300 instrument

¹H and ¹³C NMR spectra were obtained using a Bruker 300 instrument, and chemical shifts are reported in ppm on the δ scale relative to TMS, TSP, or solvent. Electrospray iodization (ESI) high resolution mass spectra (HRMS) were obtained on JEOL double sector JMS-AX505HA mass spectrometer (University of Notre Dame, IN). Analytical SE-HPLC was performed on an Agilent 1200 (Agilent, Santa Clara, CA) equipped with a diode array detector (λ = 254 and 280 nm), with the themostat set at 35°C. All absorbance measurements for the protein concentration and ligand protein ratio were obtained on an Agilent 8453 diode array UV-Vis spectrometer equipped with an 8-cell transport system (designed for 1 cm cells).

¹H and ¹³C NMR spectra were obtained using a Bruker 300 instrument and chemical shifts are reported in ppm on the δ scale relative to TMS or solvent. Electrospray iodization (ESI) high resolution mass spectra (HRMS) were obtained on JEOL double sector JMS-AX505HA mass spectrometer (University of Notre Dame, IN). Structure determination of compound 5a was conducted using SMART V5.054 (Bruker Analytical X-ray Systems, Madison, WI) at the X-Ray Crystallographic Laboratory (Department of Chemistry, University of Minnesota). Analytical chiral HPLC was performed on an Agilent 1200 (Agilent, Santa Clara, CA) equipped with a diode array detector and a column (Chiralpak® AD-H, 4.6 × 150 mm, 80Å). Enantiomeric excess of optically active compounds (20 μL, 1 mg of sample in 1 mL of hexanes) was determined by chiral HPLC (isocratic, 230 nm) using the following chromatographic conditions: method A (1/99 = i-PrOH/Hexanes at a flow rate of 0.5 mL/min, 30 min); method B (1/99 = i-PrOH/Hexanes at a flow rate of 1 mL/min, 15 min); method C (10/90 = i-PrOH/Hexanes at a flow rate of 0.5 mL/min, 60 min); method D (8/92 = i-PrOH/Hexanes at a flow rate of 0.5 mL/min, 160 min); method E (0.2/99.8 = i-PrOH/Hexanes at a flow rate of 0.5 mL/min, 15 min); method F (3/97 = i-PrOH/Hexanes at a flow rate of 1 mL/min, 15 min). Optical rotation was determined using JASCO P-2000 polarimeter.

¹H and ¹³C NMR spectra were obtained using a Bruker 300 instrument, and chemical shifts are reported in ppm on the δ scale relative to TMS or solvent. Fast atom bombardment (FAB) high resolution mass spectra (HRMS) were obtained on JEOL double sector JMS-AX505HA mass spectrometer (University of Notre Dame, IN). Analytical HPLC was performed on Agilent 1200 (Agilent, Santa Clara, CA) equipped with a diode array detector (λ = 254 and 280 nm), thermostat set at 35 °C and a Zorbax Eclipse XDB-C18 column (4.6 × 150 mm, 80Å, Agilent, Santa Clara, CA). The mobile phase of a binary gradient (0–100%B/40 min; solvent A = 0.05 M AcOH/Et₃N, pH 6.0; solvent B = CH₃CN for method 1). Enantiomeric excess of optically active compounds (20 µL, 1 mg of sample in 1 mL of hexanes) was determined by chiral HPLC (Chiralpak® AD-H, 4.6 × 150 mm, 80Å) using the following chromatographic conditions: method 2 (binary isocratic, 1% i-PrOH/Hexanes, 15 min, λ = 230 nm, flow rate = 1.0 mL/min) or method 3 (binary isocratic, 30% i-PrOH/Hexanes, 20 min, λ = 230 nm, flow rate = 1.0 mL/min). Optical rotation of chiral molecules was determined using JASCO P-2000 polarimeter.

¹H, ¹³C, and DEPT NMR spectra were obtained using a Bruker 300 instrument and chemical shifts are reported in parts per million (ppm) on the δ scale relative to TMS. Electrospray (ESI) high-resolution mass spectra (HRMS) were obtained on JEOL double sector JMS-AX505HA mass spectrometer (University of Notre Dame, South Bend, IN). ⁹⁰Y (0.05M HCl) and ¹⁷⁷Lu (0.05M HCl) were purchased from Perkin Elmer.