Five new polyfluoroalcohols, HOC (cyclo-C6H11) 2 (CF3), HO (cyclo-C6H11)(CF3) 2, HOC (2, 4, 6-C6H2 (CF3) 3)(CF3) 2, HOC (4-Si (i-Pr) 3-2, 6-C6H2 (CF3) 2)(CF3) 2, and HOC (3, 5- C6H3 (CH3) 2)(CF3) 2, have been synthesized, and new procedures with improved yields for two known polyfluoroalcohols (HOC (cyclo-C6H11)(CF3) 2, HOC (4-C6H4 (t-Bu))(CF3) 2) have been developed. Variable temperature 19F NMR spectra and the X-ray structure of ...