TY - JOUR A1 - Hollamby, M. J. A1 - Aratsu, K. A1 - Pauw, Brian Richard A1 - Rogers, S. E. A1 - Smith, A. J. A1 - Yamauchi, M. A1 - Lin, X. A1 - Yagai, S. T1 - Simultaneous SAXS and SANS Analysis for the Detection of Toroidal Supramolecular Polymers Composed of Noncovalent Supermacrocycles in Solution N2 - Molecular self-assembly primarily occurs in solution. To better understand this process, techniques capable of probing the solvated state are consequently required. Smallangle scattering (SAS) has a proven ability to detect and characterize solutions, but it is rarely applied to more complex assembly shapes. Here, small-angle X-ray and neutron scattering are applied to observe toroidal assemblies in solution. Combined analysis confirms that the toroids have a core–shell structure, with a p-conjugated core and an alkyl shell into which solvent penetrates. The dimensions determined by SAS agree well with those obtained by (dried-state) atomic force microscopy. Increasing the number of naphthalene units in the molecular building block yields greater rigidity, as evidenced by a larger toroid and a reduction in solvent penetration into the shell. The detailed structural analysis demonstrates the applicability of SAS to monitor complex solution-based selfassembly. KW - Nanorings KW - Self-assembly KW - Small-angle scattering KW - Supramolecular chemistry KW - Toroids PY - 2016 U6 - https://doi.org/10.1002/anie.201603370 SN - 1433-7851 SN - 1521-3773 IS - 128 SP - 10044 EP - 10047 PB - Wiley-VCH Verlag GmbH CY - Weinheim AN - OPUS4-37144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Shebanova, O. A1 - Sutter, J. P. A1 - Hermida-Merino, D. A1 - Smales, Glen Jacob A1 - Terrill, N. J. A1 - Thünemann, Andreas A1 - Bras, W. T1 - Extending SAXS instrument ranges through addition of a portable, inexpensive USAXS module N2 - Ultra-SAXS can enhance the capabilities of existing SAXS/WAXS beamlines and laboratory instruments. A compact Ultra-SAXS module has been developed, which extends the measurable q-range with 0:0015 < q 1/nm) < 0:2, allowing structural dimensions between 30 < D(nm) < 4000 to be probed in addition to the range covered by a high-end SAXS/WAXS instrument. By shifting the module components in and out on their respective motor stages, SAXS/WAXS measurements can be easily and rapidly interleaved with USAXS measurements. KW - Small-angle scattering PY - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-504867 UR - https://arxiv.org/abs/1904.00080 SN - 2331-8422 SP - 1 EP - 25 PB - Cornell University CY - Ithaca, NY AN - OPUS4-50486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Anker, A. S. A1 - Annadurai, V. A1 - Balazs, D. M. A1 - Bienert, Ralf A1 - Bouwman, W. G. A1 - Breßler, Ingo A1 - Breternitz, J. A1 - Brok, E. S. A1 - Bryant, G. A1 - Clulow, A. J. A1 - Crater, E. R. A1 - De Geuser, F. A1 - Del Giudice, A. A1 - Deumer, J. A1 - Disch, S. A1 - Dutt, S. A1 - Frank, K. A1 - Fratini, E. A1 - Garcia, P. R. A. F. A1 - Gilbert, E. P. A1 - Hahn, Marc Benjamin A1 - Hallett, J. A1 - Hohenschutz, M. A1 - Hollamby, M. A1 - Huband, S. A1 - Ilavsky, J. A1 - Jochum, J. K. A1 - Juelsholt, M. A1 - Mansel, B. W. A1 - Penttilä, P. A1 - Pittkowski, R. K. A1 - Portale, G. A1 - Pozzo, L. D. A1 - Rochels, L. A1 - Rosalie, Julian M. A1 - Saloga, Patrick E. J. A1 - Seibt, S. A1 - Smith, A. J. A1 - Smith, G. N. A1 - Spiering, G. A. A1 - Stawski, Tomasz M. A1 - Taché, O. A1 - Thünemann, Andreas A1 - Toth, K. A1 - Whitten, A. E. A1 - Wuttke, J. T1 - The human factor: results of a small-angle scattering data analysis round robin N2 - A round-robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%. Due to the added complexity of the structure factor, far fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 and 86%, respectively. This round-robin experiment highlights several causes for the discrepancies, for which solutions are proposed. KW - Round Robin KW - Data analysis KW - Small-angle scattering KW - Nanomaterials KW - Interlaboratory comparability KW - Nanostructure quantification KW - Methodology KW - MOUSE PY - 2023 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-587091 VL - 56 IS - 6 SP - 1618 EP - 1629 PB - International Union of Crystallography (IUCr) AN - OPUS4-58709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -