Search results for "Nuclear magnetic resonance"

Resorcinarene Bis-Thiacrowns: Prospective Host Molecules for Silver Encapsulation

2012

Mixed-donor atom tetramethoxy resorcinarene bis-thiacrown hosts, in which the crown unit contains both hard oxygen and soft sulfur donor atoms, were synthesized for soft metal cation binding. The binding properties were investigated both in solution and in the solid state by NMR spectroscopy and X-ray crystallography. It was found that the resorcinarene bis-thiacrowns were able to complex silver cations with remarkable affinity forming readily 1:2 host–guest complexes in solution. The solid state structures also revealed that the bis-thiacrowns form silver complexes in an unanticipated endo- and exo-cavity fashion within the same host molecule. Both the solution and solid state studies indi…

Cation binding resorcinarene bis-crowns: the effect of lower rim alkyl chain length on crystal packing and solid lipid nanoparticles

2012

A group of seven resorcinarene bis-crown ethers (CNBC5) with two polyether bridges at the upper rim and either propyl, butyl, pentyl, heptyl, nonyl, decyl or undecyl groups at the lower rim were synthesized and their binding properties with Cs+ were investigated by NMR titration. The bis-crowns form 1:2 complexes with Cs+ with binding constants of logK 4–5. Crystal structures of bis-crowns and their Cs+ and K+ complexes were studied and different packing motifs were found depending on the alkyl chain length. Short ethyl, propyl and butyl alkyl chains gave a layer or pillar packing where the polar and non-polar regions cannot be distinguished, whereas longer pentyl and decyl chains formed bi…

Re-investigation of the conformational interconversion of the 1,2,3,6,7,8-hexahydropyrene cation radical by EPR, ENDOR and TRIPLE spectroscopy

1985

The conformational interconversion of the 1,2,3,6,7,8-hexahydropyrene cation radical has been re-examined by EPR, ENDOR and TRIPLE spectroscopy, and the Arrhenius plot is presented for a wider temperature range than that used earlier. The EPR spectra were measured from 143 to 369 K and the ENDOR spectra from 143 to 263 K. The thermodynamic constants of the conformational interconversion of the cation radical were determined on the basis of the temperature-dependent spectra. The high-resolution spectra clearly show that there are two overlapping spectra at low temperature, and this is confirmed by simulation.

Cyclic heptapeptides from the soil-derived fungus Clonostachys rosea

2019

Abstract Three new cyclic heptapeptides (1–3) together with three known compounds (4–6) were isolated from a solid rice culture of the soil-derived fungus Clonostachys rosea. Fermentation of the fungus on white beans instead of rice afforded a new γ-lactam (7) and a known γ-lactone (8) that were not detected in the former extracts. The structures of the new compounds were elucidated on the basis of 1D and 2D NMR spectra as well as by HRESIMS data. Compounds 1 and 4 exhibited significant cytotoxicity against the L5178Y mouse lymphoma cell line with IC50 values of 4.1 and 0.1 µM, respectively. Compound 4 also displayed cytotoxicity against the A2780 human ovarian cancer cell line with an IC50…

Comparison between room-temperature susceptometry and MRI with respect to the cell-specific detection of liver iron

2018

Characterization by solid-state NMR and selective dissolution techniques of anhydrous and hydrated CEM V cement pastes.

2010

International audience; The long term behaviour of cement based materials is strongly dependent on the paste microstructure and also on the internal chemistry. A CEM V blended cement containing pulverised fly ash (PFA) and blastfurnace slag (BFS) has been studied in order to understand hydration processes which influence the paste microstructure. Solid-state NMR spectroscopy with complementary X-ray diffraction analysis and selective dissolution techniques have been used for the characterization of the various phases (C3S, C2S, C3A and C4AF) of the clinker and additives and then for estimation of the degree of hydration of these same phases. Their quantification after simulation of experime…

Crystal structure and magnetic properties of Cu(TIM)CuBr4: An alternating site-alternating exchange chain system

2007

Abstract The title compound, Cu(TIM)CuBr4 (where TIM is a macrocycle ligand) is a member of the Cu(TIM)MX4 family, which contains linear chain structures with ⋯ Cu ⋯ X – M – X ⋯ Cu ⋯ X – M - ⋯ linkages. This chain structure defines an alternating exchange/alternating site 1d system. For M=Cu, alternating FM/AFM chains are formed with JFM>| JAFM|. Structural and magnetic data are presented, along with an analysis of the exchange pathways.

Junceosides A-C, new triterpene saponins from Arenaria juncea.

2002

Three novel triterpenoid saponins, junceosides A (1), B (2), and C (3), together with two known saponins have been isolated from the roots of Arenaria juncea. Their structures were elucidated using a combination of homo- and heteronuclear 2D NMR techniques (COSY, TOCSY, NOESY, HSQC, and HMBC) and by FABMS. The new compounds were characterized as 3-O-alpha-L-arabinopyranosyl-(1-->2)-[beta-D-galactopyranosyl-(1-->3)]-beta-D-glucuronopyranosylgypsogenin-28-O-beta-D-glucopyranosyl(1-->3)-[beta-D-xylopyranosyl-(1-->4)]-alpha-L-rhamnopyranosyl-(1-->2)-beta-D-fucopyranoside (1), 3-O-alpha-L-arabinopyranosyl-(1-->2)-[beta-D-galactopyranosyl-(1-->3)]-beta-D-glucuronopyranosylgypsogenin-28-O-beta-D-x…

A method for measurement of spin-spin couplings with sub-mHz precision using zero- to ultralow-field nuclear magnetic resonance.

2017

We present a method which allows for the extraction of physical quantities directly from zero- to ultralow-field nuclear magnetic resonance (ZULF NMR) data. A numerical density matrix evolution is used to simulate ZULF NMR spectra of several molecules in order to fit experimental data. The method is utilized to determine the indirect spin-spin couplings ($J$-couplings) in these, which is achieved with precision of $10^{-2}$--$10^{-4}$ Hz. The simulated and measured spectra are compared to earlier research. Agreement and precision improvement for most of the $J$-coupling estimates are achieved. The availability of an efficient, flexible fitting method for ZULF NMR enables a new generation of…

Measuring molecular parity nonconservation using nuclear-magnetic-resonance spectroscopy

2017

The weak interaction does not conserve parity and therefore induces energy shifts in chiral enantiomers that should in principle be detectable in molecular spectra. Unfortunately, the magnitude of the expected shifts are small and in spectra of a mixture of enantiomers, the energy shifts are not resolvable. We propose a nuclear magnetic resonance (NMR) experiment in which we titrate the chirality (enantiomeric excess) of a solvent and measure the diasteriomeric splitting in the spectra of a chiral solute in order to search for an anomalous offset due to parity nonconservation (PNC). We present a proof-of-principle experiment in which we search for PNC in the \textsuperscript{13}C resonances…