Micro Crystalline Sponge Method Combined with Small-Wedge Synchrotron Crystallography for Nanogram Scale Molecular Structure Elucidation.

J Am Chem Soc

Department of Applied Chemistry, School of Engineering, The University of Tokyo, Mitsui Link Lab Kashiwanoha 1, FS CREATION, 6-6-2 Kashiwanoha, Kashiwa, Chiba 277-0882, Japan.

Published: July 2025


Category Ranking

98%

Total Visits

921

Avg Visit Duration

2 minutes

Citations

20

Article Abstract

The crystalline sponge (CS) method enables X-ray structural analysis without the requirement of crystallization of the target compound. However, several technical and crystallographic challenges, such as low guest occupancy, static disorder, and crystal degradation, continue to limit both the accuracy and the success rate of the method. In this study, we explored the downsizing of CS crystals to the range of 1-10 μm to improve data quality and reduce the amount of sample required. By employing the small-wedge synchrotron crystallography method, which utilizes synchrotron X-ray sources and data merging techniques, we achieved significant improvements in structural accuracy and broadened the method's applicability, even to trace samples at the nanogram level (∼3 ng).

Download full-text PDF

Source
http://dx.doi.org/10.1021/jacs.5c06360DOI Listing

Publication Analysis

Top Keywords

crystalline sponge
8
sponge method
8
small-wedge synchrotron
8
synchrotron crystallography
8
micro crystalline
4
method
4
method combined
4
combined small-wedge
4
crystallography nanogram
4
nanogram scale
4

Similar Publications

Single crystal diffraction is one of the most common and powerful tools for structural elucidation. However, obtaining single crystals of adequate size and quality is not always trivial. The "crystalline sponge" method has been used for crystallizing intrinsically amorphous compounds inside a metal organic framework,, but its application is limited by the size and stability of the pores within the networks.

View Article and Find Full Text PDF

Bioinspired Design of PVDF/SiO--PEGDA Membranes Via Vapor-Induced Phase Separation for Oil/Water Separation.

Langmuir

August 2025

Yunnan Key Laboratory of Crystalline Porous Organic Functional Materials, College of Chemical and Materials Engineering, Qujing Normal University, Qujing 655011, China.

The eco-friendly nature and energy efficiency of polymeric membranes have established them as pivotal materials for oil-in-water emulsion separation. However, persistent membrane fouling caused by oil deposition remains a major challenge, significantly hindering their practical implementation in industrial settings. In this work, thiol-ene photochemistry was employed to synthesize PEGylated silica nanoparticles (SiO--PEGDA) using poly(ethylene glycol) diacrylate (PEGDA) and hexanedithiol (HD) as monomers.

View Article and Find Full Text PDF

A Triple-Layered Composite Scaffold of Silk Fibroin and Decellularized Amniotic Membrane for Bladder Tissue Engineering.

Macromol Biosci

August 2025

Pediatric Urology and Regenerative Medicine Research Center, Gene, Cell and Tissue Research Institute, Tehran University of Medical Sciences, Tehran, Iran.

Augmentation cystoplasty has different side effects in urinary bladder reconstruction. Accordingly, it is necessary to develop substitutes using natural and synthetic biomaterials to address current problems. This study evaluates the potential of a triple-layered composite scaffold for bladder regeneration.

View Article and Find Full Text PDF

This study presents the development of a novel metal-organic framework (MOF) denoted as APF-80, suitable for the structural analysis of nucleophilic compounds that have traditionally been challenging to analyze using the crystalline sponge method. It was synthesized using a new mixed-substituent hexaazaphenalene ligand (344-TPHAP) featuring both 3-pyridyl and 4-pyridyl groups. This framework demonstrated remarkable stability toward nucleophilic molecules, which could be captured inside the pores through a synergistic combination of coordination and hydrogen-bonding interactions.

View Article and Find Full Text PDF

Boron beats nitrogen: strained boron-boron bonds as (molecular) proton sponges.

Phys Chem Chem Phys

August 2025

Departamento de Química, Módulo 13, Facultad de Ciencias, and Institute of Advanced Chemical Sciences (IAdChem), Universidad Autónoma de Madrid, Campus de Excelencia UAM-CSIC, Cantoblanco, 28049 Madrid, Spain.

Although boron usually behaves as a Lewis acid, some molecular structures containing B-B bonds can act as electron donors. Inspired in reported crystalline structures, the basicity and the hydrogen bond (HB) acceptor capability of diborane derivatives of dipyrazole 1 have been studied theoretically using M06-2x and CCSD(T) computational methods. The topology of the electron density and molecular electrostatic potential of compound 1 reveal that the richest electron region is located above the B-B bond, making it suitable to be a strong donor and a very effective proton catcher.

View Article and Find Full Text PDF