I11-High Resolution Powder Diffraction
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Diamond Proposal Number(s):
[36314]
Open Access
Abstract: Ocean-bearing icy worlds may harbour the necessary conditions for life, but we do not yet understand the processes that deliver ocean fluids to the surface where they are accessible to spacecraft. We demonstrate that hydrates of sodium-chloride (NaCl), a constituent of icy world oceans, record the thermal conditions experienced by NaCl rich fluids as they freeze. Through laboratory experiments, we identify four distinct NaCl-H2O assemblages, comprising crystalline and amorphous phases. The specific phase assemblage produced by freezing of brine depends on both the cooling rate and the initial brine salinity, with the production of metastable phases favoured at lower salinities and faster cooling rates. Different NaCl–H₂O assemblages exhibit characteristic near-infrared signatures that may provide a valuable tool for interpreting data collected by upcoming orbital missions to icy worlds. These results establish that the NaCl-H2O solid phase composition could be used as a new diagnostic probe of cryogenic processes on icy worlds, providing a means to reconstruct geological history of ocean-derived surface material and enabling space missions to assess the evolution of icy worlds across the outer Solar System.
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Sep 2026
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B21-High Throughput SAXS
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Diamond Proposal Number(s):
[35585]
Open Access
Abstract: The self-assembly in aqueous solutions, cytocompatibility, and collagen production of lipopeptide C16–KTTKS and a variant with arginine substitution for lysine, C16–RTTRS, are investigated. C16–KTTKS is known commercially as Matrixyl and is used in cosmetic formulations as it can stimulate collagen production. The self-assembly and conformations and collagen-stimulating effects of the two lipopeptides in two salt forms, trifluoroacetate (TFA) and acetate, are compared. Lipopeptide C16-KTTKS self-assembles into nanotapes based on a multi-bilayer stacking across a pH range pH 4–7 and micelles at pH 2, with little influence of the counterion. In contrast, C16-RTTRS forms a substantial population of spherical micelles for the acetate salt for pH 2–7, but mainly nanotapes for the TFA salt for pH 4–7. Conditions for hydrogel formation by C16-KTTKS were identified. Both lipopeptides show good cytocompatibility to fibroblasts at sufficiently low concentration. The two lipopeptides also stimulate collagen production in Human Dermal Fibroblasts (HDFa) at low concentration (0.0062 wt%). No significant effect of the counterion was noted on cell viability or collagen production. Our results suggest that the peptide sequence influences the pH-dependent self-assembly properties and that this can be modulated for certain lipopeptides by the nature of the counterions.
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Aug 2026
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B07-B1-Versatile Soft X-ray beamline: High Throughput ES1
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Diamond Proposal Number(s):
[43895]
Open Access
Abstract: X-ray photoelectron spectroscopy (XPS) is a major technique in catalyst research due to its ability to determine chemical states on the surface. Near ambient pressure XPS (NAP-XPS) enables in situ analysis, offering valuable insight into catalytic processes. However, modern catalysts are often supported on non-conductive supports such as TiO2 or SiO2, which can present significant challenges for XPS analysis due to charging and differential charging. These issues can distort spectral data, rendering data unusable and wasting valuable instrument time. While several sample preparation strategies exist, many are limited by not allowing high temperature analysis, the risk of sample loss (e.g., from powder flaking off), or continued susceptibility to charging. In this work, we introduce a simple, robust, and time-efficient method for mounting catalyst powders by compressing them between aluminium foil disks. This approach provides excellent sample hold, minimises charging effects, and is suitable for high-temperature NAP-XPS analysis and synchrotron x-ray sources. The method addresses key limitations of conventional preparation techniques and enables more reliable characterisation of insulating catalyst materials.
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Aug 2026
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I18-Microfocus Spectroscopy
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Open Access
Abstract: Predicting steel corrosion in porous media – e.g. soil, bentonite, concrete – remains challenging due to the limited understanding of the precipitation and evolution of corrosion products under realistic conditions. To shed light on these processes, we investigate the long-term temporal and spatial evolution of iron (hydr)oxides at the pore-scale, employing in-situ synchrotron-based chemical imaging including X-ray fluorescence, X-ray diffraction, X-ray absorption spectroscopy, and absorption contrast. A pore is simulated in a 300 μm diameter capillary, containing iron and stagnant electrolyte, and is aged for up to 2.7 years. The electrolyte is buffered at pH 8, with HCO3-, Cl-, and SO42- ions, both under aerobic and near-anaerobic conditions. Results show that, in electrolytes containing HCO3-, ferrihydrite initially formed remotely from the iron and transformed into goethite over time. In the long-term, mixed-valence green rust and magnetite formed near the iron. The spatial distribution and oxidation states of corrosion products can be rationalized using a reactive transport conceptual framework: Fe(II) and O2 release or consumption in electrochemical, diffusion, oxidation and additional reactions determine the concentration profiles and hence the location and time when corrosion products precipitate. Electrolyte composition – Cl- and SO42- – further influences which corrosion product is formed and stabilized over a certain time (e.g. green rust and lepidocrocite). Our findings demonstrate preferential precipitation on pore walls and far from the iron, with prolonged green rust stability, showcasing the relevance of investigating iron (hydr)oxides in realistic pore models. These insights improve predictions of corrosion product evolution, pore clogging, and stresses in porous media.
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Jul 2026
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B21-High Throughput SAXS
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Bridget
Tang
,
Philip
Kitchen
,
Luke M.
Broadbent
,
Steven D.
Quinn
,
Nawal
Hassan
,
Siriporn
Chaimueangchuen
,
Barbara
Gerbelli
,
Katsuaki
Inoue
,
Nathan
Cowieson
,
Fátima
Herranz-Trillo
,
Alice J.
Rothnie
,
Roslyn M.
Bill
,
Paul D.
Topham
,
Alan D.
Goddard
,
Jacob J. K.
Kirkensgaard
,
Matthew J.
Derry
,
Andreas Haahr
Larsen
Diamond Proposal Number(s):
[39511]
Open Access
Abstract: Amphiphilic copolymers have emerged as powerful, detergent-free tools for solubilizing biological membranes, enabling the extraction and stabilization of membrane proteins within native-like lipid environments. We report a comprehensive, multi-technique elucidation of how polymer:lipid stoichiometry governs the formation, size, and stability of styrene-maleic acid lipid particles (SMALPs). Using commercial SMA2000, a styrene-maleic acid copolymer made using free radical polymerization and 1,2-ditetradecanoyl-sn-glycero-3-phosphocholine (DMPC) as a model phospholipid, we prepared SMALPs across a wide range of polymer-to-lipid weight ratios and employed an integrated suite of orthogonal characterization methods, including size exclusion chromatography (SEC), dynamic light scattering (DLS), flow-induced dispersion analysis (FIDA), mass photometry, ensemble and time-resolved Förster resonance energy transfer (FRET), and small-angle X-ray scattering (SAXS), to establish the structural consequences of varying polymer content. Our data reveal that efficient lipid solubilization into nanodiscs requires a minimum amount of polymer. Above ~1% (w/v) SMA2000: 1% DMPC, well-defined nanodiscs of ~10 nm diameter are formed that, on average, exhibit a consistent stoichiometry of ~130 lipids encircled by ~11 polymer chains. Through a new molecularly-constrained SAXS model, we show that these nanodiscs possess a stable bilayer height across variations in polymer to lipid ratio and a narrow polymer belt, and that their structural parameters remain invariant once excess polymer is used. In contrast, insufficient polymer (<1% w/v) generates bimodal populations including substantially larger discs. Notably, nanodiscs formed at optimal polymer:lipid ratios remain structurally stable for at least two months. Together, these results provide a rigorous quantification of SMALP composition and preferred size, enhancing our understanding of polymer-lipid nanodisc formation and offering critical design rules for detergent-free membrane protein extraction.
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Jul 2026
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I13-2-Diamond Manchester Imaging
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Louis
Verschuren
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Vladimir
Matskovsky
,
Matthieu N
Boone
,
Pieter
De Frenne
,
Tom
De Mil
,
Kristof
Haneca
,
Shashidhara
Marathe
,
Charlotte
Pearson
,
Christoph
Rau
,
Ute
Sass-Klaassen
,
Joris
Van Acker
,
Kris
Vandekerkhove
,
Kaz
Wanelik
,
Julia
Weidemüller
,
Valerie
Trouet
,
Jan
Van Den Bulcke
Diamond Proposal Number(s):
[36278]
Open Access
Abstract: Maximum latewood density of conifers is the most widely used annual-resolution summer temperature proxy. Regions with few conifers, however, remain underrepresented in global paleoclimate records. Here, we use x-ray micro–computed tomography (micro-CT) to show that latewood density measurements of European beech (Fagus sylvatica L.) in a temperate lowland forest exhibit a strong summer (May to September) temperature signal (r = 0.73; 1833 to 2022 CE). Complementary wood anatomical analyses using deep learning segmentation reveal that both vessel and fiber anatomy are key drivers of latewood density variability and its temperature sensitivity. By integrating these anatomical responses, x-ray micro-CT–based latewood density measurements generate a robust and temporally stable summer temperature signal. Our results highlight the untapped potential of broad-leaved tree species for density-based climate reconstructions in temperate regions and open previously unidentified avenues for high-resolution paleoclimatology beyond the use of conifers.
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Jul 2026
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labSAXS-Offline SAXS and Sample Environment Development
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Diamond Proposal Number(s):
[34017, 37151, 39136]
Open Access
Abstract: Alpha olefin sulfonate (AOS) is a widely used anionic surfactant, yet its phase behaviour has not previously been systematically mapped. Here, a comprehensive phase diagram is constructed over a concentration range of 2–70 wt% and temperatures from 25 to 80 °C using cross-polarized optical microscopy and small-angle X-ray scattering (SAXS). Polarized microscopy was used to delineate isotropic and anisotropic regions and identify phase boundaries, while SAXS provided quantitative structural characterisation, including lattice parameters, electron density reconstructions, and micellar size and shape analysis. Measurements were performed in sealed capillaries under controlled thermal conditions, with refined temperature increments used to resolve phase transitions. Five distinct phases were identified with decreasing water content: a micellar dispersion; a 2D hexagonal phase; a 2D ribbon phase; a previously unreported 3D hexagonal phase; and two lamellar phases. This temperature- and concentration-dependent sequence is structurally analogous to that of sodium dodecyl sulfate (SDS), though key distinctions arise from the molecular architecture of AOS, which promotes unique intermediate mesophases through differences in molecular packing and constrained hydration. Structural analysis reveals a systematic evolution of spatial water organisation, progressing from excess bulk water in the micellar phase, to tubular confinement within hexagonal and ribbon phases, to discrete water pockets embedded within surfactant bilayers in the 3D hexagonal phase, and finally to residual interfacial hydration in the lamellar phases. This work establishes the relationship between hydration state and mesophase structure, and provides the first complete structural phase diagram for this important surfactant system, enabling prediction of phase behaviour under the complex conditions encountered in industrial processing.
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Jun 2026
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I03-Macromolecular Crystallography
I04-Macromolecular Crystallography
I24-Microfocus Macromolecular Crystallography
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Daming
Zhou
,
Abhay
Kotecha
,
James T.
Kelly
,
Peng-Nien
Huang
,
Yi-Yin
Chen
,
Thomas S.
Walter
,
Helen M. E.
Duyvesteyn
,
Raymond J.
Owens
,
Shu-Yuan
Ho
,
Tzou-Yien
Lin
,
Elizabeth E.
Fry
,
Jingshan
Ren
,
Kuan-Ying A.
Huang
,
David I.
Stuart
Diamond Proposal Number(s):
[14744]
Open Access
Abstract: EV-A71 has been responsible for recent severe HFMD outbreaks. We report structures for 12 potently neutralizing human anti–EV-A71 monoclonal antibody Fabs, alone and complexed with virus. Most recognize the native antigenic state with epitopes that span interfaces, together covering 85% of the capsid surface. The majority (8 of 12) bind the canyon, while the others cluster around the icosahedral two- and threefold axes. Blocking SCARB2 receptor binding likely contributes to neutralization for all, and a subset induces empty particles. A predominant gene family (IGHV4-39) does not dictate a common binding pose. Long CDR-H3 loops are frequently key to binding, especially at the canyon, suggesting that antigenicity data based on antibodies with shorter CDR3s (e.g., murine) may be misleading. This dataset reveals neutralization mechanisms for recently circulating EV-A71 genotypes, which will inform immunotherapies. We demonstrate synergy in vitro between canyon binding and both two- and threefold binding antibodies to increase neutralization potency.
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Jun 2026
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I04-Macromolecular Crystallography
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Jogi
Madhuprakash
,
Amirali
Toghani
,
Hsuan
Pai
,
Madia
Harvey
,
Adam R.
Bentham
,
Benjamin A.
Seager
,
Enoch Lok Him
Yuen
,
Juan Carlos
De La Concepcion
,
David M.
Lawson
,
Clare E. M.
Stevenson
,
Angel
Vergara-Cruces
,
Lida
Derevnina
,
Tolga O.
Bozkurt
,
Mark J.
Banfield
,
Sophien
Kamoun
,
Mauricio P.
Contreras
Diamond Proposal Number(s):
[25108]
Open Access
Abstract: Pathogens counteract central nodes of NLR immune receptor networks to suppress immunity. However, the mechanisms by which pathogens hijack helper NLR pathways are poorly understood. We show that an effector from the late blight pathogen Phytophthora infestans interacts with the host protein NbTOL9a and a helper NLR to suppress immunity. We solved the crystal structure of the RXLR-LWY effector AVRcap1b in complex with the ENTH domain of NbTOL9a. The structure revealed that, unlike other RXLR-LWY effectors, AVRcap1b has a previously unidentified L-shaped fold that defines a distinct structural family of effectors in the genus Phytophthora. We defined the AVRcap1b/NbTOL9a binding interface and designed effector mutants that do not bind NbTOL9a, impairing immune suppression. This suggests that ENTH binding is required for full virulence activity. Last, we show that AVRcap1b associates specifically with activated NbNRC2 independently of NbTOL9a binding. We propose a model in which the effector interconnects NbNRC2 with the NbTOL9a pathway. Our results illustrate a previously uncharacterized pathogen mechanism to hijack NLR pathways and suppress immunity.
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Jun 2026
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I19-Small Molecule Single Crystal Diffraction
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Diamond Proposal Number(s):
[32131]
Open Access
Abstract: Artemisinin (ART) is mainly used for the treatment of malaria and exhibits polymorphism with two known crystalline forms. In this study, the high-pressure behaviour of these two polymorphs was investigated to evaluate their compressibility and identify if any pressure-induced phase transitions occur with a view to assessing the impact of manufacturing pressure on the active pharmaceutical ingredient. Form (I), the orthorhombic polymorph, is found to be the most compressible of the three. Form (II), a triclinic phase, undergoes a phase transition to a new polymorph that is observed at different pressures depending on the pressure-transmitting medium (PTM) used. The transition to form (III) occurs at 0.75 GPa when compressed in petroleum ether, however, this transition is delayed to 2.02 GPa in silicone oil. This highlights the influence of the PTM on the stability of the crystal structure. The newly characterized form (III) shares structural similarities with form (II) but differs in symmetry where a pseudo-21 screw axis in form (II) becomes a formal 21 screw axis in form (III), resulting in a change from triclinic to monoclinic and a reduction of the asymmetric unit from Z′ = 4 to Z′ = 2. These findings contribute to a deeper understanding of pressure-induced polymorphism in ART and underscores the importance of external factors such as PTM in influencing solid-state transitions relevant to pharmaceutical processing and formulation.
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Jun 2026
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