We report two-dimensional (2D) O-17 multiple-quantum magic-angle spinning (MQMAS) NMR spectra for four O-17-labeled organic compounds: [O-17(2)]-D-alanine (1), potassium hydrogen [O-17(4)]dibenzoate (2), [O-17(4)]D,L-glutamic acid.HCl (3) and [2,4-O-17(2)]uracil (4). The high spectral resolution observed in-the 2D O-17 MQMAS NMR spectra allows extraction of precise O-17 NMR parameters for all crystallographically distinct oxygen sites. We demonstrate that rotor synchronization is important in obtaining high-quality O-17 MQMAS spectra for organic compounds. Several issues related to the potential of O-17 MQMAS NMR for large biomolecular, systems are also discussed.