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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Characterization of CST Post-Processing AP-105 Hanford Tank Waste

The primary goal of the Tank Side Cesium Removal (TSCR) system, under development by Washington River Protection Solutions, LLC (WRPS), is to remove entrained solids and 137 Cs from the Hanford tank waste supernate to expedite production of low-activity waste. Ion exchange (IX) testing of 10.9 L of waste from Hanford tank 241-AP-105 (AP-105), performed by Pacific Northwest National Laboratory, used a lead-lag-polish column format, with a bed volume of 10 mL per column, to decontaminate tank waste supernate using crystalline silicotitanate (CST) as the IX media. The AP-105 Cs IX processing test, discussed elsewhere, resulted in a shorter transition zone (i.e., steeper load curve) than those defined by wastes from tanks 241-AP-107 and 241-AW-102.1 The shorter transition zone was indicative of a matrix effect retarding Cs capacity. Therefore, aliquots of spent CST from the lead, lag, and polish columns were subjected to a digestion protocol to quantify analytes retained by the CST and extrapolate the impact on Cs capacity. The spent CST was digested using a combination of 5 M HNO 3 and H 2 O 2 with vigorous heating and stirring. Due to the radiation dose accompanying the 137 Cs on the CST columns, a secondary Cs separation by ammonium molybdophosphate embedded in polyacrylonitrile (AMP-PAN) was performed to separate the 137 Cs from the CST so the samples could be contact-handled for analysis outside of a shielded facility.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Geant4 Event Biasing and Fast Simulation

Geant4 offers advanced event biasing techniques to significantly accelerate simulations involving rare events. Various biasing methods, such as leading particle selection, cross-section biasing, radioactive decay enhancement, and bremsstrahlung splitting, enable efficient event sampling, though they require careful handling. Additionally, Geant4 provides a Fast Simulation Interface, allowing the replacement of standard processes in specific region and for selected particles, enabling faster execution or external code integration. Applications of fast simulation include electromagnetic shower modeling in calorimeters, machine learning inference, and offloading tasks to specialized hardware like GPUs, making Geant4 a powerful tool for computationally demanding simulations.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2023

High-Throughput Characterization and Optimization of Polyamide Hydrolase Activity Using Open Port Sampling Interface Mass Spectrometry

Enzymatic biodegradation of polymers, such as polyamides (PA), has the potential to cost-effectively reduce plastic waste, but enhancements in degradation efficiency are needed. Engineering enzymes through directed evolution is one pathway toward identification of critical domains needed for improving activity. However, screening such enzymatic libraries (100s-to-1000s of samples) is time-consuming. Here we demonstrate the use of robotic autosampler (PAL) and immediate drop on demand technology (I.DOT) liquid handling systems coupled with open-port sampling interface-mass spectrometry (OPSI-MS) to screen for PA6 and PA66 hydrolysis by 6-aminohexanoate-oligomer endo-hydrolase (nylon hydrolase, NylC) in a high-throughput (8–20 s/sample) manner. The OPSI-MS technique required minimal sample preparation and was amenable to 96-well plate formats for automated processing. Enzymatic hydrolysis of PA characteristically produced soluble linear oligomer products that could be identified by OPSI-MS. Incubation temperatures and times were optimized for PA6 (65 °C, 24 h) and PA66 (75 °C, 24 h) over 108 experiments. In addition, the I.DOT/OPSI-MS quantified production of PA6 linear dimer (8.3 ± 1.6 μg/mL) and PA66 linear monomer (13.5 ± 1.5 μg/mL) by NylC with a lower limit of detection of 0.029 and 0.032 μg/mL, respectively. For PA6 and PA66, linear oligomer production corresponded to 0.096 ± 0.018% and 0.204 ± 0.028% conversion of dry pellet mass, respectively. The developed methodology is expected to be utilized to assess enzymatic hydrolysis of engineered enzyme libraries, comprising hundreds to thousands of individual samples.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Plug-and-play polymer microfluidic chips for hydrated, room temperature, fixed-target serial crystallography

The practice of serial X-ray crystallography (SX) depends on efficient, continuous delivery of hydrated protein crystals while minimizing background scattering. Of the two major types of sample delivery devices, fixed-target devices offer several advantages over widely adopted jet injectors, including: lower sample consumption, clog-free delivery, and the ability to control on-chip crystal density to improve hit rates. In this study we present our development of versatile, inexpensive, and robust polymer microfluidic chips for routine and reliable room temperature serial measurements at both synchrotrons and X-ray free electron lasers (XFELs). Our design includes highly X-ray-transparent enclosing thin film layers tuned to minimize scatter background, adaptable sample flow layers tuned to match crystal size, and a large sample area compatible with both raster scanning and rotation based serial data collection. The optically transparent chips can be used both for in situ protein crystallization (to eliminate crystal handling) or crystal slurry loading, with prepared samples stable for weeks in a humidified environment and for several hours in ambient conditions. Serial oscillation crystallography, using a multi-crystal rotational data collection approach, at a microfocus synchrotron beamline (SSRL, beamline 12-1) was used to benchmark the performance of the chips. Furthermore, high-resolution structures (1.3–2.7 Å) were collected from five different proteins – hen egg white lysozyme, thaumatin, bovine liver catalase, concanavalin-A (type VI), and SARS-CoV-2 nonstructural protein NSP5. Overall, our modular fabrication approach enables precise control over the cross-section of materials in the X-ray beam path and facilitates chip adaption to different sample and beamline requirements for user-friendly, straightforward diffraction measurements at room temperature.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2021

Adapting a Low-Cost and Open-Source Commercial Pipetting Robot for Nanoliter Liquid Handling

Nanoliter liquid handling capabilities in bioanalytical workflows can reduce reagent costs and improve sample processing efficiency. Here we report the successful modification of a low-cost commercially available pipetting robot, the Opentrons 1 (OT1), using inexpensive 3D-printed parts to accommodate low-nanoliter volumes. The pipetting accuracy and precision of the modified OT1 for 50 nL volumes of water was 0.2% and 2%, respectively. The accuracy and precision at 20 nL was 1% and 3.8%, respectively. The platform was successfully applied to the preparation of low-nanogram proteomic samples for liquid chromatography-mass spectrometry analysis. The modified OT1 is thus an effective platform for nanoliter liquid handling and, at a total cost of less than $6000 including the commercial liquid handler and all modifications, is far less expensive and more versatile than other platforms with similar capabilities, placing this technology within reach of a far broader scientific community.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Transboundary determinants of avian zoonotic infectious diseases: challenges for strengthening research capacity and connecting surveillance networks

As the climate changes, global systems have become increasingly unstable and unpredictable. This is particularly true for many disease systems, including subtypes of highly pathogenic avian influenzas (HPAIs) that are circulating the world. Ecological patterns once thought stable are changing, bringing new populations and organisms into contact with one another. Wild birds continue to be hosts and reservoirs for numerous zoonotic pathogens, and strains of HPAI and other pathogens have been introduced into new regions via migrating birds and transboundary trade of wild birds. With these expanding environmental changes, it is even more crucial that regions or counties that previously did not have surveillance programs develop the appropriate skills to sample wild birds and add to the understanding of pathogens in migratory and breeding birds through research. For example, little is known about wild bird infectious diseases and migration along the Mediterranean and Black Sea Flyway (MBSF), which connects Europe, Asia, and Africa. Focusing on avian influenza and the microbiome in migratory wild birds along the MBSF, this project seeks to understand the determinants of transboundary disease propagation and coinfection in regions that are connected by this flyway. Through the creation of a threat reduction network for avian diseases (Avian Zoonotic Disease Network, AZDN) in three countries along the MBSF (Georgia, Ukraine, and Jordan), this project is strengthening capacities for disease diagnostics; microbiomes; ecoimmunology; field biosafety; proper wildlife capture and handling; experimental design; statistical analysis; and vector sampling and biology. Here, we cover what is required to build a wild bird infectious disease research and surveillance program, which includes learning skills in proper bird capture and handling; biosafety and biosecurity; permits; next generation sequencing; leading-edge bioinformatics and statistical analyses; and vector and environmental sampling. Creating connected networks for avian influenzas and other pathogen surveillance will increase coordination and strengthen biosurveillance globally in wild birds.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

The effect of hardness on polymer-bonded pentaerythritol tetranitrate (PETN) explosive impact sensitivity

Handling sensitivity is an important property to assess when working with explosive samples and can be measured using a variety of tests, including drop-weight impact sensitivity. There exists a longstanding interest in the explosives community on the importance of measurable chemical, physical, and mechanical properties of explosives in impact sensitivity. However, most recent work in this area has explored chemical attributes rather than physical and mechanical properties of explosives. In this study, we measure hardness of explosive samples of pentaerythritol tetranitrate and Sylgard binder (XTX) during the curing process. The samples have been characterized for particle morphology through scanning electron microscopy and handling sensitivity through drop-weight impact testing. The relative importance of states of cure, methods of curing, morphology, and age of material are discussed. The data indicate that although there is a notable difference in morphology and mechanical properties for the samples as the polymer-bonded mixtures cure, the resulting changes to mechanical properties have a minimal effect on the sensitivity of the XTX.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Airborne Acoustic Vortex End Effector‐Based Contactless, Multi‐Mode, Programmable Control of Object Surfing

Abstract Tweezers based on optical, electric, magnetic, and acoustic fields have shown great potential for contactless object manipulation. However, current tweezers designed for manipulating millimeter‐sized objects such as droplets, particles, and small animals exhibit limitations in translation resolution, range, and path complexity. Here, a novel acoustic vortex tweezers system is introduced, which leverages a unique airborne acoustic vortex end effector integrated with a three‐degree‐of‐freedom (DoF) linear motion stage, for enabling contactless, multi‐mode, programmable manipulation of millimeter‐sized objects. The acoustic vortex end effector utilizes a cascaded circular acoustic array, which is portable and battery‐powered, to generate an acoustic vortex with a ring‐shaped energy pattern. The vortex applies acoustic radiation forces to trap and spin an object at its center, simultaneously protecting this object by repelling other materials away with its high‐energy ring. Moreover, The vortex tweezers system facilitates contactless, multi‐mode, programmable object surfing, as demonstrated in experiments involving trapping, repelling, and spinning particles, translating particles along complex paths, guiding particles around barriers, translating and rotating droplets containing zebrafish larvae, and merging droplets. With these capabilities, It is anticipated that the tweezers system will become a valuable tool for the automated, contactless handling of droplets, particles, and bio‐samples in biomedical and biochemical research.

Li, Teng↗
DOE OSTI2020

Analytical and Computational Advances, Opportunities, and Challenges in Marine Organic Biogeochemistry in an Era of “Omics”

Advances in sampling tools, analytical methods, and data handling capabilities have been fundamental to the growth of marine organic biogeochemistry over the past four decades. There has always been a strong feedback between analytical advances and scientific advances. However, whereas advances in analytical technology were often the driving force that made possible progress in elucidating the sources and fate of organic matter in the ocean in the first decades of marine organic biogeochemistry, today process-based scientific questions should drive analytical developments. Several paradigm shifts and challenges for the future are related to the intersection between analytical progress and scientific evolution. Untargeted “molecular headhunting” for its own sake is now being subsumed into process-driven targeted investigations that ask new questions and thus require new analytical capabilities. However, there are still major gaps in characterizing the chemical composition and biochemical behavior of macromolecules, as well as in generating reference standards for relevant types of organic matter. Field-based measurements are now routinely complemented by controlled laboratory experiments and in situ rate measurements of key biogeochemical processes. And finally, the multidisciplinary investigations that are becoming more common generate large and diverse datasets, requiring innovative computational tools to integrate often disparate data sets, including better global coverage and mapping. Here, we compile examples of developments in analytical methods that have enabled transformative scientific advances since 2004, and we project some challenges and opportunities in the near future. We believe that addressing these challenges and capitalizing on these opportunities will ensure continued progress in understanding the cycling of organic carbon in the ocean.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Conceptual Design and Analysis of In-Vessel Components for the Materials Plasma Exposure eXperiment (MPEX)

The materials plasma exposure experiment (MPEX) is a linear plasma divertor simulator currently undergoing conceptual design. The facility will expose material samples to steady-state plasma fluxes to examine plasma–material interactions (PMIs) that are expected in the next generation of fusion devices. The plasmas will be generated by a helicon source, with electron and ion heating sources of up to 800 kW possible. The peak heat fluxes of the target are expected to be up to 10 MW/m 2 . The facility will be capable of handling low-activation neutron-irradiated samples in order to examine the multivariate effects of neutron damage and plasma fluence. Neutron-irradiated samples are planned to be roughly of 10-mm diameter; however, plasma-facing components up to 60×600 mm can be accommodated. The steady-state nature of the device will require the magnetic confinement of the plasma to be achieved with superconducting magnets, with a maximum on-axis field of 2.5 T. In addition, since MPEX will be a steady-state device, in-vessel components need to be water cooled. The primary in-vessel components will be the target, the dump plate, the limiter, the skimmers, and the microwave absorber. The conceptual design of these components is presented here, including analyses that confirm that the designs are adequate to meet the requirements of MPEX operation.

Lumsdaine, Arnold↗
DOE OSTI2020

Simulating sticky particles: A Monte Carlo method to sample a stratification

Many problems in materials science and biology involve particles interacting with strong, short-ranged bonds that can break and form on experimental timescales. Treating such bonds as constraints can significantly speed up sampling their equilibrium distribution, and there are several methods to sample probability distributions subject to fixed constraints. We introduce a Monte Carlo method to handle the case when constraints can break and form. More generally, the method samples a probability distribution on a stratification: a collection of manifolds of different dimensions, where the lower-dimensional manifolds lie on the boundaries of the higher-dimensional manifolds. We show several applications of the method in polymer physics, self-assembly of colloids, and volume calculation in high dimensions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Automated Systems for Solvent Extraction

An automated solvent extraction system for the eventual handling of radioactive materials has been designed and procured for rapid, efficient and safe liquid-liquid extraction processes. This system will be configured to carry out liquid-liquid separations from beginning to end, automating tedious and time-consuming tasks such as organic/aqueous phase prep, pH checks, phase separation, and metal ion analysis. The system features advanced liquid handling capabilities, a robotic arm for precise sample transfer, and sophisticated analytical tools including UV-VIS spectrophotometry for real-time monitoring. Additionally, it incorporates automated capping of vials, vortex mixing, and centrifugation to ensure thorough mixing and phase separation. This report provides an overview of the system and general capabilities as well as initial efforts to develop an automated workflow for liquid-liquid separations.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2026

Automatic Calibration and Health Monitoring of Infrastructure Sensors

Smart transportation infrastructure relies on networks of heterogeneous sensors - cameras, radars, and lidars - continuously monitoring traffic conditions. However, executing the initial spatial calibration of multiple sensors and the subsequent health monitoring presents significant operational challenges. Environmental factors, mechanical vibrations, and gradual drift cause spatial misalignment, degrading fusion performance and tracking accuracy. Traditional calibration approaches require manual intervention with specialized targets or survey equipment, resulting in service interruptions and high maintenance costs. This work presents an automated framework for initial calibration and continuous health monitoring without human intervention or service disruption. Our approach addresses two critical problems: (1) detecting when sensors become miscalibrated during operation, and (2) automatically re-establishing spatial alignment using only operational traffic data. The health monitoring component analyzes measurement innovations - differences between sensor observations and predicted object states - to detect systematic biases indicative of calibration drift. By computing bias magnitude, directional consistency, and rejection rates, the system identifies miscalibrations as small as 0.5 meters. Unlike traditional methods requiring known calibration targets, our diagnostic operates continuously on live traffic observations, enabling early detection before fusion quality degrades. The automatic recalibration algorithm leverages overlapping sensor fields-of-view and temporal correlation of vehicle observations. Using graph-based optimization, the system automatically discovers which sensor pairs observe common regions, estimates pairwise spatial transformations using RANSAC-based robust estimation, and jointly optimizes all sensor poses through bundle adjustment. The framework handles practical deployment challenges, including different sensor sampling rates (1-10 Hz), varying installation positions, unknown orientations, and limited overlap regions (>10%). When approximate sensor positions are available from installation surveys (+/-1m accuracy), the algorithm additionally estimates sensor orientations, refining both position and rotation to sub-meter and sub-degree accuracy. We validate the framework on multi-hour traffic datasets from six heterogeneous sensors with sampling rates ranging from 1 Hz to 10 Hz. Results demonstrate successful calibration even with sparse overlap (<20%) and automatic detection of miscalibrations exceeding 0.8 meters. This work enables a "deploy-and-forget" sensor infrastructure that maintains calibration autonomously, reducing maintenance costs while improving tracking accuracy. The techniques generalize beyond transportation to any multi-sensor monitoring application requiring robust spatial alignment, including smart cities, industrial monitoring, and surveillance systems.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2025

Effects of sampling techniques on short-term survival and genotyping success of salmonid fry

ABSTRACT Objective Genetics tools have become an integral part of managing and understanding fish populations. Generally, a small tissue sample, such as a fin clip, is taken and then genotyped, with little effect on survival of the fish. However, tissue sampling may have a larger effect on juvenile fish survival compared to their adult counterparts. We evaluated survival and genotyping success of various genetic sampling techniques for Chinook Salmon Oncorhynchus tshawytscha and Rainbow Trout Oncorhynchus mykiss fry. Methods Three sampling treatments were evaluated including control (anesthetized and handled), fin clipping (partial caudal fin clip), and swabbing (OmniSwab was used to collect external mucus). Survival was monitored for 12 d posttreatment, and genotyping success was evaluated. Results Survival was high in all treatment groups (i.e., 0.93–1.00) but, on average, was lower in the swab treatment group. Genotyping was successful in 100% of the fin clip samples and 11–50% of the swab samples. Conclusions Results of this study suggest that sampling caudal-fin tissue does not negatively affect fry short-term survival and the small tissue samples yield highly successful genotyping results. Swabbing did not produce successful genotyping results, and fish sampled with swabs experienced higher mortality than those that received fin clips. Results indicate that fin clips should be used for collection of genetic samples from fry.

McCarrick, Darcy K.↗
DOE OSTI2025

JGI-Trichoderma v1.0

There is a series of Python and bash scripts to parse genomics datasets used to evaluate the coevolution of gene families and the feature importance of gene families using an SVM classifier. - Cover analysis: takes a list of single-copy genes in a set of genomes, aligns and builds the gene trees to determine if two gene families have a signature of covariation with one another. It parses the files to run phykit cover script described here: https://jlsteenwyk.com/PhyKIT/usage/index.html - SVM-classifier: This Python script is an SVM-based genomic classifier designed for biological data analysis. It combines machine learning with feature selection to identify important genomic markers and classify biological samples. Core Functionality: The script uses Support Vector Machines from scikit-learn to classify genomic data, incorporating SelectKBest for automated feature selection and leave-one-out cross-validation for performance assessment. It operates in multiple modes: feature ranking, optimal combination discovery, and sample prediction. Primary Applications: Genomic sample classification and biomarker discovery Feature importance analysis in high-dimensional biological datasets Prediction of sample categories based on genomic profiles Research applications requiring robust classification of biological data Key Advantages: High-dimensional handling: SVMs excel with genomic data's typical high feature-to-sample ratios Integrated feature selection: Reduces noise and computational overhead while identifying key markers Probability estimation: Provides confidence scores essential for biological interpretation Validation robustness: Leave-one-out cross-validation ensures reliable performance metrics Operational flexibility: Multiple analysis modes support different research phases from exploration to prediction

Stecca Steindorff, Andrei [Lawrence Berkeley Natio↗
DOE OSTI2026

PISCES two-detector covariance matrix fit for the NOvA Experiment

NOvA is a long-baseline neutrino oscillation experiment with two functionally identical detectors: a Near Detector (ND) at Fermilab, placed 1 km from the neutrino source, and a Far Detector (FD) located 810 km away from the ND in Minnesota. NOvA's primary physics goals are the precise measurements of neutrino oscillation parameters $\theta_{23}$ and $\Delta m^2_{32}$ , determine the neutrino mass ordering, and constrain the value of $\delta_{CP}$, via the study of muon neutrino to electron neutrino oscillation. In the standard NOvA three-flavor analysis, oscillation parameters are extracted using an extrapolation technique in which the ND data constrain the FD prediction through a ratio method. While this allows for systematic uncertainties sharing the same effects in both detectors to cancel, it remains an FD-only fit and does not fully leverage the constraining power of the high-statistics ND. This analysis proposes a simultaneous ND+FD fit using the PISCES method. PISCES (Parameter Inference with Systematic Covariance and Exact Statistics) is a framework designed to support complex configurations such as a joint ND+FD fit. This allows PISCES to take full advantage of the ND data to directly constrain systematic uncertainties across all samples. In PISCES, systematic uncertainties are encoded in a fractional covariance matrix, and statistical uncertainties are handled with a Poisson likelihood, making the approach well suited for low-statistics samples. For interpretability, we further use a Newton–Raphson + PCA method to recover per-systematic pulls from the covariance formulation. This poster presents the full PISCES joint ND+FD fit for the NOvA three-flavor analysis, describes its implementation and evaluates its performance through extensive robustness tests and fake data studies. It also provides a comparison between the PISCES joint ND+FD results and the standard NOvA extrapolation method.

Rajaoalisoa, Miriama [Cincinnati U.] (ORCID:000000↗
DOE OSTI2022

NSUF Report EBSD analyses on metallic fuel samples: Tips and improvements in sample preparation

EBSD (Electron Backscatter Diffraction) is an analytic technique used to evaluate the microstructure of a specimen. It can be used to evaluate interesting crystallographic data ranging from grains size to grain orientation, from grain boundaries to stresses. Moreover, in the field of nuclear materials EBSD can aid in estimating properties important for reactor performance, such as dislocation and residual strain [1]. EBSD patterns are generated by focusing a stationary electron gun on the specimen and detecting the backscatter electrons that satisfy Bragg conditions, and thus are diffracted by the crystal planes forming the so called Kikuchi bands. These bands correspond to each of the lattice diffracting crystal planes and are detected on a phosphor screen via a low-light CCD camera [2]. The patterns are generated within a small interaction volume located at a depth of less than 50-100 nm. Because of this, the data quality is extremely sensitive to the integrity of the crystallographic lattice order at the surface of the sample and thus to sample preparation and to oxidation [3]. While conventional sample preparation methods are widely used in materials science, they often do not lead to quality electron backscatter patterns needed for the characterization of nuclear materials [4]. This has been related by many authors to the challenges associated with handling radiological specimens, their rapid oxidation, and artifacts in such samples (e.g. high number of defects, precipitates and/or porosities) [4-8]. EBSD, however, can be an invaluable technique to evaluate microstructural evolution during fabrication and after irradiation at the required mesoscale for model and simulation. It also provides important information on grain structure necessary to understand irradiation effect, such as grain subdivision. Thus, it is of paramount importance to further the application of this technique to nuclear materials and especially irradiated fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

f-Element complexes with benzyl and cyclohexyl substituted trihydroborates

Actinide complexes containing the simplest borohydrides (BH 4 ) 1- and (MeBH 3 ) 1- can exhibit remarkably highly volatility, which creates unique hazards and handling challenges, especially when making measurements on solid samples under vacuum. Here we describe efforts to prepare new actinide borohydride complexes with attenuated volatility by adding bulkier benzyl (Bn) and cyclohexyl (Cy) substituents to boron. Reactions of ThCl 4 , UI 3 (thf) 4 , and NdI 3 with the mixed alkali metal salt Li/K(BnBH 3 )(thf) n yielded Th(BnBH 3 ) 4 (thf) 2 , U(BnBH 3 ) 4 (thf) 2 , and K[Nd(BnBH 3 ) 4 ], respectively. Notable amongst these, the reaction with UI 3 (thf) 4 proceeds via oxidation of U(III) to U(IV) despite the presence of reducing borohydride ligands. Similarly, reactions of the same metal halides with four equivalents of Li(CyBH 3 )(Et 2 O) n yielded Th(CyBH 3 ) 4 , U(CyBH 3 ) 4 (thf) 2 , and [Li(Et 2 O) 3 ][Nd(CyBH 3 ) 4 ]. Single crystal X-ray diffraction studies of the M(BnBH 3 ) 4 (thf) 2 complexes with M = Th and U confirmed their formulations. Furthermore, the complexes have approximate D 2d point group symmetry and adopt bicapped hexagonal antiprismatic coordination geometries with axial thf ligands and κ 3 -BnBH 3 ligands bound in the equatorial plane. K[Nd(BnBH 3 ) 4 ] and [Li(Et 2 O) 3 ][Nd(CyBH 3 ) 4 ], which were prepared for comparison to U(III) complexes that were unsuccessfully targeted, were also structurally characterized to reveal complex anions with tetrahedral arrangements of trihydroborate ligands bound to Nd(III). Crystals obtained for Th(CyBH 3 ) 4 and U(CyBH 3 ) 4 (thf) 2 were not suitable for XRD studies, but 1 H and 11 B NMR spectra were consistent with their formulations. Collectively, these complexes represent rare examples of structurally characterized f-element trihydroborate complexes with carbon substituents other than methyl.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗