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At least 73 records · Page 4

Materials Data on Ho2(B2Rh3)3 by Materials Project

Ho2(Rh3B2)3 crystallizes in the hexagonal P6/mmm space group. The structure is three-dimensional. Ho is bonded in a 12-coordinate geometry to one Ho, twelve Rh, and six equivalent B atoms. The Ho–Ho bond length is 3.50 Å. There are six shorter (3.01 Å) and six longer (3.30 Å) Ho–Rh bond lengths. All Ho–B bond lengths are 3.24 Å. There are two inequivalent Rh sites. In the first Rh site, Rh is bonded in a 4-coordinate geometry to two equivalent Ho and four B atoms. There are two shorter (2.14 Å) and two longer (2.16 Å) Rh–B bond lengths. In the second Rh site, Rh is bonded in a distorted square co-planar geometry to four equivalent Ho and four equivalent B atoms. All Rh–B bond lengths are 2.16 Å. There are two inequivalent B sites. In the first B site, B is bonded to six equivalent Rh atoms to form distorted edge-sharing BRh6 pentagonal pyramids. In the second B site, B is bonded in a 6-coordinate geometry to three equivalent Ho and six Rh atoms.

36 MATERIALS SCIENCE↗

Materials Data on Yb2(B2Rh3)3 by Materials Project

Yb2(Rh3B2)3 crystallizes in the hexagonal P6/mmm space group. The structure is three-dimensional. Yb is bonded in a 12-coordinate geometry to one Yb, twelve Rh, and six equivalent B atoms. The Yb–Yb bond length is 3.47 Å. There are six shorter (3.03 Å) and six longer (3.31 Å) Yb–Rh bond lengths. All Yb–B bond lengths are 3.26 Å. There are two inequivalent Rh sites. In the first Rh site, Rh is bonded in a 4-coordinate geometry to two equivalent Yb and four B atoms. There are two shorter (2.15 Å) and two longer (2.16 Å) Rh–B bond lengths. In the second Rh site, Rh is bonded in a distorted square co-planar geometry to four equivalent Yb and four equivalent B atoms. All Rh–B bond lengths are 2.16 Å. There are two inequivalent B sites. In the first B site, B is bonded to six equivalent Rh atoms to form distorted edge-sharing BRh6 pentagonal pyramids. In the second B site, B is bonded in a 6-coordinate geometry to three equivalent Yb and six Rh atoms.

36 MATERIALS SCIENCE↗

Materials Data on Lu2(B2Rh3)3 by Materials Project

Lu2(Rh3B2)3 crystallizes in the hexagonal P6/mmm space group. The structure is three-dimensional. Lu is bonded in a 12-coordinate geometry to one Lu, twelve Rh, and six equivalent B atoms. The Lu–Lu bond length is 3.49 Å. There are six shorter (3.01 Å) and six longer (3.29 Å) Lu–Rh bond lengths. All Lu–B bond lengths are 3.24 Å. There are two inequivalent Rh sites. In the first Rh site, Rh is bonded in a 4-coordinate geometry to two equivalent Lu and four B atoms. There are two shorter (2.15 Å) and two longer (2.16 Å) Rh–B bond lengths. In the second Rh site, Rh is bonded in a distorted square co-planar geometry to four equivalent Lu and four equivalent B atoms. All Rh–B bond lengths are 2.16 Å. There are two inequivalent B sites. In the first B site, B is bonded to six equivalent Rh atoms to form distorted edge-sharing BRh6 pentagonal pyramids. In the second B site, B is bonded in a 6-coordinate geometry to three equivalent Lu and six Rh atoms.

36 MATERIALS SCIENCE↗

Materials Data on Tm2(B2Rh3)3 by Materials Project

Tm2(Rh3B2)3 crystallizes in the hexagonal P6/mmm space group. The structure is three-dimensional. Tm is bonded in a 12-coordinate geometry to one Tm, twelve Rh, and six equivalent B atoms. The Tm–Tm bond length is 3.51 Å. There are six shorter (3.01 Å) and six longer (3.30 Å) Tm–Rh bond lengths. All Tm–B bond lengths are 3.24 Å. There are two inequivalent Rh sites. In the first Rh site, Rh is bonded in a 4-coordinate geometry to two equivalent Tm and four B atoms. There are two shorter (2.15 Å) and two longer (2.16 Å) Rh–B bond lengths. In the second Rh site, Rh is bonded in a distorted square co-planar geometry to four equivalent Tm and four equivalent B atoms. All Rh–B bond lengths are 2.16 Å. There are two inequivalent B sites. In the first B site, B is bonded to six equivalent Rh atoms to form distorted edge-sharing BRh6 pentagonal pyramids. In the second B site, B is bonded in a 6-coordinate geometry to three equivalent Tm and six Rh atoms.

36 MATERIALS SCIENCE↗

Materials Data on Si2Bi14RhI12 by Materials Project

Rh(SiBi7I6)2 crystallizes in the tetragonal P4/mcc space group. The structure is two-dimensional and consists of two rhodium molecules and two SiBi7I6 sheets oriented in the (0, 0, 1) direction. In each SiBi7I6 sheet, Si4- is bonded in a 4-coordinate geometry to four equivalent Bi+1.21+ atoms. All Si–Bi bond lengths are 2.90 Å. There are three inequivalent Bi+1.21+ sites. In the first Bi+1.21+ site, Bi+1.21+ is bonded in a distorted square co-planar geometry to four I1- atoms. There are a spread of Bi–I bond distances ranging from 3.17–3.29 Å. In the second Bi+1.21+ site, Bi+1.21+ is bonded in a distorted water-like geometry to one Si4- and one I1- atom. The Bi–I bond length is 3.73 Å. In the third Bi+1.21+ site, Bi+1.21+ is bonded in a distorted square co-planar geometry to four equivalent I1- atoms. All Bi–I bond lengths are 3.24 Å. There are two inequivalent I1- sites. In the first I1- site, I1- is bonded in a 2-coordinate geometry to two equivalent Bi+1.21+ atoms. In the second I1- site, I1- is bonded in a 3-coordinate geometry to three Bi+1.21+ atoms.

36 MATERIALS SCIENCE↗

Determination of Ce 3+ , Co 2+ , Mn 2+ and Fe 2+ diffusion coefficients in Nafion® membrane

Concentration gradient diffusion coefficients for Ce 3+ , Co 2+ , Mn 2+ and Fe 2+ cations are determined in Nafion®211 membranes over a wide range of environmental conditions. Measurements are made using finite-width cation-rich bands introduced to NR211 via a hot-pressing procedure. A robust method of accurate diffusion coefficient determination of the finite-width deposits is developed using a Fick's second law of diffusion solution for one-dimensional systems. The transition metal dications are found to have nearly identical NR211 diffusion coefficients under water saturated conditions over the 22–80 °C range. The powerful chemical mitigant, Ce 3+ , is about one-half as diffusive as the dications under identical conditions. Derived diffusion coefficients for Ce 3+ and Co 2+ are found to be independent of initial cation concentration over the range of 12.5–70 mol% exchange level. The diffusion behavior of Ce 3+ in 80 °C liquid water and saturated water vapor is identical. The diffusion coefficients of Ce 3+ are shown to have a strong dependence on membrane hydration level varying by a factor of more than 30 over the range of 95 to 40% RH. Finally, the implications of these new diffusion findings are applied to a discussion of potential guidelines for the development of highly durable fuel cell systems, which employ mobile metal cations as lifetime-extending redox stabilizers.

08 HYDROGEN↗

Data-Driven Discovery of Bimetallic Nanoparticles Catalysts for the Hydrogenolysis of Polyethylene

Supported platinum nanoparticles are known to convert polyolefins to high-quality liquid hydrocarbons with hydrogen under relatively mild conditions. However, no systematic study has been undertaken using bimetallic catalysts for polyethylene upcycling. Specifically, a total of 98 monometallic and bimetallic combinations (Ag, Cr, Co, Cu, Fe, Ga, In, Mn, Ni, Pd, Pt, Rh, Ru, Zr) on alumina were synthesized utilizing surface organometallic chemistry (SOMC) technique via robotic platform. These were investigated at a small scale (10 mg of catalyst and 50 mg of polyethylene) for their activity for the hydrogenolysis of polyethylene in a high-throughput batch reactor. Combinations of Ni and Co were selected as candidates with high activity toward conversion into paraffin oils. Reaction conditions were optimized with Ni/Co/Al 2 O 3 catalyst at a larger scale (300 mg catalyst and 3 g polyethylene) to obtain a high yield (93.1%) of paraffin wax with desired properties (M n = 380 Da) and low polydispersity (Đ = 1.2). Ni/Co/Al 2 O 3 was compared against Co/Ni/Al 2 O 3 to understand the role of the deposition sequence. When Co is deposited before Ni, a layer of cobalt aluminate is formed upon reduction, stabilizing the deposition of 5 nm metallic Ni particles. When nickel is deposited before Co, particles are larger (average >20 nm) and more oxidized (Ni δ+ in NiAl 2 O 4 ), decreasing the availability of the catalytically active metallic Ni. In conclusion, the difference in electronic environments was also described by DFT calculations, which revealed that smaller 3D clusters of Ni are preferred on CoAl2O4 over the 3D clusters on NiAl 2 O 4 and that these smaller clusters are more reducible, as confirmed experimentally.

Polymer↗

Baselining Activity and Stability of ORR Catalysts and Electrodes for Proton Exchange Membrane Fuel Cells for Heavy-Duty Applications

Activity and stability of electrodes with Pt and PtCo alloy catalysts supported on high surface area carbon, hereafter to as a-Pt/C and d-PtCo/C, were evaluated for heavy-duty applications. Both catalysts had nearly identical Pt loading (50-wt% Pt on carbon and 0.25 mg Pt cm −2 ) and had undergone thermal treatment to stabilize them by growing the average particle size to 4–5 nm. Both were subjected to 90,000 (90 k) standard accelerated stress tests (AST) cycles consisting of 0.6–0.95 V square wave potentials, 3-s hold at upper and lower potential limits in H 2 /N 2 at 1.5 atm, 80 °C and 100% RH. Test protocols were developed to monitor the performance losses and characterize them in terms of activity for the oxygen reduction reaction (ORR), oxygen transport in the electrode and proton transport in the membrane and cathode catalyst layer. Despite the nearly double initial ORR activity, the PtCo/C electrode degraded faster due to the leaching of Co from the catalyst that had started even before the imposition of the AST potential cycles. Commensurate with Co leaching, Co poisoning of ionomer is responsible for the inferior performance of d-PtCo/C electrode at high current densities both before and after AST.

30 DIRECT ENERGY CONVERSION↗

Design of Efficient Molecular Electrocatalysts for Water and Carbon Dioxide Reduction Using Predictive Models of Thermodynamic Properties

Objectives: 1) To design and synthesize water soluble transition metal complexes that function as electrocatalysts for the reduction of water to hydrogen or carbon dioxide to formate 2) To experimentally measure thermochemical properties, such as hydride donor ability, and use these quantities to optimize catalyst performance in solutions of varying pH 3) To incorporate results from detailed mechanistic and kinetic studies to direct improvements in catalyst design 4) To use thermochemical data from objective 2 to generate predictive models for the properties of new complexes to apply to the development of catalysts for other reductive reactions, with an emphasis on carbon dioxide reduction to methanol Description: Wide-spread implementation of renewable but intermittent energy sources, such as solar, requires the development of efficient methods for energy storage. The high energy density of chemical bonds makes chemical fuels an ideal solution for energy storage. Hydrogen and reduced carbon compounds have been proposed as ideal candidates for chemical fuels. However, the generation of chemical fuels from electricity requires competent electrocatalysts. The proposed research focuses on developing electrocatalysts for the reduction of water to hydrogen, and carbon dioxide to formate. Both products can be used directly as an energy carrier in fuel cells, or as a reductant for more saturated chemical fuels. Hydrogen is the most common fuel used in current commercial fuel cells. Additionally, there is interest in formic acid as a liquid carrier for hydrogen because of its increased storage density and ease of dehydrogenation. Formate is also an intermediate in the sequential reduction of CO 2 to methanol, another potential chemical fuel with high energy storage density. Despite the utility of formate as a chemical fuel or precursor, there are very few examples of electrocatalysts for its production from CO 2 , and even fewer demonstrate high product selectivity. In heterogeneous catalysis, the Sabatier principle is used to generate volcano curves that describe optimal thermochemical properties for key intermediates that result in peak catalytic activity. In most cases, such as hydrogen production and oxidation, the most favorable metals (Pt, Re, Rh, and Ir) are rare and expensive. Molecular inorganic complexes provide an opportunity to use electronic and steric ligand effects to tune the critical thermodynamic parameters of abundant metals to values comparable to key surface intermediates on precious metals. This principle will be applied to the design of aqueous homogeneous catalysts for the reduction of H 2 O and CO 2 optimized to function at specific pH ranges. The critical intermediate in both of these reactions is a metal hydride. The strength of this bond, or hydricity (ΔGH - ) dictates the overall thermodynamics of the reduction of H + to H 2 and the sequential reduction of C1 substrates, such as CO 2 , CO, and H 2 CO (the latter to CH 3 OH). ΔGH - will be systematically measured for a series of first row metal complexes to form predictive models for metal and ligand electronic effects. Benefits and Outcomes: This approach addresses thermodynamic requirements essential for energy-efficient catalyst design and transition state barrier considerations for faster catalysis. The advancements made from this research will include the discovery of efficient, stable, and fast catalysts for hydrogen and formate generation from electricity. The ability to store energy efficiently is critical to the widespread use of renewable energy schemes. This provides a viable solution to produce high energy density fuels for stationary and mobile energy applications. The fundamental research conducted is also directly applicable to the design of catalysts for the generation of further reduced products such as methanol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Self-Supported Branched Poly(ethylenimine) Monoliths from Inverse Template 3D Printing for Direct Air Capture

3D-printed inverse templates are combined with ice templating to develop self-supported branched poly(ethylenimine) monoliths with regular channels of varying channel density and ordered macropores. A maximum uptake of 0.96 mmol of CO 2 /g of monolith from ambient air containing 45.5% RH is achieved from dynamic breakthrough experiments, which is a 31% increase compared to the CO 2 uptake from adsorption under dry conditions for the same duration. The breakthrough experiments show characteristics of internal mass-transfer limitations. The cyclic dynamic breakthrough experiments indicate stable operation without significant loss in CO 2 uptake across eight cycles. Moreover, the self-supported monolith shows minimal loss in adsorption capacity (7.7%) upon exposure to air containing 21% oxygen at 110 °C, in comparison to a conventional sorbent consisting of poly(ethylenimine) impregnated on Al 2 O 3 (18.9%). The monoliths exhibit good mechanical stability, contributed by elastic deformation, corresponding to up to 74% strain and lower pressure drop compared to many existing monoliths in the literature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A General Approach for Metal Nanoparticle Encapsulation Within Porous Oxides

Abstract Encapsulation of metal nanoparticles within oxide materials has been shown as an effective strategy to improve activity, selectivity, and stability in several catalytic applications. Several approaches have been proposed to encapsulate nanoparticles, such as forming core‐shell structures, growing ordered structures (zeolites or metal‐organic frameworks) on nanoparticles, or directly depositing support materials on nanoparticles. Here, a general nanocasting method is demonstrated that can produce diverse encapsulated metal@oxide structures with different compositions (Pt, Pd, Rh) and multiple types of oxides (Al 2 O 3 , Al 2 O 3 ‐CeO 2 , ZrO 2 , ZnZrO x , In 2 O 3 , Mn 2 O 3 , TiO 2 ) while controlling the size and dispersion of nanoparticles and the porous structure of the oxide. Metal@polymer structures are first prepared, and then the oxide precursor is infiltrated into such structures and the resulting material is calcined to form the metal@oxide structures. Most Pt@oxides catalysts show similar catalytic activity, demonstrating the availability of surface Pt sites in the encapsulated structures. However, the Pt@Mn 2 O 3 sample showed much higher CO oxidation activity, while also being stable under aging conditions. This work demonstrated a robust nanocasting method to synthesize metal@oxide structures, which can be utilized in catalysis to finely tune metal‐oxide interfaces.

Zhou, Chengshuang↗

Low Regeneration Temperature Sorbents for Direct Air Capture of CO 2

Susteon Inc., in partnership with University of Wyoming and SoCalGas, successfully met all major technical objectives to (1) scale up the ionic liquid catalyst for amine-based sorbents for improved desorption and absorption kinetics, (2) evaluate the catalyzed amine-based sorbents for direct CO 2 capture process to determine CO 2 adsorption and desorption rates and energy requirements, and (3) based on the experimental results, develop a conceptual process design to perform a preliminary economic assessment to evaluate the potential for DAC process cost reduction using the catalyzed sorbents. Amine doped solid sorbents are effective for DAC applications and can be regenerated by heat or by a combination of heat, steam, and vacuum. The best sorbent composition identified was polyethyleneimine (PEI) on fumed silica with 200 ppm ionic liquid catalyst. This sorbent formulation was shown to have a CO 2 breakthrough capacity twice that of the non-catalyzed sorbent, in laboratory tests with air at 75% relative humidity (RH). The CO 2 adsorption rate was also 40% higher than that of the non-catalyzed sorbent. This type of sorbents has the attributes required for lowering the overall cost of DAC with high CO 2 capacity and high rate of adsorption. The combination of an industrially utilized amine-based sorbent with a highly active catalyst to form a new class of materials for DAC provides a technically viable pathway for reducing the cost of DAC to <$100/tonne of CO 2 . Laboratory measurements show that the silica/PEI (polyethyleneimine) sorbents with 100 ppm of ionic liquid catalyst have almost 100% higher CO 2 cyclic capacity and 40% higher adsorption rate. Generally, CO 2 desorption occurred at higher temperatures with a rate of desorption 10 times faster than adsorption (which occurred at ambient conditions). Therefore, adsorption rate is a much more important factor in the cost of DAC because it is directly linked to the CAPEX of the total system and the cycle time (i.e., sorbent productivity in ton/day of CO 2 captured per unit volume of the air contactor). An initial process design, coupled with techno-economic analysis, based on optimal experimental results and preliminary resulting from structured sorbent testing, showed a path to lower the DAC cost from the current cost of over $200/tonne CO 2 to less than $100/tonne with a scale-up, mature state of the technology, with projected material and process improvements. These results demonstrate the effectiveness of the catalyst in silica/PEI sorbents in enhancing sorbents’ CO 2 working capacity, in (a) increasing the rate of adsorption and desorption, and (b) in lowering the CAPEX and OPEX of the DAC system employing the ionic liquid catalyzed sorbents.

01 COAL, LIGNITE, AND PEAT↗

Antiferromagnet to ferromagnet crossover driven by nonmagnetic Co doping in heavy-fermion YbRh 3 Si 7

YbRh 3 ⁢Si 7 is a heavy fermion compound that stands out among Yb-based heavy fermions, with its relatively high magnetic ordering temperature and large Yb-Yb distance. To investigate the origin of the magnetic properties in this compound, we synthesized Co doped YbRh 3⁢ Si 7 , achieving a record-high ferromagnetic ordering temperature T C =15.6K, only limited by the Co solubility of 20%. Furthermore, we find a crossover from antiferromagnetic to ferromagnetic order with Co doping. Additionally, the specific heat and magnetotransport measurements show heavy fermion behavior and the persistence of Kondo latticelike behavior in the Yb⁢(Rh 1-x Co x ) 3⁢ Si 7 series.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Functional variability in specific root respiration translates to autotrophic differences in soil respiration in a temperate deciduous forest

CO 2 release from forest soils (R s ) is a prominent flux in the global carbon cycle. Rs is derived from roots (autotrophic respiration, R a ) and microbial (heterotrophic) respiration and is highly dynamic, as it depends on edaphic and environmental conditions as well as root functional traits and microbial community composition. It is unclear how root functional traits affect root and microbial respiration rates; however, their consideration may help parse out the relative contributions of root and microbial respiration to R s . At a temperate forest site, root systems of 3–4 functional root orders and their surrounding surface soil were carefully excavated and placed into custom trays designed to repeatedly measure R s in situ on eight temperate tree species that varied in their root functional strategies and mycorrhizal affinity. R s was measured bi-weekly to monthly for nearly one year using a custom chamber attached to a gas exchange system. R s varied over time, ranging from 0.3 to 12 µmol m -2 s -1 . Comparable root systems of the same species were excised from the soil and specific root respiration rates (R r ) were measured. Rr ranged from 2.5 to 9.0 nmol g -1 s -1 and was negatively correlated with root tissue density and positively related to root tissue nitrogen concentration. Using R r to estimate R a , we estimate that R a accounts for <10%, on average 2–3%, of R s for individual root systems (averaging 1.2 g dry biomass) housed in surrounding soil (average 1.3 kg dry mass) in situ; thus, Ra was roughly 20 times greater than Rh per unit mass. The contribution of R a peaked in the fall and coincided with leaf senescence of the forest canopy. A soil-sterilizing experimental treatment designed to help isolate R a in situ reduced bacterial biomass and shifted fungal community composition, but there was no reduction in Rs of the in-situ root-soil tray systems. The relative R a to R s ratio increased with root functional strategies characterized by greater specific root length and tip abundance, but also to greater root tissue density. The ratio of R a to R s also increased with warmer soil temperatures and decreased slightly with increasing soil moisture. We discuss how incorporating root functional traits as modulators of the autotrophic contribution to R s could be considered when modeling total soil CO 2 efflux from forests.

54 ENVIRONMENTAL SCIENCES↗

Unraveling the Structural Sensitivity of Metal Catalysts in Ethylene Hydroformylation: Insights from Theory and Experiments

Here, in this study, we combined experimental and theoretical methods to investigate the structural sensitivity of metal catalysts in the ethylene hydroformylation reaction. Among Rh, Pt, Ir, Ni, Au, Ag, Pd, and Cu catalysts studied using experimental and theoretical methods, Rh showed the highest selectivity toward the C-C coupling product from CO and C 2 H 5 (i.e., C 2 H 5 CHO). The results from DFT and microkinetic simulations revealed that the activation energy barrier for C-C coupling is lowest on the Rh nanocluster, which explains the experimentally observed highest C 2 H 5 CHO selectivity on the Rh catalyst. Furthermore, DFT results demonstrated that the sites located on the flat surfaces of nanoparticles primarily promote the hydrogenation reaction, leading to the formation of undesired C 2 H 6 . In contrast, undercoordinated edge and corner sites of the nanocluster promote the C-C coupling reaction. Thus, our results illustrate that the selectivity toward C 3 oxygenates in ethylene hydroformylation reaction can be steered by tuning the size of Rh nanoparticles (the best-performing catalyst) to optimize the active (edge and corner) sites that preferentially promote the C-C coupling reaction.

58 GEOSCIENCES↗

Regolith Volatile Characterization (RVC) in RESOLVE

Resource investigation in the lunar poles is of importance to the potential impact of in-situ resource utilization (ISRU). The RESOLVE project developed a payload to investigate the permanently shadowed areas of the lunar poles and demonstrate ISRU technology. As a part of the RESOLVE project, the regolith volatile characterization (RVC) subsystem was designed to examine the release of volatiles from sample cores. The test sample was heated in the reactor to release the volatiles where they were analyzed with gas chromatography. Subsequently, the volatile sample was introduced into the lunar water resource demonstration (LWRD) subsystem where the released hydrogen and water were selectively captured. The objective of the Regolith Volatile Characterization (RVC) subsystem was to heat the crushed core sample and determine the desorption of volatile species of interest. The RVC subsystem encompasses the reactor and the system for volatile analysis. The system was designed to analyze H2, He, CO, CO2, N2, 02, CH4, H2S and H2O. The GC chosen for this work is a Siemens MicroSAM process GC with 3 columns and 8 TCD detectors. Neon was chosen as the carrier gas to enhance the analysis of hydrogen and helium.The limit of detection for the gases is approx.1000ppm for H2, CO. CO2 , N2, O2 and H2 S. The limit of detection for CH4 is approx.4000ppm and the water limit of detection is -10000 ppm with a sample analysis time of 2-3 minutes. These values (with the exception of water and H2S) were determined by dilution of a six gas mixture from Scott Gas (5% CO2, CO, O2, N2, 4% CH4 and H2) using mass flow controllers (MFC5). Water was calibrated at low levels using an in house relative humidity (RH) generator. H 2S and high concentrations of H2 were calibrated by diluting a pure stream of gas with MFCs. Higher concentrations of N2 and 02 were calibrated using Air again diluting with MFCs. There were three modification goals for the GC in EBU2 that would allow this process GC to be used in the field demo for RESOLVE. The first modification was to decrease the weight associated with the GC, this included eliminating the explosion proof case (Figure 1) and replacing it with a lightweight case as well as using an on board COPV tank for the neon carrier gas. The next goal was to add a second oven for the molecular sieve column to allow for dual temperature control during GC operation; the separation of hydrogen and helium is optimum at lower temperatures while the water analysis required higher temperatures creating a competing design requirement. The second oven also allows a lower limit of detection for water quantification and avoids the possibility of water condensing in the GC which could ruin the column characteristics. The final goal was to modify the column arrangement to optimize the system for our specific application. Figure 2 shows the internal details of the module optimized optimized for our field application. The modifications and performance of the gas analysis system will be discussed in detail.

Captain, Janine↗

Materials Data on Pr4(BRh4)3 by Materials Project

Pr4(Rh4B)3 crystallizes in the tetragonal P4/mmm space group. The structure is three-dimensional. there are two inequivalent Pr sites. In the first Pr site, Pr is bonded to twelve Rh atoms to form PrRh12 cuboctahedra that share corners with twelve PrRh12 cuboctahedra, faces with six PrRh12 cuboctahedra, and faces with four equivalent BRh6 octahedra. There are a spread of Pr–Rh bond distances ranging from 2.93–3.03 Å. In the second Pr site, Pr is bonded to twelve Rh atoms to form PrRh12 cuboctahedra that share corners with twelve PrRh12 cuboctahedra, faces with six PrRh12 cuboctahedra, and faces with eight BRh6 octahedra. There are a spread of Pr–Rh bond distances ranging from 3.00–3.03 Å. There are five inequivalent Rh sites. In the first Rh site, Rh is bonded in a distorted single-bond geometry to four equivalent Pr and one B atom. The Rh–B bond length is 2.08 Å. In the second Rh site, Rh is bonded to four equivalent Pr and two B atoms to form a mixture of distorted corner, edge, and face-sharing RhPr4B2 octahedra. The corner-sharing octahedra tilt angles range from 0–61°. There are one shorter (2.16 Å) and one longer (2.20 Å) Rh–B bond lengths. In the third Rh site, Rh is bonded in a distorted square co-planar geometry to four equivalent Pr atoms. In the fourth Rh site, Rh is bonded to four Pr and two equivalent B atoms to form a mixture of distorted corner, edge, and face-sharing RhPr4B2 octahedra. The corner-sharing octahedra tilt angles range from 0–61°. Both Rh–B bond lengths are 2.14 Å. In the fifth Rh site, Rh is bonded to four equivalent Pr and two equivalent B atoms to form a mixture of distorted corner, edge, and face-sharing RhPr4B2 octahedra. The corner-sharing octahedra tilt angles range from 0–60°. Both Rh–B bond lengths are 2.14 Å. There are two inequivalent B sites. In the first B site, B is bonded to six Rh atoms to form BRh6 octahedra that share corners with five BRh6 octahedra and faces with eight PrRh12 cuboctahedra. The corner-sharing octahedra tilt angles range from 0–7°. In the second B site, B is bonded to six Rh atoms to form BRh6 octahedra that share corners with six BRh6 octahedra and faces with eight equivalent PrRh12 cuboctahedra. The corner-sharing octahedral tilt angles are 0°.

36 MATERIALS SCIENCE↗

A Positive Charge in the Outer Coordination Sphere of an Artificial Enzyme Increases CO 2 Hydrogenation

The protein scaffold around the active site of enzymes is known to influence catalytic activity, but specific scaffold features responsible for favorable influences are often not known. This study focuses on using an artificial metalloenzyme to probe one specific feature of the scaffold, the position of a positive charge in the outer coordination sphere around the active site. Previous work showed that a small molecular complex, [Rh(P Et 2 N glycine P Et 2 )2 ] – , immobilized covalently within a protein scaffold was activated for CO 2 hydrogenation. In this work, using an iterative design where the effect of arginine, histidine, or lysine residues placed in the outer coordination sphere of the catalytic active site were evaluated, we tested the hypothesis that positively charged groups facilitate CO 2 hydrogenation with seven unique constructs. Single-, double-, and triple-point mutations were introduced to directly compare catalytic activity, as monitored by turnover frequencies (TOFs) measured in real time with 1 H NMR spectroscopy, and evaluate related structural and electronic properties. Two of the seven constructs showed a 2- and 3-fold increase relative to the wild type, with overall rates ranging from 0.2 to 0.7 h –1 , and a crystal structure of the fastest of these shows the positive charge positioned next to the active site. A crystal structure of the arginine-containing complex shows that the arginines are positioned near the metal. Molecular dynamics (MD) studies also suggest that the positive charge is oriented next to the active site in the two constructs with faster rates but not in the others and that the positive charge near the active site holds the CO 2 near the metal, all consistent with a positive charge appropriately positioned in the scaffold benefiting catalysis. The MD studies also suggest that changes in the water distribution around the active site may contribute to catalytic activity, while modest structural changes and movement of the complex within the scaffold do not.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗