pb_2(HL)(bib)_1_._5(H_2O)]·H_2O}{sub n} (2) have been synthesized and characterized by EA, IR, TG, PXRD. Structure analyses reveal that complexes 1 and 2 are both (3,4,4)-connected structures with the same stoichiometry of (3-c){sub 2}(4-c){sub 2}(4-c), the 2D {6"3}{sub 2}{6"4.8.10}{6"4.8"2}{sub 2} trilayer for 1, and 3D {6.8"2}{sub 2}{6"4.8"2}{sub 2}{8.10"4.12} network for 2. Complexes 1 and 2 exhibit excellent recyclable, selective, and sensitive detection of Cr(VI) anions in aqueous solution. The possible mechanism for selective luminescence quenching responses toward Cr(VI) anions is also discussed in detail.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗