Mechanochemical and solution synthesis, X-ray structure and IR and 31P solid state NMR spectroscopic studies of copper(i) thiocyanate adducts with bulky monodentate tertiary phosphine ligands

The aim of this critical review is to provide a broad but digestible overview of mechanochemical synthesis, i.e. reactions conducted by grinding solid reactants together with no or minimal solvent. Although mechanochemistry has historically been a sideline approach to synthesis it may soon move into the mainstream because it is increasingly apparent that it can be practical, and even advantageous, and because of the opportunities it provides for developing more sustainable methods. Concentrating on recent advances, this article covers industrial aspects, inorganic materials, organic synthesis, cocrystallisation, pharmaceutical aspects, metal complexes (including metal-organic frameworks), supramolecular aspects and characterization methods. The historical development, mechanistic aspects, limitations and opportunities are also discussed (314 references). This journal is © The Royal Society of Chemistry 2012

Two-dimensional correlated spectroscopy (COSY) is used for measurements of proton-proton spin-spin coupling constants in protein 1H NMR spectra. High digital resolution along the frequency axis omega 2 is achieved by placing the carrier frequency in the center of the spectrum, using quadrature detection in both dimensions and presenting the spectrum in the phase sensitive mode. Compared to other techniques for studies of spin-spin coupling constants, COSY provides greatly improved spectral resolution. This is illustrated by experiments with H2O solutions of the small globular protein BUSI IIA (bull seminal inhibitor IIA).