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- HPβCD Milwaukee, WI, , USA : Aldrich Chemical Co. . and HDCA (Sigma Chemical Co., St. Louis, MO, USA) were used as received from the manufacturers. The inclusion complex was prepared at a 1:1 molar ratio of HDCA to HPβCD. Typically, 1.38 g (1 mM) of HPβCD was dissolved at room temperature in 50 mL of water to which 30 mL of ethyl alcohol containing 392 mg (1 mM) of HDCA was added. The solution was evaporated immediately after its preparation under vacuum in a rotary evaporator (model R-114; Büchi, Buchs, Switzerland) at a temperature of 45°C. 1H and 13C NMR spectra were obtained at 303 K using a Bruker AMX-400 WB spectrometer operating at 400.13 and 100.61 MHz, respectively, on 3 10−2 M CD3OD solutions. δ values refer to internal CHD2OD and 13CD3OD set to 3.30 and 49.3 ppm, respectively. Typical digital resolution was × 0.1 and × 0.3 Hz for 1H and 13C NMR spectra, respectively. Conditions for ROESY8 phase-sensitive spectrum via time-proportional phase incrementation (TPPI) were: presaturation of residual HDO signal during relaxation delay 0.5 s; mixing time 200 ms; spin-lock field 4000 Hz; spectral width 9 ppm; 4096 complex points in f2; 256 t1 values and 192 scans per t1 value, total acquisition time: 18 hours. Lorentz-Gauss enahancement (LB= −0.5; GB=0.01) in f1 and square-sine function (SSB=2) in f2 were applied before Fourier transformation.
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