Spatially multiplexed single-molecule translocations through a nanopore at controlled speeds.

In current nanopore-based label-free single-molecule sensing technologies, stochastic processes influence the selection of translocating molecule, translocation rate and translocation velocity. As a result, single-molecule translocations are challenging to control both spatially and temporally. Here we present a method using a glass nanopore mounted on a three-dimensional nanopositioner to spatially select molecules, deterministically tethered on a glass surface, for controlled translocations. By controlling the distance between the nanopore and glass surface, we can actively select the region of interest on the molecule and scan it a controlled number of times and at a controlled velocity. Decreasing the velocity and averaging thousands of consecutive readings of the same molecule increases the signal-to-noise ratio by two orders of magnitude compared with free translocations. We demonstrate the method's versatility by assessing DNA-protein complexes, DNA rulers and DNA gaps, achieving down to single-nucleotide gap detection.

Synergy of diffraction and spectroscopic techniques to unveil the crystal structure of antimonic acid.

The elusive crystal structure of the so-called 'antimonic acid' has been investigated by means of robust and state-of-the-art techniques. The synergic results of solid-state magic-angle spinning nuclear magnetic resonance spectroscopy and a combined Rietveld refinement from synchrotron X-ray and neutron powder diffraction data reveal that this compound contains two types of protons, in a pyrochlore-type structure of stoichiometric formula (H3O)1.20(7)H0.77(9)Sb2O6. Some protons belong to heavily delocalized H3O+ subunits, while some H+ are directly bonded to the oxygen atoms of the covalent framework of the pyrochlore structure, with O-H distances close to 1 Å. A proton diffusion mechanism is proposed relying on percolation pathways determined by bond-valence energy landscape analysis. X-ray absorption spectroscopy results corroborate the structural data around Sb5+ ions at short-range order. Thermogravimetric analysis and differential scanning calorimetry endorsed the conclusions on the water content within antimonic acid. Additional 0.7 water molecules per formula were assessed as moisture water by thermal analysis.

A comprehensive examination of the local- and long-range structure of Sb6O13 pyrochlore oxide.

The crystal structure of the Sb6O13 oxide, exhibiting a defect pyrochlore crystal structure with atomic vacancies, has been studied using a complete set of state-of-the-art techniques. The degree of antimony disproportionation in Sb3+ and Sb5+ valence states has been directly determined around 36% and 64%, respectively, using X-ray absorption near edge structure (XANES). These findings are in excellent agreement with our Rietveld analysis of synchrotron X-ray (SXRD) and neutron powder diffraction (NPD) results. Moreover, the highly distorted Sb3+ coordination due to its lone electron pair has been critically revisited. The bonding distances and coordination of Sb3+ and Sb5+ species closely agree with an extensive dynamic and crystallographic determination using the Extended X-ray Absorption Fine Structure (EXAFS) technique. Most importantly, the specific local disorder of the two distinctive Sb ions has been crosschecked monitoring their unusual Debye-Waller factors.

Simultaneous direct high-performance liquid chromatographic enantioseparation of 2-methylglycidol-1-benzyl ether and 2-methylglycerol-1-benzyl ether using a solvent-switching technique.

Simultaneous HPLC separation of the enantiomers of 3-benzyloxy-2-methyl-1,2-propanediol and the corresponding 3-benzyloxy-2-methyl-1,2-propene oxide could be accomplished on amylose derived Chiralpak AD switching between 10% 2-propanol and 3% 1,2-dimethoxyethane as polar modifier in n-heptane.