Heteronuclear dipolar decoupling in solid-state nuclear magnetic resonance under ultra-high magic-angle spinning

We compare in this communication several heteronuclear dipolar decoupling sequences in solid-state nuclear magnetic resonance experiments under a magic-angle spinning frequency of 60 kHz. The decoupling radiofrequency field amplitudes considered are 190 and 10 kHz. No substantial difference was found among the sequences considered here in performance barring the difference in the optimisation protocol of the various schemes, an aspect that favours the use of swept-frequency two pulse phase modulation (SW(f)-TPPM).     

Experimental realization of constant current device using hydrogen bond ferroelectric liquid crystals

The European Physical Journal E - Magnetorheological fluid (MRF) is a smart responsive fluid, when exposed to the magnetic field, reflects a noticeable transformation in fluid viscosity due to the...     

An analysis of phase-modulated heteronuclear dipolar decoupling sequences in solid-state nuclear magnetic resonance

The design of variants of the swept-frequency two-pulse phase modulation sequence for heteronuclear dipolar decoupling in solid-state NMR is reported, their performance evaluated, and compared with other established sequences like TPPM and SPINAL. Simulations performed to probe the role of the homonuclear (1)H-(1)H bath show that the robustness of the decoupling schemes improves with the size of the bath. In addition, these simulations reveal that the homonuclear (1)H-(1)H bath also leads to broad baselines at high MAS rates. Results from a study of the SPINAL decoupling scheme indicate that optimisation of the starting phase and phase increment improves its performance and efficiency at high MAS rates. Additionally, experiments performed on a liquid crystal display the role of the initial phase in SPINAL-64 and sequences in the SW(f)-TPPM family.     

Experimental study on novel phase change composites for thermal energy storage

Journal of Thermal Analysis and Calorimetry - In this study, beeswax is studied as a phase change material (PCM) to store heat due to its high latent heat. The disadvantages of using beeswax were...     

New trends in sustainable nanocatalysis: Emerging use of earth abundant metals

Noble metals are well-known to afford highly active, selective and durable catalysts, and have thus been at the core of the development of greener processes. In recent years, however, growing concerns about their scarcity, cost and toxicity has triggered research efforts towards the development of earth-abundant catalysts. In this Current Opinion, recent examples of the use in catalysis of pure earth-abundant metals, earth-abundant metals with minute quantities of noble metals, or earth-abundant metals activated by light are presented. This highlight article showcases the current trends in sustainable organic transformations, catalyzed by nanomaterials.     

Effect of heterocyclic ring system on formation of dimeric quinolones under catalyst-free conditions: a green approach

The intermediate-dependent green and efficient synthesis of dimeric quinolones 4a–l and 7a–l by the Knoevenagel condensation followed by Michael-type addition of 4-hydroxy-1-methylquinolin-2(1H)-one 1a, b to indole-3-aldehydes 2a–f and aromatic aldehydes 5a–l in water through the condensed compound 3a–l under catalyst-free conditions is described. This reaction was found to be environmentally friendly, has easy-workup and shorter reaction times giving good yields of the product without the need for its isolation using column chromatography.     

Nickel-catalyzed Negishi cross-coupling reactions of secondary alkylzinc halides and aryl iodides

A general Ni-catalyzed process for the cross-coupling of secondary alkylzinc halides and aryl/heteroaryl iodides has been developed. This is the first process to overcome the isomerization and β-hydride elimination problems that are associated with the use of secondary nucleophiles, and that have limited the analogous Pd-catalyzed systems. The impact of salt additives was also investigated. It was found that the presence of LiBF(4) dramatically improves both isomeric retention and yield for challenging substrates.     

Photocatalytic splitting of CS2 to S8 and a carbon-sulfur polymer catalyzed by a bimetallic ruthenium(II) compound with a tertiary amine binding site: toward photocatalytic splitting of CO2?

The catalytic photocleavage of CS(2) to S(8) and a (C(x)S(y))(n) polymer with visible light using a dinuclear ruthenium(II) compound with a bipyridine units for photoactivity and a vicinal tertiary amine binding site for CS(2) activation was studied. The catalyst was characterized by X-ray diffraction, (1)H NMR, and (13)C NMR, ESI-MS and elemental analysis. CS(2) photocleavage was significant (240 turnovers, 20 h) to yield isolable S(8) and a (C(x)S(y))(n) polymer. A mononuclear catalyst or one without an amine binding site showed significantly less activity. XPS of the (C(x)S(y))(n) polymer showed a carbon/sulfur ratio ～1.5-1.6 indicating that in part both C-S bonds of CS(2) had been cleaved. Catalyst was also included within the polymer. The absence of peaks in the (1)H NMR verified the (C(x)S(y))(n) nature of the polymer, while (13)C NMR and IR indicated that the polymer had multiple types of C-S and C-C bonds.     

A new diacylated labdane diterpenoid from Andrographis wightiana

A new acylated labdane diterpenoid, 14-deoxy-3,19-diacetyl-11,12-didehydroandrographolide (1), together with three known labdane diterpenoids, wightionolide (2), andrographolide (3) and neoandrographolide (4), and three known flavones, echioidinin (5), skullcapflavone I 2'-methyl ether (6) and echioidin (7), were isolated from the whole plant of Andrographis wightiana. The structure of compound 1 was elucidated by 1D and extensive 2D-NMR spectral studies.