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A new goniometer for single-crystal nuclear magnetic resonance (NMR) spectroscopy has been constructed and built into a multinuclear X–1H double-tuned probe for cross-polarization and/or 1H decoupling. Improvements in the ease of mounting/remounting the crystal on the three rotational axes and in the accuracy of the stepwise rotation about these axes have been achieved compared to the usual cube goniometer. A similar improvement is achieved for the determination of the orientation of the crystal relative to the goniometer frame. The NMR goniometer has three dovetail mortises that enable rotation of the crystal about three orthogonal axes, all perpendicular to the magnetic field. The crystal is glued onto a tenon that fits precisely into the dovetails of the NMR goniometer and also into a slightly modified x-ray diffraction goniometer, thereby allowing a high-accuracy determination of the orientation for the tensorial NMR interactions with respect to the crystal frame. The performance of the goniometer is illustrated by single-crystal 23Na NMR spectra of NaNO3.

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The construction of a single-crystal nuclear magnetic resonance (NMR) probe with a new two-axis geometry for the goniometer has improved the sensitivity of the NMR response from small crystals. This allows studies of the smallest crystals used so far in single-crystal NMR. The goniometer of the probe uses only two different mountings of the crystal, and the rotation axis of the goniometer is tilted 45° with respect to the direction of the magnetic field. By moving the goniometer outside the radio frequency coil, the filling factor and the probe sensitivity increase. The improved sensitivity for the probe is illustrated by the P-{H1}31 cross-polarization spectrum of a 0.088 mm3 crystal of (NH4)2HPO4 and a Rb87 single-pulse spectrum of a 0.048 mm3 crystal of RbZn2(HPO4)PO4. Moreover, the capability to determine precise parameters for the solid-state NMR interactions using the new probe is demonstrated by Na23 and Rb87 single-crystal studies of NaNO3 and RbClO4.