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Simultaneous SAXS and SANS Analysis for the Detection of Toroidal Supramolecular Polymers Composed of Noncovalent Supermacrocycles in Solution

DOI: 10.1002/anie.201603370 DOI Help

Authors: Martin J. Hollamby , Keisuke Aratsu (Graduate School of Engineering, Chiba University) , B R. Pauw (BAM Federal Institute for Materials Research and Testing) , Sarah Rogers (ISIS Pulsed Neutron and Muon Source) , Andrew J. Smith (Diamond Light Source) , Mitsuaki Yamauchi (Graduate School of Engineering, Chiba University) , Xu Lin (Graduate School of Engineering, Chiba University) , Shiki Yagai (Graduate School of Engineering, Chiba University)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Angewandte Chemie International Edition

State: Published (Approved)
Published: July 2016
Diamond Proposal Number(s): 11969

Abstract: Molecular self-assembly primarily occurs in solution. To better understand this process, techniques capable of probing the solvated state are consequently required. Small-angle 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 π-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 self-assembly.

Journal Keywords: nanorings; self-assembly; small-angle scattering; supramolecular chemistry; toroids

Subject Areas: Chemistry, Materials, Technique Development

Instruments: I22-Small angle scattering & Diffraction

Other Facilities: ISIS