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We demonstrate that two-dimensional solid-state NMR chemical-shift correlation spectra can be recorded under low-power conditions. Except for the cross-polarization period, no rf-field amplitudes above 40 kHz are used. Such experiments require the use of fast (>50 kHz) magic-angle spinning (MAS). A comparison with the high-power version of the experiment(More)
Recent developments in sample rotation technology have had a profound impact on magic-angle-spinning NMR. First, rotation frequencies approaching, and even exceeding, strong homonuclear spin interactions have made high-resolution solid-state (1)H spectroscopy much more accessible. Second, the new concept of fast rotation sweep spectroscopy has emerged.(More)
Resolution in 1H NMR spectra of solids can be significantly enhanced with fast magic-angle spinning and high magnetic fields. A variable field and spinning speed study up to 25 T and 40 kHz shows that the homogeneous line broadening is inversely proportional to the product of magnetic field strength and spinning speed. The combination of high field and fast(More)
Low-power XiX proton decoupling under fast magic-angle spinning is introduced. The method is applicable if the MAS frequency exceeds the proton-proton interactions. For rigid organic solids this is the case for MAS frequencies above approximately 40 kHz. It is shown that the quality of the decoupling as well as the sensitivity to frequency offsets can be(More)
We present an overview of solid-state NMR studies of endohedral H(2)-fullerene complexes, including (1)H and (13)C NMR spectra, (1)H and (13)C spin relaxation studies, and the results of (1)H dipole-dipole recoupling experiments. The available data involves three different endohedral H(2)-fullerene complexes, studied over a wide range of temperatures and(More)
We have observed 1H NMR spectra of hydrogen molecules trapped inside modified fullerene cages under cryogenic conditions. Experiments on static samples were performed at sample temperatures down to 4.3 K, while magic-angle-spinning (MAS) experiments were performed at temperatures down to 20 K at spinning frequencies of 15 kHz. Both types of NMR spectra show(More)
The 23Na magic-angle spinning (MAS), double rotation (DOR) and multiple-quantum magic-angle spinning (MQMAS) NMR spectra of anhydrous sodium pyrophosphate, Na4P2O7, measured at five different Larmor frequencies (nuL) ranging from 105.8 MHz (corresponding to 400 MHz 1H frequency) to 211.6 MHz (800 MHz) are analysed and the complete set of NMR parameters(More)
Chemical structure of human bone mineral was studied by solid-state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS). Trabecular and cortical bone samples from adult subjects were compared with mineral standards: hydroxyapatite (HA), hydrated and calcined, carbonatoapatite of type B with 9 wt% of CO 3 2− (CHA-B), brushite (BRU) and mixtures(More)
We present an approach that accelerates protein solid-state NMR 5-20-fold using paramagnetic doping to condense data-collection time (to approximately 0.2 s per scan), overcoming a long-standing limitation on slow recycling owing to intrinsic (1)H T(1) longitudinal spin relaxation. Using low-power schemes under magic-angle spinning at 40 kHz, we obtained(More)
We discuss a simple approach to enhance sensitivity for (13)C high-resolution solid-state NMR for proteins in microcrystals by reducing (1)H T(1) relaxation times with paramagnetic relaxation reagents. It was shown that (1)H T(1) values can be reduced from 0.4-0.8s to 60-70 ms for ubiquitin and lysozyme in D(2)O in the presence of 10 mM Cu(II)Na(2)EDTA(More)