UltraLow temperature NMR experiments
Description: By using liquid nitrogen as a cooling source, the extremely low temperature solution NMR is feasible, with caution and with hardware availability
Instrument:Bruker Avance III 600 MHz equipped with 5mm BBI probe
Experiments: 1D 1H and 13C, and 2D COSY, HSQC, HMBC, NOESY, etc.
- Northwestern. Juricek, M.; Strutt, N. L.; Barnes, J. C.; Butterfield, A. M.; Dale, E. J.; Baldridge, K. K.; Stoddart, J. F.; Siegel, J. S. Induced-fit catalysis of corannulene bowl-to-bowl inversion. Nature Chem. 2014, 6, 222-228
- UIUC. Andy A. Thomas and Scott E. Denmark, Pre-transmetalation intermediates in the Suzuki-Miyaura reaction revealed: The missing link. Science 2016, 352, 329-332.
- Acetone-d6 m.p. -94C
- Ethanol-d6 m.p. -114C
- Methanol-d4 m.p. -98C
- THF-d8 m.p. -108C
- Toluene-d8 m.p. -95C
Bismuth (Bi 209) NMR:
Prof. Danna Freedman group has been extensively performing Bi 209 NMR on our Inova 500 MHz system.
Given that the bismuth 209 frequency (80.3 MHz on I500) is so close to deuterium (76.7 MHz on I500), most of our newer instruments can’t do Bi209 NMR without hardware reconfiguration. That’s why we set up this on I500, which is relatively easier to change the hardware settings.
Once the probe is tuned to Bi209, you can simply load the default parameter set to run your sample. Please contact Yongbo/Yuyang for help if you are interested in doing this. Right figure is a bismuth NMR spectrum collected on I500 for Bi(NO3)3 in D2O/DCl with 10 seconds acquisition time, courtesy of Prof. Freedman group: