3D NMR
Band-selective 13C pulses

The band-selective13C pulse calibrations should be done in the inverse mode (13C through the 2nd channel) using the pulse sequence decp90sp and decp180sp, respectively. (see Tutorial: Pulse Calibrations). You also calculate the values by using the shape tool in XWINNMR, stdisp. For instance, a sample of 0.1 M CH3OH-13C in DMSO-d6. can be used. The 13C-offset for the methyl group in methanol is 49 ppm, the methyl 1H-offset is 3.28 ppm and the one-bond coupling constant is 142 Hz. The calibration affords an antiphase signal that its intensity depends on the flip angle of the selective 13C-pulse. When the 13C-pulse is a perfect 90-pulse, the magnetization is completely converted to a multiple quantum coherence and the obseved signal reaches its minimum.

You can also calculate the values by using the shape tool in XWINNMR, stdisp

Selective excitation

Acquisition parameters for band-selective 13C 90 degree pulse calibration.

PULPROG: decp90sp
NUC1: 1H nucleus on f1 channel
O1P: 3.5 ppm 1 H offset 
NUC2: 13C nucleus on f2 channel
O2P: 49 ppm 
13C: offset 
NS: 1 
DS: 0
CNST2: 139
PL2: 120dB
P13: selective pulse length (409us, e.g.) 
SP2: dB power level for selective pulse
SPNAM2: G4.256
SPOAL2: 0.5
SPOFF2: 0.0

  • 13C 90deg shaped pulse name (spnam2=G4.256), length (p13=409u), and power (sp2) applied on-resonance. When applied off-resonance, the pulse is specified with sp4, p13=409u and spnam4=G4.256.
  • 13C 90deg time-reversed shaped pulse name (spnam8=G4tr.256), length (p13), and power (sp8)
  • Selective inversion

    Acquisition parameters for band-selective 13C 1800 degree pulse calibration. If the selective 13C-pulse, applied after the 180- 1H-pulse, is a perfect 180-pulse, the magnetization stays as multiple quantum coherence and the observable signal is minimal.

    PULPROG: decp180sp pulse program 
    NUC1: 1H nucleus on f1 channel
    O1P: 3.5 ppm 1 H offset 
    NUC2: 13C nucleus on f2 channel
    O2P: 49 ppm 
    13C: offset 
    NS: 2 
    DS: 2
    CNST2: 139
    PL2: 120dB
    P13: selective pulse length (256us, e.g.) 
    SP3: dB power level for selective pulse
    SPNAM3: G3.256 
    SPOAL3: 0.5
    SPOFF3: 0.0 
    

  • 13C 180deg shaped pulse name (spnam3=G3.256), length (p14=256u), and power (sp3) usually applied on CA/CB resonances. Otherwhise, when applied off-resonance, is specified with sp5/sp7.
  • 13C 180deg shaped pulse name applied exclusively on CA resonances (spnam9), length p24=768u, and power (sp9)
  • Selective decoupling

    Selective decoupling is applied on the alpha-carbon region (centered at 52 ppm) during the constant time evolution of the 15N-magnetization, in order to ensure that the scalar coupling between 13C a and amide 15N does not evolve. The frequency offset is given through the parameter SPOFF15 which should be given a negative value, in Hz, corresponding to the difference 173-52 ppm=121 ppm of 13C at the field you are working at.

  • 13C 180deg decoupling shaped pulse name applied exclusively on CA resonances (spnam15=g3.256), length pcpd2=768u, and power (sp15=pl12) using cpdprg2=mlevsp180
  • This is an example of carbon pulses defined in edprosol: