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These dynamics include not only biomacromolecules but also small solutes, ions, and water. To establish an NMR framework for characterizing such heterogeneous dynamic regimes, we employ two homogeneous viscous model systems, glycerol and PEG400, which reproduce the slowed molecular motions characteristic of condensed biomolecular environments while avoiding the structural complexity of phase-separated systems. Using solid-state NMR relaxometry, we investigate multi-time scale dynamics in these model solvents and examine water behavior under crowded conditions. Nanosecond motions are characterized by heteronuclear Overhauser effects and 13C T1 relaxation, while microsecond dynamics are probed via T2 and T1\u03c1 relaxation; and translational self-diffusion is quantified using diffusion-ordered spectroscopy (DOSY). Glycerol and PEG400 exhibit similar fast nanosecond rotational motions (\u223c 0.7\u20131.0 ns), yet their distinct viscosities are associated with differences in slower rotational dynamics and translational self-diffusion. Water exhibits constrained nanosecond motion in both systems, indicating partially immobilized populations shaped by variations in free volume. This work establishes an NMR-based framework for resolving multi-time scale dynamics in viscous systems, providing insights into LLPS and hydration behavior.<\/jats:p>","DOI":"10.1021\/acs.jpcb.6c04720","type":"journal-article","created":{"date-parts":[[2026,9,12]],"date-time":"2026-09-12T15:02:52Z","timestamp":1789225372000},"page":"10783-10791","source":"Crossref","is-referenced-by-count":0,"title":["Molecular Motion\nof Viscous Solvents from Solid-State\nNMR"],"prefix":"10.1021","volume":"130","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-7207-6010","authenticated-orcid":true,"given":"Wanli","family":"Zhang","sequence":"first","affiliation":[{"name":"Nanyang Technological University , , 21 Nanyang Link , ,","place":["Singapore, Singapore, 637371"]},{"name":"Nanyang Technological University , , 21 Nanyang Link , ,","place":["Singapore, Singapore, 637371"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuling","family":"Feng","sequence":"additional","affiliation":[{"name":"Shanghai Jiao Tong University , , ,","place":["Shanghai, China, 200062"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hong","family":"Ye","sequence":"additional","affiliation":[{"name":"Nanyang Technological University , , ,","place":["Singapore, Singapore, 637551"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kai","family":"Xue","sequence":"additional","affiliation":[{"name":"Nanyang Technological University , , 21 Nanyang Link , ,","place":["Singapore, Singapore, 637371"]},{"name":"Nanyang Technological University , , 21 Nanyang Link , ,","place":["Singapore, Singapore, 637371"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,12]]},"reference":[{"issue":"3","key":"2026100809100004700_cit1","doi-asserted-by":"publisher","first-page":"419","DOI":"10.1016\/j.cell.2018.12.035","article-title":"Considerations and Challenges in\nStudying Liquid\u2013Liquid Phase Separation and Biomolecular Condensates","volume":"176","author":"Alberti","year":"2019","journal-title":"Cell"},{"key":"2026100809100004700_cit2","doi-asserted-by":"publisher","first-page":"39","DOI":"10.1146\/annurev-cellbio-100913-013325","article-title":"Liquid\u2013Liquid\nPhase Separation\nin Biology","volume":"30","author":"Hyman","year":"2014","journal-title":"Annu. 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Genet."},{"key":"2026100809100004700_cit4","doi-asserted-by":"publisher","first-page":"290","DOI":"10.1038\/s41392-021-00678-1","article-title":"Liquid\u2013Liquid\nPhase Separation\nin Human Health and Diseases","volume":"6","author":"Wang","year":"2021","journal-title":"Signal Transduction\nTargeted Ther."},{"key":"2026100809100004700_cit5","doi-asserted-by":"publisher","first-page":"1767","DOI":"10.1038\/s41467-022-29408-z","article-title":"Temporal\nand Spatial Characterisation of Protein Liquid\u2013Liquid\nPhase Separation Using NMR Spectroscopy","volume":"13","author":"Bramham","year":"2022","journal-title":"Nat.\nCommun."},{"issue":"8","key":"2026100809100004700_cit6","doi-asserted-by":"publisher","first-page":"2375","DOI":"10.1074\/jbc.REV119.009847","article-title":"The (Un)Structural\nBiology of Biomolecular Liquid\u2013Liquid\nPhase Separation Using NMR Spectroscopy","volume":"295","author":"Murthy","year":"2020","journal-title":"J.\nBiol. 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Chem.\nB"},{"issue":"12","key":"2026100809100004700_cit27","doi-asserted-by":"publisher","first-page":"6031","DOI":"10.1021\/jp0445122","article-title":"Relaxation Dynamics\nin Glycerol-\nWater Mixtures: I. Glycerol-Rich Mixtures","volume":"109","author":"Puzenko","year":"2005","journal-title":"J.\nPhys. Chem. B"},{"issue":"3","key":"2026100809100004700_cit28","doi-asserted-by":"publisher","first-page":"034508","DOI":"10.1063\/1.3672096","article-title":"Intermolecular\nRelaxation in Glycerol as Revealed by Field Cycling 1H\nNMR Relaxometry Dilution Experiments","volume":"136","author":"Meier","year":"2012","journal-title":"J. Chem.\nPhys."},{"issue":"9","key":"2026100809100004700_cit29","doi-asserted-by":"publisher","first-page":"2117","DOI":"10.1021\/ie50501a040","article-title":"Viscosity of Glycerol\nand Its Aqueous Solutions","volume":"43","author":"Segur","year":"1951","journal-title":"Ind. Eng. 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Reson."},{"issue":"41","key":"2026100809100004700_cit33","doi-asserted-by":"publisher","first-page":"7864","DOI":"10.1002\/anie.200801338","article-title":"Bicelle-Enabled Structural Studies\non a Membrane-Associated\nCytochrome B5 by Solid-State MAS NMR Spectroscopy","volume":"47","author":"Xu","year":"2008","journal-title":"Angew. Chem., Int. Ed."},{"issue":"1","key":"2026100809100004700_cit34","doi-asserted-by":"publisher","first-page":"1","DOI":"10.1016\/j.jmr.2007.06.002","article-title":"The Truncated Driven\nNOE and 13C NMR Sensitivity Enhancement in Magnetically-Aligned\nBicelles","volume":"188","author":"Macdonald","year":"2007","journal-title":"J. Magn. Reson."},{"issue":"38","key":"2026100809100004700_cit35","doi-asserted-by":"publisher","first-page":"12398","DOI":"10.1021\/ja064037g","article-title":"Observation of Heteronuclear\nOverhauser Effects Confirms the 15N- H Dipolar Relaxation Mechanism\nin a Crystalline Protein","volume":"128","author":"Giraud","year":"2006","journal-title":"J. Am. Chem. Soc."},{"issue":"15","key":"2026100809100004700_cit36","doi-asserted-by":"publisher","first-page":"5896","DOI":"10.1021\/ja00171a049","article-title":"Nuclear Overhauser\nEffect in Solids","volume":"112","author":"White","year":"1990","journal-title":"J. Am. Chem. Soc."},{"key":"2026100809100004700_cit37","doi-asserted-by":"publisher","first-page":"59","DOI":"10.1016\/j.jmr.2016.03.006","article-title":"Hybridizing Cross-Polarization with\nNOE or Refocused-INEPT Enhances the Sensitivity of MAS NMR Spectroscopy","volume":"266","author":"Zhang","year":"2016","journal-title":"J. Magn. Reson."},{"issue":"31","key":"2026100809100004700_cit38","doi-asserted-by":"publisher","first-page":"13311","DOI":"10.1021\/acs.jpcc.2c03798","article-title":"2D HETCOR Solid-State NMR Spectroscopy\nfor Multiphase Materials with Mobility Contrast","volume":"126","author":"Yan","year":"2022","journal-title":"J. Phys. Chem. C"},{"key":"2026100809100004700_cit39","doi-asserted-by":"publisher","first-page":"505","DOI":"10.1016\/S0022-2860(01)00731-1","article-title":"Heteronuclear\nNOE in the Solid State","volume":"602","author":"Higgins","year":"2002","journal-title":"J. Mol. Struct."},{"issue":"1\u20132","key":"2026100809100004700_cit40","doi-asserted-by":"publisher","first-page":"79","DOI":"10.1016\/S0926-2040(97)00017-9","article-title":"Exploiting\nMethyl Groups as Motional Labels for Structure Analysis in Solid Polymers","volume":"10","author":"White","year":"1997","journal-title":"Solid State Nucl. Magn. 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Soc."},{"issue":"50","key":"2026100809100004700_cit44","doi-asserted-by":"publisher","first-page":"19888","DOI":"10.1021\/jacs.9b11195","article-title":"Exploring Protein Structures by DNP-Enhanced\nMethyl\nSolid-State NMR Spectroscopy","volume":"141","author":"Mao","year":"2019","journal-title":"J. Am. Chem. Soc."},{"issue":"4","key":"2026100809100004700_cit45","doi-asserted-by":"publisher","first-page":"1150","DOI":"10.1021\/acs.jpclett.4c03331","article-title":"Nanosecond Molecular Motion in pHP1\u03b1 Liquid\u2013Liquid Phase\nSeparation Captured by Solid-State NMR","volume":"16","author":"Chin","year":"2025","journal-title":"J. Phys.\nChem. 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Res.\nDev."},{"key":"2026100809100004700_cit49","first-page":"1","article-title":"Intramolecular\nDipolar Relaxation in Multi-Spin Systems","volume-title":"Advances in Magnetic and Optical Resonance","author":"Redfield","year":"1966"},{"key":"2026100809100004700_cit50","doi-asserted-by":"publisher","first-page":"728","DOI":"10.1103\/PhysRev.89.728","article-title":"The Dynamical Theory of Nuclear Induction","volume":"89","author":"Wangsness","year":"1953","journal-title":"Phys. Rev."},{"issue":"17","key":"2026100809100004700_cit51","doi-asserted-by":"publisher","first-page":"4546","DOI":"10.1021\/ja00381a009","article-title":"Model-Free Approach to the Interpretation of Nuclear Magnetic Resonance\nRelaxation in Macromolecules. I. Theory and Range of Validity","volume":"104","author":"Lipari","year":"1982","journal-title":"J. Am. Chem. 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