I am sometimes asked to acquire 13C NMR spectra of highly paramagnetic compounds. Those of you attempting to acquire such spectra for the first time should be aware of the following:
1. You should use a large spectra width as the 13C chemical shifts can be very extreme. In order to get a wide uniform excitation, use very short high power pulses.
2. Both the T1's and the T2's are short, so you can use short acquisition times and short recycle delays.
3. The 1H chemical shift range for paramagnetic compounds can span hundreds of ppm. The 1H decoupling schemes used to collect 13C data do not permit such a broad decoupling bandwidth and you may have to collect several 13C spectra with different 1H offsets. It is always best to collect a proton spectrum first to evaluate the 1H decoupling needs in the 13C spectrum.
4. The lines are often very broad and therefore many scans are needed to build up the signal-to-noise ratio.
5. The 2H lock signal may be shifted by the paramagnetic compound, so don't be surprised if your automatic locking routines do not work.