--- OA_place: publisher OA_type: hybrid PlanS_conform: '1' _id: '20258' abstract: - lang: eng text: The specific introduction of ^1H-^13C or ^1H-^15N moieties into otherwise deuterated proteins holds great potential for high-resolution solution and magic-angle spinning (MAS) NMR studies of protein structure and dynamics. Arginine residues play key roles for example at active sites of enzymes. Taking advantage of a chemically synthesized Arg with a ^13C-^1H2 group in an otherwise deuterated backbone, we demonstrate here the usefulness of proton-detected MAS NMR approaches to probe arginine dynamics. In experiments with crystalline ubiquitin and the 134 kDa tetrameric enzyme malate dehydrogenase we detected a wide range of motions, from sites that are rigid on time scales of at least tens of milliseconds to residues undergoing predominantly nanosecond motions. Spin-relaxation and dipolar-coupling measurements enabled quantitative determination of these dynamics. We observed microsecond dynamics of residue Arg54 in crystalline ubiquitin, whose backbone is known to sample different β-turn conformations on this time scale. The labeling scheme and experiments presented here expand the toolkit for high-resolution proton-detected MAS NMR. acknowledged_ssus: - _id: NMR - _id: LifeSc acknowledgement: This work was supported financially by the Austrian Science Fund (FWF, Grant No. I5812-B, “AlloSpace”). This research was supported by the Scientific Service Units (SSU) of Institute of Science and Technology Austria (ISTA) through resources provided by the Nuclear Magnetic Resonance Facility and the Lab Support Facility (LSF). We thank Petra Rovò and Margarita Valhondo Falcón for excellent support of the NMR facility. article_number: '169379' article_processing_charge: Yes (via OA deal) article_type: original author: - first_name: Darja full_name: Rohden, Darja id: 81dc668a-19fa-11f0-bf31-d56534059ef3 last_name: Rohden - first_name: Federico full_name: Napoli, Federico id: d42e08e7-f4fc-11eb-af0a-d71e26138f1b last_name: Napoli orcid: 0000-0002-9043-136X - first_name: Anna full_name: Kapitonova, Anna id: 9fb2a840-89e1-11ee-a8b7-cc5c7ba62471 last_name: Kapitonova - first_name: Benjamin full_name: Tatman, Benjamin id: 71cda2f3-e604-11ee-a1df-da10587eda3f last_name: Tatman - first_name: Roman J. full_name: Lichtenecker, Roman J. last_name: Lichtenecker - first_name: Paul full_name: Schanda, Paul id: 7B541462-FAF6-11E9-A490-E8DFE5697425 last_name: Schanda orcid: 0000-0002-9350-7606 citation: ama: Rohden D, Napoli F, Kapitonova A, Tatman B, Lichtenecker RJ, Schanda P. Arginine dynamics probed by magic-angle spinning NMR with a specific isotope-labeling scheme. Journal of Molecular Biology. 2025;437(23). doi:10.1016/j.jmb.2025.169379 apa: Rohden, D., Napoli, F., Kapitonova, A., Tatman, B., Lichtenecker, R. J., & Schanda, P. (2025). Arginine dynamics probed by magic-angle spinning NMR with a specific isotope-labeling scheme. Journal of Molecular Biology. Elsevier. https://doi.org/10.1016/j.jmb.2025.169379 chicago: Rohden, Darja, Federico Napoli, Anna Kapitonova, Benjamin Tatman, Roman J. Lichtenecker, and Paul Schanda. “Arginine Dynamics Probed by Magic-Angle Spinning NMR with a Specific Isotope-Labeling Scheme.” Journal of Molecular Biology. Elsevier, 2025. https://doi.org/10.1016/j.jmb.2025.169379. ieee: D. Rohden, F. Napoli, A. Kapitonova, B. Tatman, R. J. Lichtenecker, and P. Schanda, “Arginine dynamics probed by magic-angle spinning NMR with a specific isotope-labeling scheme,” Journal of Molecular Biology, vol. 437, no. 23. Elsevier, 2025. ista: Rohden D, Napoli F, Kapitonova A, Tatman B, Lichtenecker RJ, Schanda P. 2025. Arginine dynamics probed by magic-angle spinning NMR with a specific isotope-labeling scheme. Journal of Molecular Biology. 437(23), 169379. mla: Rohden, Darja, et al. “Arginine Dynamics Probed by Magic-Angle Spinning NMR with a Specific Isotope-Labeling Scheme.” Journal of Molecular Biology, vol. 437, no. 23, 169379, Elsevier, 2025, doi:10.1016/j.jmb.2025.169379. short: D. Rohden, F. Napoli, A. Kapitonova, B. Tatman, R.J. Lichtenecker, P. Schanda, Journal of Molecular Biology 437 (2025). corr_author: '1' date_created: 2025-08-31T22:01:33Z date_published: 2025-12-01T00:00:00Z date_updated: 2025-12-29T14:52:17Z day: '01' ddc: - '540' department: - _id: PaSc doi: 10.1016/j.jmb.2025.169379 external_id: isi: - '001618289100020' file: - access_level: open_access checksum: 90d50594d8ea9860ac5da41297992847 content_type: application/pdf creator: dernst date_created: 2025-12-29T14:51:40Z date_updated: 2025-12-29T14:51:40Z file_id: '20876' file_name: 2025_JourMolecularBiology_Rohden.pdf file_size: 2270555 relation: main_file success: 1 file_date_updated: 2025-12-29T14:51:40Z has_accepted_license: '1' intvolume: ' 437' isi: 1 issue: '23' language: - iso: eng month: '12' oa: 1 oa_version: Published Version project: - _id: eb9c82eb-77a9-11ec-83b8-aadd536561cf grant_number: I05812 name: AlloSpace. The emergence and mechanisms of allostery publication: Journal of Molecular Biology publication_identifier: eissn: - 1089-8638 issn: - 0022-2836 publication_status: published publisher: Elsevier quality_controlled: '1' related_material: record: - id: '19956' relation: research_data status: public scopus_import: '1' status: public title: Arginine dynamics probed by magic-angle spinning NMR with a specific isotope-labeling scheme tmp: image: /images/cc_by.png legal_code_url: https://creativecommons.org/licenses/by/4.0/legalcode name: Creative Commons Attribution 4.0 International Public License (CC-BY 4.0) short: CC BY (4.0) type: journal_article user_id: 2DF688A6-F248-11E8-B48F-1D18A9856A87 volume: 437 year: '2025' ... --- OA_place: publisher OA_type: hybrid PlanS_conform: '1' _id: '20321' abstract: - lang: eng text: Microsecond-to-millisecond motions are instrumental for many biomolecular functions, including enzymatic activity and ligand binding. Bloch-McConnell Relaxation Dispersion (BMRD) Nuclear Magnetic Resonance (NMR) spectroscopy is a key technique for studying these dynamic processes. While BMRD experiments are routinely used to probe protein motions in solution, the experiment is more demanding in the solid state, where dipolar couplings complicate the spin dynamics. It is believed that high deuteration levels are required and sufficient to obtain accurate and quantitative data. Here we show that even under fast magic-angle spinning and high levels of deuteration artifactual “bumps” in 15N R1ρ BMRD profiles are common. The origin of these artifacts is identified as a second-order three-spin Mixed Rotational and Rotary Resonance (MIRROR) recoupling condition. These artifacts are found to be a significant confounding factor for the accurate quantification of microsecond protein dynamics using BMRD in the solid state. We show that the application of low-power continuous wave (CW) decoupling simultaneously with the 15N spin-lock leads to the suppression of these conditions and enables quantitative measurements of microsecond exchange in the solid state. Remarkably, the application of decoupling allows the measurement of accurate BMRD even in fully protonated proteins at 100 kHz MAS, thus extending the scope of μs dynamics measurements in MAS NMR. acknowledged_ssus: - _id: NMR - _id: LifeSc acknowledgement: The authors thank Alexey Krushelnitsky for useful discussions. C.P.J. thanks NSF (MCB-2303862) and NIH (R35GM156238 and S10OD012303) for funding. This research was supported by the Scientific Service Units (SSU) of Institute of Science and Technology Austria (ISTA) through resources provided by the Nuclear Magnetic Resonance and the Lab Support Facilities. article_processing_charge: Yes (via OA deal) article_type: original author: - first_name: Benjamin full_name: Tatman, Benjamin id: 71cda2f3-e604-11ee-a1df-da10587eda3f last_name: Tatman - first_name: Vidhyalakshmi full_name: Sridharan, Vidhyalakshmi last_name: Sridharan - first_name: Motilal full_name: Uttarkabat, Motilal last_name: Uttarkabat - first_name: Christopher P. full_name: Jaroniec, Christopher P. last_name: Jaroniec - first_name: Matthias full_name: Ernst, Matthias last_name: Ernst - first_name: Petra full_name: Rovo, Petra id: c316e53f-b965-11eb-b128-bb26acc59c00 last_name: Rovo orcid: 0000-0001-8729-7326 - first_name: Paul full_name: Schanda, Paul id: 7B541462-FAF6-11E9-A490-E8DFE5697425 last_name: Schanda orcid: 0000-0002-9350-7606 citation: ama: 'Tatman B, Sridharan V, Uttarkabat M, et al. Bumps on the road: The way to clean relaxation dispersion magic-angle spinning NMR. Journal of the American Chemical Society. 2025;147(32):29315-29326. doi:10.1021/jacs.5c09057' apa: 'Tatman, B., Sridharan, V., Uttarkabat, M., Jaroniec, C. P., Ernst, M., Rovo, P., & Schanda, P. (2025). Bumps on the road: The way to clean relaxation dispersion magic-angle spinning NMR. Journal of the American Chemical Society. American Chemical Society. https://doi.org/10.1021/jacs.5c09057' chicago: 'Tatman, Benjamin, Vidhyalakshmi Sridharan, Motilal Uttarkabat, Christopher P. Jaroniec, Matthias Ernst, Petra Rovo, and Paul Schanda. “Bumps on the Road: The Way to Clean Relaxation Dispersion Magic-Angle Spinning NMR.” Journal of the American Chemical Society. American Chemical Society, 2025. https://doi.org/10.1021/jacs.5c09057.' ieee: 'B. Tatman et al., “Bumps on the road: The way to clean relaxation dispersion magic-angle spinning NMR,” Journal of the American Chemical Society, vol. 147, no. 32. American Chemical Society, pp. 29315–29326, 2025.' ista: 'Tatman B, Sridharan V, Uttarkabat M, Jaroniec CP, Ernst M, Rovo P, Schanda P. 2025. Bumps on the road: The way to clean relaxation dispersion magic-angle spinning NMR. Journal of the American Chemical Society. 147(32), 29315–29326.' mla: 'Tatman, Benjamin, et al. “Bumps on the Road: The Way to Clean Relaxation Dispersion Magic-Angle Spinning NMR.” Journal of the American Chemical Society, vol. 147, no. 32, American Chemical Society, 2025, pp. 29315–26, doi:10.1021/jacs.5c09057.' short: B. Tatman, V. Sridharan, M. Uttarkabat, C.P. Jaroniec, M. Ernst, P. Rovo, P. Schanda, Journal of the American Chemical Society 147 (2025) 29315–29326. corr_author: '1' date_created: 2025-09-10T05:37:19Z date_published: 2025-08-01T00:00:00Z date_updated: 2026-01-28T12:36:30Z day: '01' ddc: - '540' department: - _id: PaSc - _id: NMR doi: 10.1021/jacs.5c09057 external_id: isi: - '001542746200001' pmid: - '40748291' file: - access_level: open_access checksum: b350d56ddddefea96cebd62c277c0ff5 content_type: application/pdf creator: dernst date_created: 2025-09-10T07:53:10Z date_updated: 2025-09-10T07:53:10Z file_id: '20337' file_name: 2025_JACS_Tatman.pdf file_size: 5235353 relation: main_file success: 1 file_date_updated: 2025-09-10T07:53:10Z has_accepted_license: '1' intvolume: ' 147' isi: 1 issue: '32' language: - iso: eng month: '08' oa: 1 oa_version: Published Version page: 29315-29326 pmid: 1 publication: Journal of the American Chemical Society publication_identifier: eissn: - 1520-5126 issn: - 0002-7863 publication_status: published publisher: American Chemical Society quality_controlled: '1' related_material: record: - id: '19696' relation: used_in_publication status: public scopus_import: '1' status: public title: 'Bumps on the road: The way to clean relaxation dispersion magic-angle spinning NMR' tmp: image: /images/cc_by.png legal_code_url: https://creativecommons.org/licenses/by/4.0/legalcode name: Creative Commons Attribution 4.0 International Public License (CC-BY 4.0) short: CC BY (4.0) type: journal_article user_id: 317138e5-6ab7-11ef-aa6d-ffef3953e345 volume: 147 year: '2025' ... --- _id: '19696' acknowledged_ssus: - _id: NMR - _id: LifeSc article_processing_charge: No author: - first_name: Benjamin full_name: Tatman, Benjamin id: 71cda2f3-e604-11ee-a1df-da10587eda3f last_name: Tatman citation: ama: 'Tatman B. Dataset for “Bumps on the Road: The Way to Clean Relaxation Dispersion in the Solid State.” 2025. doi:10.15479/AT-ISTA-19696' apa: 'Tatman, B. (2025). Dataset for “Bumps on the Road: The Way to Clean Relaxation Dispersion in the Solid State.” Institute of Science and Technology Austria. https://doi.org/10.15479/AT-ISTA-19696' chicago: 'Tatman, Benjamin. “Dataset for ‘Bumps on the Road: The Way to Clean Relaxation Dispersion in the Solid State.’” Institute of Science and Technology Austria, 2025. https://doi.org/10.15479/AT-ISTA-19696.' ieee: 'B. Tatman, “Dataset for ‘Bumps on the Road: The Way to Clean Relaxation Dispersion in the Solid State.’” Institute of Science and Technology Austria, 2025.' ista: 'Tatman B. 2025. Dataset for ‘Bumps on the Road: The Way to Clean Relaxation Dispersion in the Solid State’, Institute of Science and Technology Austria, 10.15479/AT-ISTA-19696.' mla: 'Tatman, Benjamin. Dataset for “Bumps on the Road: The Way to Clean Relaxation Dispersion in the Solid State.” Institute of Science and Technology Austria, 2025, doi:10.15479/AT-ISTA-19696.' short: B. Tatman, (2025). contributor: - contributor_type: project_leader first_name: Paul id: 7B541462-FAF6-11E9-A490-E8DFE5697425 last_name: Schanda orcid: 0000-0002-9350-7606 - contributor_type: researcher first_name: Vidhyalakshmi last_name: Sridharan - contributor_type: researcher first_name: Motilal last_name: Uttarkabat - contributor_type: researcher first_name: Christopher last_name: Jaroniec - contributor_type: researcher first_name: Matthias last_name: Ernst - contributor_type: researcher first_name: Petra id: c316e53f-b965-11eb-b128-bb26acc59c00 last_name: Rovo orcid: 0000-0001-8729-7326 corr_author: '1' date_created: 2025-05-14T10:46:07Z date_published: 2025-07-31T00:00:00Z date_updated: 2026-01-28T12:36:30Z day: '31' department: - _id: PaSc doi: 10.15479/AT-ISTA-19696 file: - access_level: open_access checksum: 4c2d29404e070bda7d5619f728ec555c content_type: application/zip creator: btatman date_created: 2025-07-31T08:14:40Z date_updated: 2025-07-31T08:14:40Z file_id: '20094' file_name: dataset.zip file_size: 557878455 relation: main_file success: 1 - access_level: open_access checksum: 6cbccd602be0ecb6ddb1f81fdfcadf92 content_type: text/plain creator: btatman date_created: 2025-07-31T08:14:21Z date_updated: 2025-07-31T08:14:21Z file_id: '20095' file_name: readme.txt file_size: 3514 relation: main_file success: 1 file_date_updated: 2025-07-31T08:14:40Z has_accepted_license: '1' license: https://creativecommons.org/licenses/by-nc-sa/4.0/ month: '07' oa: 1 oa_version: None publisher: Institute of Science and Technology Austria related_material: link: - description: Paper to which the dataset corresponds. relation: research_paper url: http.//doi.org/10.1021/jacs.5c09057 record: - id: '20321' relation: research_data status: public status: public title: 'Dataset for "Bumps on the Road: The Way to Clean Relaxation Dispersion in the Solid State"' tmp: image: /images/cc_by_nc_sa.png legal_code_url: https://creativecommons.org/licenses/by-nc-sa/4.0/legalcode name: Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International (CC BY-NC-SA 4.0) short: CC BY-NC-SA (4.0) type: research_data user_id: 2EBD1598-F248-11E8-B48F-1D18A9856A87 year: '2025' ...