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At least 19 records

Structural and Mechanistic Advances in the Chemistry of Methyl-Coenzyme M Reductase (MCR)

Methane represents 34% of U.S. energy consumption and is a major greenhouse gas related to the global carbon cycle and energy production. However, current industrial practices significantly increase atmospheric methane levels, necessitating a deeper understanding of its biosynthesis and oxidation. Methyl-coenzyme M reductase (MCR) is central to biological methane metabolism, catalyzing the final step of methanogenesis and the first step in anaerobic methane oxidation. It is also a key target for strategies to capture and transform methane into value-added chemicals.The active site of MCR is a buried Ni-based cofactor only accessible by the substrates via a 50 Å long tunnel. Although the Ni(I) state is required to initiate catalysis, capturing this state remains a challenge for the current structural techniques. Recent advances in structural biology using X-ray Free-Electron Laser serial crystallography have provided insights into MCR's inactive Ni(II) state at room temperature and show promise for capturing its active Ni(I) form.Our team has established several critical aspects of the MCR mechanism using a combination of experimental and computational studies. MCR uses CH 3 -SCoM and CoBSH as substrates, producing methane and a disulfide product CoMSSCoB. Kinetic analysis showed that productive substrate binding requires CH 3 -SCoM to bind first, inducing conformational changes that optimize the active site for subsequent CoBSH binding. Following substrate binding, four proposed methane production/oxidation mechanisms were examined, establishing whether the reaction proceeds through an organometallic methyl-nickel(III), methyl anion ion, or methyl radical intermediate. Experimental measurements using CoBSH analogs successfully slowed the reaction, allowing for mechanistic insight that demonstrated the methyl radical pathway, where the initial interactions involve homolytic cleavage of the methyl-sulfur bond, generating a methyl radical that quickly abstracts the thiol hydrogen atom of CoBSH to form methane. Computational studies further confirmed that, compared to other mechanisms, the methyl radical mechanism is thermodynamically more favorable and accessible under physiological conditions.Spectroscopic and computational studies challenged the conventional understanding of substrate binding in MCR by proposing an alternative positioning of CH 3 -SCoM and CoMSSCoB in the active site pocket. The research suggested that CH 3 -SCoM (substrate) and CoMSSCoB (product) bind via their sulfonate groups to the Ni(I) center of cofactor F 430 . This binding allows for the reaction without substrate reorganization in the pocket but would require a long-range electron transfer. Altogether, the work summarized in this review reflects our current understanding of the enzyme's catalytic mechanism and structural dynamics. This is essential for developing efficient methane conversion technologies that could mitigate its environmental impact while harnessing energy-storage properties.

03 NATURAL GAS↗

A Mass Conservation Relaxed (MCR) LSTM Model for Streamflow Simulation Across CONUS

The recent development of the physics-aware Mass-Conserving Long Short-Term Memory network (MC-LSTM) provides an alternative to other data-driven Deep Learning (DL) models in hydrology. Mass-Conserving Long Short-Term Memory incorporates mass conservation directly into the LSTM architecture. Despite the theoretical advancements, studies have reported a surprisingly limited performance of the MC-LSTM in streamflow simulation. We hypothesize that such a limitation is due to the unrealistic mass conservation scheme in MC-LSTM, which overlooks unobserved incoming water fluxes beyond precipitation. As an attempt to verify this hypothesis, we propose a Mass Conservation Relaxed LSTM (MCR-LSTM), which incorporates a bi-directional mass relaxation (MR) component to account for potential incoming water fluxes beyond precipitation. We train and test the proposed MCR-LSTM model across 531 watersheds in the contiguous United States (CONUS) against three baseline models: the Sacramento Soil Moisture Accounting, LSTM, and MC-LSTM. Our results show that MCR-LSTM outperforms MC-LSTM despite its underperformance compared to LSTM. Specifically, MCR-LSTM's advantage over MC-LSTM is mainly seen in the Plains and Western U.S., where the newly incorporated MR component better simulates water loss and suggests the likely existence of additional incoming water fluxes beyond precipitation, respectively. The novelty and contribution of this study are twofold: firstly, it introduces an alternative physics-aware DL tool (i.e., MCR-LSTM) in hydrology with higher accuracy in specific regions compared to MC-LSTM. Secondly, it provides a diagnosis of regions where strict, precipitation-based mass conservation constraints may be unrealistic in streamflow simulation.

deep learning↗

MCR Container Tools

MathWorks' MATLAB is widely used in academia and industry for prototyping, data analysis, data processing, etc. Many users compile their programs using the MATLAB Compiler to run on workstations/computing clusters via the free MATLAB Compiler Runtime (MCR). The MCR facilitates the execution of code calling Application Programming Interfaces (API) functions from both base MATLAB and MATLAB toolboxes. In a Linux environment, a sizable number of third-party runtime dependencies (i.e. shared libraries) are necessary. Unfortunately, to the MTLAB community's knowledge, these dependencies are not documented, leaving system administrators and/or end-users to find/install the necessary libraries either as runtime errors resulting from them missing or by inspecting the header information of Executable and Linkable Format (ELF) libraries of the MCR to determine which ones are missing from the system. To address various shortcomings, Docker Images based on Community Enterprise Operating System (CentOS) 7, a derivative of Redhat Enterprise Linux (RHEL) 7, containing recent (2015-2017) MCR releases and their dependencies were created. These images, along with a provided sample Docker Compose YAML Script, can be used to create a simulated computing cluster where MATLAB Compiler created binaries can be executed using a sample Slurm Workload Manager script.

Haas, NicholasQ↗

Dissemination of blaNDM-5 and mcr-8.1 in carbapenem-resistant Klebsiella pneumoniae and Klebsiella quasipneumoniae in an animal breeding area in Eastern China

Animal farms have become one of the most important reservoirs of carbapenem-resistant Klebsiella spp. (CRK) owing to the wide usage of veterinary antibiotics. “One Health”-studies observing animals, the environment, and humans are necessary to understand the dissemination of CRK in animal breeding areas. Based on the concept of “One-Health,” 263 samples of animal feces, wastewater, well water, and human feces from 60 livestock and poultry farms in Shandong province, China were screened for CRK. Five carbapenem-resistant Klebsiella pneumoniae (CRKP) and three carbapenem-resistant Klebsiella quasipneumoniae (CRKQ) strains were isolated from animal feces, human feces, and well water. The eight strains were characterized by antimicrobial susceptibility testing, plasmid conjugation assays, whole-genome sequencing, and bioinformatics analysis. All strains carried the carbapenemase-encoding gene bla NDM-5 , which was flanked by the same core genetic structure (IS 5 - bla NDM-5 - ble MBL - trpF - dsbD -IS 26 -IS Kox3 ) and was located on highly related conjugative IncX3 plasmids. The colistin resistance gene mcr-8.1 was carried by three CRKP and located on self-transmissible IncFII(K)/IncFIA(HI1) and IncFII(pKP91)/IncFIA(HI1) plasmids. The genetic context of mcr-8.1 consisted of IS 903 - orf - mcr-8.1-copR-baeS-dgkA - orf -IS 903 in three strains. Single nucleotide polymorphism (SNP) analysis confirmed the clonal spread of CRKP carrying- bla NDM-5 and mcr-8.1 between two human workers in the same chicken farm. Additionally, the SNP analysis showed clonal expansion of CRKP and CRKQ strains from well water in different farms, and the clonal CRKP was clonally related to isolates from animal farms and a wastewater treatment plant collected in other studies in the same province. These findings suggest that CRKP and CRKQ are capable of disseminating via horizontal gene transfer and clonal expansion and may pose a significant threat to public health unless preventative measures are taken.

Yang, Chengxia↗

Collaboration for the Management of the Bruce Power Major Component Replacement (MCR) Nuclear Waste - 19630

Bruce Power's Major Component Replacement (MCR) Program will generate large volume waste via steam generators (SGs) and intermediate-level nuclear waste, which will require specialized packaging and handling to safely receive and store it at Ontario Power Generation's (OPG) Western Waste Management Facility (WWMF). The refurbishment of a Candu reactor involves, in part, the removal and replacement of all of a reactor core's fuel channel assemblies. Bruce Power and OPG collaborated to develop nuclear waste management solutions to optimize the use of OPG's existing Steam Generator Storage Building (SGSB) and Retube Component Storage Building (RCSB). By designing specialized Retube Waste Containers (RWCs) and optimizing configurations for the waste to be stored in the buildings, we will reduce the interim nuclear waste storage needs at the OPG WWMF, while improving Bruce Power MCR process efficiencies and reducing the overall costs of the MCR Program (Units 3 through 8). (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Multivariate Curve Resolution (MCR) using Principal Components Inputs and Rigorous Equality and Inequality Constraints

This MATLAB pseudocode perform multivariate curve resolution (MCR) using PCA scores & loadings of data as inputs. It employs rigorous least squares equality and inequality constraints for all elements in the solution factor matrices. It also can be used to perform nonnegative matrix factorization. SAND2020-12650 M Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-NA0003525.

Van Benthem, Mark↗

Improving perfusion defect detection with respiratory motion correction in cardiac SPECT at standard and reduced doses

Background: In cardiac SPECT perfusion imaging, respiratory motion can cause non-uniform blurring in the reconstructed myocardium. We investigate the potential benefit of respiratory correction with respiratory-binned acquisitions, both at standard dose and at reduced dose, for defect detection and for left ventricular (LV) wall resolution. Methods: We applied two reconstruction methods for respiratory motion correction: post-reconstruction motion correction (PMC) and motion-compensated reconstruction (MCR), and compared with reconstruction without motion correction (Non-MC). We quantified the presence of perfusion defects in reconstructed images by using the total perfusion deficit (TPD) scores and conducted receiver-operating-characteristic (ROC) studies using TPD. We quantified the LV spatial resolution by using the FWHM of its cross-sectional intensity profile. Results: The values in the area-under-the-ROC-curve (AUC) achieved by MCR, PMC, and Non-MC at standard dose were 0.835, 0.830, and 0.798, respectively. Similar AUC improvements were also obtained by MCR and PMC over Non-MC at 50%, 25%, and 12.5% of full dose. Improvements in LV resolution were also observed with motion correction. Conclusions: Respiratory-binned acquisitions can improve perfusion-defect detection accuracy over traditional reconstruction both at standard dose and at reduced dose. Motion correction may contribute to achieving further dose reduction while maintaining the diagnostic accuracy of traditional acquisitions. [French] French Abstract: Contexte: Les mouvements respiratoires peuvent entrainer des artefacts de uniformité lors de la reconstruction des images de perfusion myocardique en SPECT. Dans cet article, nous rapportons nos résultats sur le bénéfice potentiel du « gating » respiratoire avec des doses standards et réduites de radio-pharmaceutiques pour la détection des anomalies de perfusion et les mesures de la paroi ventriculaire gauche. Méthodes: Nous avons appliqué deux méthodes de reconstruction pour la correction du mouvement respiratoire: la première fait appel a une correction après reconstruction des images (PMC) ; la seconde fait appel à la correction des images avant reconstruction (MRC). Les deux approches ont été comparées à la reconstruction sans correction de mouvement (Non-MC). Nous avons quantifié les déficits de perfusion myocardiques sur les images reconstruites avec le système des scores de déficit de perfusion et analysé les résultats en utilisant les courbes ROC. Nous avons quantifié la résolution spatiale du VG en utilisant le FWHM du profil d’intensité de sa section transversale. Résultats: Les valeurs des surfaces en dessous des courbes ROC (AUC) obtenues par MCR, PMC et Non-MC avec doses standard de radio-pharmaceutiques étaient de 0,835, 0,830 et 0,798, respectivement. Des améliorations similaires de l’AUC ont également été obtenues par MCR et PMC sur Non-MC avec 50%, 25% et 12,5% des doses entières. Les mesures de résolution spatiale de la paroi du VG ont également été améliorées avec la correction des mouvements respiratoires. Conclusions: La correction des images de perfusion myocardiques en SPECT par « gating » respiratoire paraît améliorer la quantification des déficits perfusionels à la fois à dose standard et à dose réduite de radio-pharmaceutiques. L’application de cette correction devrait permettre de réduire les doses de radio-pharmaceutiques utilisées tout en maintenant la précision diagnostique des acquisitions traditionnelles. [Spanish] Spanish Abstract: Antecedentes: En los estudios de perfusión cardiaca por SPECT, los movimientos respiratorios pueden causar distorsión no uniforme en el miocardio reconstruido. Investigamos el beneficio potencial de la corrección respiratoria con adquisición de imágenes sincronizadas con la respiración, tanto a dosis estándar como a dosis reducida, para detección de defectos y para resolución de pared de ventrículo izquierdo (VI). Métodos: Aplicamos dos métodos de reconstrucción para corrección de movimientos respiratorios: Corrección de movimiento post reconstrucción (PMC) y reconstrucción compensada a movimiento (MCR), y los comparamos con la reconstrucción sin corrección de movimiento (Non-MC). Cuantificamos la presencia de defectos de perfusión en las imágenes reconstruidas usando los scores de déficit total de perfusión (TPD) y análisis ROC usando el TPD. Cuantificamos la resolución espacial del VI usando la anchura a media altura de su perfil de intensidad transversal. Resultados: Los valores en el área bajo la curva ROC (ABC) obtenidos por MCR, PMC y Non-MC a dosis estándar fueron 0.835, 0.830 y 0.798, respectivamente. Mejorías similares del ABC también se obtuvieron por MCR y PMC, sobre Non-MC a 50%, 25% y 12.5% de la dosis completa. Las mejorías en la resolución del VI fueron observadas también con corrección del movimiento. Conclusiones: Las adquisiciones sincronizadas con la respiración pueden mejorar la precisión de la detección de defectos de perfusión sobre las reconstrucciones tradicionales tanto a dosis estándar como a dosis reducida. La corrección de movimiento puede contribuir a lograr mayor reducción de la dosis manteniendo la precisión diagnóstica de las adquisiciones tradicionales. [Chinese] Chinese Abstract: 背景: 在心脏 SPECT 灌注成像中, 呼吸运动会导致心肌重建的不均匀模糊。我们研究了无论是标准剂量还是减少剂量的情况下, 呼吸跟踪采集的呼吸校正用于图像缺损检测和左心室 (LV) 室壁分辨率的潜在益处。 方法: 我们使用了两种呼吸运动校正的重建方法:重建后运动校正 (PMC) 和运动补偿重建 (MCR), 并与没有运动校正的重建 (Non-MC) 进行比较。 通过总灌注缺损 (TPD) 评分和其接受者操作特性曲线 (ROC) 来量化重建图像中的灌注缺陷。通过LV横截面强度分布的 FWHM来量化 LV 空间分辨率。 结果: MCR, PMC 和 Non-MC 在标准剂量下所获得的 ROC 曲线下面积 (AUC) 的值分别为0.835, 0.830 和 0.798。 在全剂量下, MCR, PMC和 Non-MC也获得类似的 AUC 提高, 分别为 50%, 25% 和 12.5%。 在运动校正下, LV的分辨率也得到了改善。 结论: 在标准剂量和减少剂量的情况下, 呼吸跟踪采集可以改善灌注缺损检测的准确性。 运动校正可能有助于进一步实现减少剂量的目标, 同时保证通过传统检测方法的诊断准确性。.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Seasonal Patterns in Mobile Colistin Resistance Gene Variants in Wastewater Bioaerosols and Liquid Sludge

To address the growing threat of global antimicrobial resistance, a one-health approach is needed to understand the complex socioecological cycling of antibiotic resistance genes. In this study, a metagenomics approach using DNA shotgun sequencing, metagenome assembly, and antibiotic resistance gene (ARG) annotation was used to examine seasonal patterns in the abundance of mobile colistin resistance (mcr) gene variants in bioaerosols and liquid sludge in three wastewater treatment plants (WWTPs). ARGs represented 0.2–0.8 and 0.1–0.2% of the bioaerosol and liquid sludge metagenomes, respectively, while mcr genes represented 0–0.3 and 0–0.5% of the identified ARGs in bioaerosol and liquid sludge metagenomes. Seven of the ten known mcr variants were detected in wastewater bioaerosol and liquid samples, with mcr-5 and mcr-8 being the most prevalent across all seasons and sites. Furthermore, additional functional and taxonomic annotation of mcr-containing metagenomic contigs showed that mcr genes were often located on contigs with other co-occurring ARGs and mobile genetic elements and may be harbored by opportunistic human pathogens and other bacterial taxa not previously associated with mcr genes. Atmospheric dispersion modeling showed that mcr-containing bioaerosols can be transported kilometers away from the WWTPs, resulting in the possible dissemination of these ARGs into surrounding environments and communities.

Antimicrobial agents↗

Overview of Diverse Methyl/Alkyl-Coenzyme M Reductases and Considerations for Their Potential Heterologous Expression

Methyl-coenzyme M reductase (MCR) is an archaeal enzyme that catalyzes the final step of methanogenesis and the first step in the anaerobic oxidation of methane, the energy metabolisms of methanogens and anaerobic methanotrophs (ANME), respectively. Variants of MCR, known as alkyl-coenzyme M reductases, are involved in the anaerobic oxidation of short-chain alkanes including ethane, propane, and butane as well as the catabolism of long-chain alkanes from oil reservoirs. MCR is a dimer of heterotrimers (encoded by mcrABG) and requires the nickel-containing tetrapyrrole prosthetic group known as coenzyme F430. MCR houses a series of unusual post-translational modifications within its active site whose identities vary depending on the organism and whose functions remain unclear. Methanogenic MCRs are encoded in a highly conserved mcrBDCGA gene cluster, which encodes two accessory proteins, McrD and McrC, that are believed to be involved in the assembly and activation of MCR, respectively. The requirement of a unique and complex coenzyme, various unusual post-translational modifications, and many remaining questions surrounding assembly and activation of MCR largely limit in vitro experiments to native enzymes with recombinant methods only recently appearing. Production of MCRs in a heterologous host is an important step toward developing optimized biocatalytic systems for methane production as well as for bioconversion of methane and other alkanes into value-added compounds. This review will first summarize MCR catalysis and structure, followed by a discussion of advances and challenges related to the production of diverse MCRs in a heterologous host.

59 BASIC BIOLOGICAL SCIENCES↗

Expression of divergent methyl/alkyl coenzyme M reductases from uncultured archaea

Abstract Methanogens and anaerobic methane-oxidizing archaea (ANME) are important players in the global carbon cycle. Methyl-coenzyme M reductase (MCR) is a key enzyme in methane metabolism, catalyzing the last step in methanogenesis and the first step in anaerobic methane oxidation. Divergent mcr and mcr -like genes have recently been identified in uncultured archaeal lineages. However, the assembly and biochemistry of MCRs from uncultured archaea remain largely unknown. Here we present an approach to study MCRs from uncultured archaea by heterologous expression in a methanogen, Methanococcus maripaludis . Promoter, operon structure, and temperature were important determinants for MCR production. Both recombinant methanococcal and ANME-2 MCR assembled with the host MCR forming hybrid complexes, whereas tested ANME-1 MCR and ethyl-coenzyme M reductase only formed homogenous complexes. Together with structural modeling, this suggests that ANME-2 and methanogen MCRs are structurally similar and their reaction directions are likely regulated by thermodynamics rather than intrinsic structural differences.

59 BASIC BIOLOGICAL SCIENCES↗

Study on the assessment method of human error probabilities in the digitalized main control room - 170

Recently, nuclear power plants (NPPs) in Republic of Korea have been constructed with the new type of main control room (MCR) which is called as digitalized MCR. In digitalized MCR, as digital technologies are being adopted, the environment of MCR has been considerably changed. The operators may obtain the plant data via digitalized human system interfaces (HSIs), large display panel (LDP), computerized procedure system (CPS), soft controls and other system features. Accordingly, the necessity to consider the new environment of MCR has been raised when performing human reliability analysis (HRA) methods. However, none of HRA methods consider the newly installed MCRs. The goal of this paper is to propose new frameworks to assess the human error probabilities (HEPs) in digitalized MCR. Generally, the HEPs are obtained by summing the probabilities of diagnosis errors and the probabilities of execution errors and those probabilities are modified by performance shaping factors (PSFs). In this paper, two parts are included; (1) Assessing the probabilities of diagnosis errors, and (2) Assessing the probabilities of execution errors. In this paper, the process to develop the frameworks are introduced and we expect that the HEPs affecting the features of digitalized MCR can be calculated by using the proposed frameworks. (authors)

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Colistin resistance plasmids dually enhance bacterial virulence and antibiotic resistance via surface polysaccharide biosynthesis

Plasmids carrying the mobilized colistin-resistance gene mcr-1 are prevalent among multidrug-resistant Gram-negative pathogens, yet their broad impact on bacterial physiology and virulence remains unclear. Here, we demonstrate that acquisition of an mcr-1 plasmid concurrently increases antimicrobial resistance and pathogenicity in Escherichia coli. On the same plasmid, the XRE-family transcriptional regulator EcaR cooperates with MCR-1 to activate the wec operon, driving biosynthesis of two surface polysaccharides: enterobacterial common antigen (ECA) and a high-molecular-weight O-chain. Expression of these surface polysaccharides increases bile resistance and virulence in a murine model and further elevates colistin resistance. MCR-1 enhances transcription of upstream genes in the wec operon, whereas EcaR directly activates an internal promoter (PwecE) to induce downstream gene expression. Thus, both components are required for surface polysaccharide expression, and deletion of either abolishes the phenotype. Genomic analysis of publicly available mcr plasmids reveals widespread co-occurrence of mcr-1 and ecaR on IncI2 and IncX4 plasmids, indicating their functional complementarity. These findings uncover a mechanism by which resistance plasmids remodel the bacterial surface, linking horizontal gene transfer to coordinated regulation of antimicrobial resistance and virulence.

Antimicrobial resistance↗

Mechanistic Studies of a Primitive Homolog of Nitrogenase Involved in Coenzyme F430 Biosynthesis (Final Report)

Methyl-coenzyme M reductase (MCR) is the key enzyme in the biological formation and anaerobic oxidation of methane (AOM). Methane is a potent greenhouse gas and the major component of natural gas. Given the abundance of natural gas reserves in remote areas, there is great current interest in a scalable bio-based process for the conversion of methane to liquid fuel and other high-value chemicals. MCR holds much promise for use in such a methane bioconversion strategy. However, MCR cannot currently be produced in an active form in a heterologous host, due in large part to the lack of genetic and biochemical information about the production of holo MCR. In an effort to overcome this deficiency, our laboratory recently elucidated the biosynthetic pathway of the unique nickel-containing coenzyme of MCR, F430. The key step in coenzyme F430 biosynthesis (Cfb) was found to involve an unprecedented reductive cyclization reaction. This remarkable transformation, which involves a 6-electron reduction, the formation of a γ-lactam ring, and the generation of 7 stereocenters, is catalyzed by a primitive homolog of nitrogenase (CfbCD). Nitrogenase is a two-component metalloenzyme that catalyzes the adenosine triphosphate (ATP)-dependent reduction of dinitrogen to ammonia (nitrogen fixation). Homologs of nitrogenase are also involved in the biosynthesis of the photosynthetic pigments chlorophyll and bacteriochlorophyll. Phylogenetic analysis of the CfbCD complex suggests that it is representative of a more ancient lineage of the nitrogenase superfamily, and a thorough investigation of its structure and function is likely to shed light on the mechanisms and evolution of these important metalloenzymes. Moreover, a detailed understanding of the mechanism of the CfbCD complex may aid in the development of specific inhibitors to help reduce natural greenhouse gas emissions and can be exploited for the heterologous production of MCR for methane bioconversion. Towards these goals, specific aims were pursued for the 1) identification of physiological electron donors and in vivo coenzyme F430 synthesis, 2) analysis of the iron sulfur centers, structure, and oligomerization state changes, and 3) characterization of transient intermediates and the intercomponent electron transfer.

03 NATURAL GAS↗

Mechanistic Studies of a Primitive Homolog of Nitrogenase Involved in Coenzyme F430 Biosynthesis

Methyl-coenzyme M reductase (MCR) is the key enzyme in the biological formation and anaerobic oxidation of methane (AOM). Methane is a potent greenhouse gas and the major component of natural gas. Given the abundance of natural gas reserves in remote areas, there is great current interest in a scalable bio-based process for the conversion of methane to liquid fuel or other high-value commodity chemicals. MCR holds much promise for use in such a methane bioconversion strategy. However, MCR cannot currently be produced in an active form in a heterologous host, due in large part to the lack of genetic and biochemical information about the production of holo MCR. In an effort to overcome this deficiency, our laboratory elucidated the biosynthetic pathway of the unique nickel-containing coenzyme of MCR, F430. The key step in coenzyme F430 biosynthesis (Cfb) was found to involve an unprecedented reductive cyclization reaction that converts Ni-sirohydrochlorin a , c -diamide to 15,17 3 -seco-F430-17 3 -acid. This remarkable transformation, which involves a 6-electron reduction of the isobacteriochlorin ring system, cyclization of the c -acetamide side chain to form a γ-lactam ring, and the formation of 7 stereocenters, is catalyzed by a primitive homolog of nitrogenase (CfbCD). Nitrogenase is a two-component metalloenzyme that catalyzes the ATP-dependent reduction of dinitrogen to ammonia (nitrogen fixation). Homologs of nitrogenase are also involved in the biosynthesis of the photosynthetic pigments chlorophyll and bacteriochlorophyll. Phylogenetic analysis of the CfbCD complex suggests that it is representative of a more ancient lineage of the nitrogenase superfamily, and a thorough investigation of its structure and function is likely to shed light on the mechanisms and evolution of these important metalloenzymes that catalyze multi-electron redox reactions. Moreover, a detailed understanding of the mechanism of the CfbCD complex may aid in the development of specific inhibitors to help reduce natural greenhouse gas emissions and can be exploited for the heterologous production of MCR for methane bioconversion. Towards these goals, the following Specific Aims will be pursued to determine the: 1) Identity of the CfbCD reaction product. The exact reaction catalyzed by CfbCD, including the number of electrons transferred and whether it involves enzymatic cyclization, is unclear. Several approaches, including reaction stoichiometry measurements, spectroelectrochemistry, and magnetic resonance spectroscopy will be applied to elucidate the structure of the reaction product and establish whether CfbCD is a reductase or reductive cyclase. 2) Structure, conformational dynamics, and oligomerization state changes of CfbCD. Significant insight into the mechanism and allosteric regulation of CfbCD can be obtained by assessing changes in the structure and dynamics of the complex during the catalytic cycle. To accomplish this, a combination of size-exclusion chromatography, hydrogen-deuterium exchange mass spectrometry, molecular dynamics simulations, and high-resolution structural methods will be employed. 3) Source, order, and stereochemistry of proton additions during CfbCD catalysis. Details regarding the order and stereochemistry of proton additions during the CfbCD reaction will be uncovered using a combined spectroscopic and computational approach. Complementary mechanistic studies employing site-directed mutagenesis and substrate analogs will establish the identity of active site acid residues and the possible involvement of substrate-assisted catalysis during the CfbCD reaction.

09 BIOMASS FUELS↗

Nickel–Sulfonate Mode of Substrate Binding for Forward and Reverse Reactions of Methyl-SCoM Reductase Suggest a Radical Mechanism Involving Long-Range Electron Transfer

Methyl-coenzyme M reductase (MCR) catalyzes both the synthesis and the anaerobic oxidation of methane (AOM). Its catalytic site contains Ni at the core of cofactor F 430 . The Ni ion, in its low-valent Ni(I) state, lights the fuse leading to homolysis of the C–S bond of methyl-coenzyme M (methyl-SCoM) to generate a methyl radical, which abstracts a hydrogen atom from coenzyme B (HSCoB) to generate methane and the mixed disulfide CoMSSCoB. Direct reversal of this reaction activates methane to initiate anaerobic methane oxidation. On the basis of the crystal structures, which reveal a Ni–thiol interaction between Ni(II)–MCR and inhibitor CoMSH, a Ni(I)–thioether complex with substrate methyl-SCoM has been transposed to canonical MCR mechanisms. Similarly, a Ni(I)–disulfide with CoMSSCoB is proposed for the reverse reaction. However, this Ni(I)–sulfur interaction poses a conundrum for the proposed hydrogen-atom abstraction reaction because the >6 Å distance between the thiol group of SCoB and the thiol of SCoM observed in the structures appears to be too long for such a reaction. The spectroscopic, kinetic, structural, and computational studies described here establish that both methyl-SCoM and CoMSSCoB bind to the active Ni(I) state of MCR through their sulfonate groups, forming a hexacoordinate Ni(I)–N/O complex, not Ni(I)–S. These studies rule out direct Ni(I)–sulfur interactions in both substrate-bound states. As a solution to the mechanistic conundrum, we propose that both the forward and the reverse MCR reactions emanate through long-range electron transfer from the Ni(I)–sulfonate complexes with methyl-SCoM and CoMSSCoB, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗