Milligram amounts of the new compounds 1,9- and 1,7-C60F(C-3) (ca. 85:15 mixture of isomers) and C60F3(CF3) were isolated from a high-temperature C-60/K2PtF6 reaction mixture and purified to 98 mol % compositional purity by two-dimensional high-performance liquid chromatography using Buckyprep and Buckyclutcher columns. The previously observed compounds C60F5(CF3) and C60F7(CF3) were also purified to 90+ mol % for the first time. Variable-temperature F-19 NMR spectra of the mixture of C60F(CF3) isomers and the previously reported mixture of C-s- and C-1-C60F17(CF3) isomers demonstrate for the first time that fullerene(F)(n)(CF3)(m) derivatives with adjacent F and CF3 substituents exhibit slow-exchange limit hindered CF3 rotation spectra at -40 +/- 10 degrees C. The experimental and density functional theory (DFT) predicted Delta H double dagger values for CF3 rotation in 1,9-C60F(CF3) are 46.8(7) and 46 M mol(-1), respectively. The DFT-predicted Delta H double dagger values for 1,7-C60F(CF3), C-s-C60F17(CF3), and C-1-C60F17(CF3) are 20, 44, and 54 kJ mol(-1), respectively. The (>= 4)J(FF) values from the slow-exchange-limit F-19 spectra, which vary from ca. 0 to 48(1) Hz, show that the dominant nuclear spin-spin coupling mechanism is through-space coupling (i.e., direct overlap of fluorine atom lone-pair orbitals) rather than coupling through the sigma-bond framework. The (2)J(FF) values within the CF3 groups vary from 107(1) to 126(1) Hz. Collectively, the NMR data provide an unambiguous set of (>= 4)wJ(FF) values for three different compounds that can be correlated with DFT-predicted or X-ray diffraction derived distances and angles and an unambiguous set of (2)J(FF) values that can serve as an internal standard for all future JFF calculations.