GLY CaHD CPMG v1 (Kay 2009)

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Basic facts about CaHD_cpmg_GLY_dfh_600_v1

Synopsis: 2D 13C,1H correlation to observe exchange with CPMG at Glycine Cα sites, with selection of CHD and suppression of CH2 moieties

Family: CPMG relaxation dispersion

Sample requirements: U-13C, 50% D isotope labeling

Code authors:

 D. Flemming Hansen, Lewis E. Kay

Copyright: L.E. Kay, University of Toronto

Instructions

Flags and loops

  • dm = 'nnny', dmm = 'cccp' 13C decoupling during acquisition
  • dm2 = 'nnnn', dmm2 = 'cccp'.
  • phase = 1,2 for States-TPPI acquisition in t1 13C
  • fsat - water presaturation
  • fscuba - SCUBA Hα recovery under water presaturation, fsat must be ='y' for scuba to work
  • f1180 - start t1 at halfdwell
  • ncyc - number of cpmg cycles
  • ncyc_dipfinal < 3 - number of times to repeat dipsi-2 program for 1H-13C cross polarisation

Delays

  • time_equil - equilibration time
  • time_T2 < 40 ms - total time for CPMG trains
  • taua - slightly < 1/4JCH
  • taub - 1/4JCH

1H channel

Carrier at HDO signal ~ 4.77 ppm.

Pulses & power levels:

  • pw @ tpwr  : hard pulse - max power
  • pw_dip @ t_dip : hetCP dipsi-2 transfer (around 33 us)
  • pwsl @ tpwrsl : spinlock during carbon CPMG.

13C channel

Carrier at 43.9 ppm.

Pulses & power levels:

  • pw_dip @ dpwr_dip - 13C pulse length and power for dipsi hetCP transfer (pw_dip is common for 1H and 13C
  • pwc @ dhpwr: hard 13C 90o pulse
  • pwc_cp @ dpwr_cp: 90o pulses flanking the CPMG period
  • pwc_ca @ d_ca, phase_ca (phase adjustment), shape = RF_CO_Ca_burp_600_v3: selective (Ca && !CO) pulses
  • pwc_reb (<2.750 ms) @ d_reb, shape=shp_reb: A selective Re-burp pulse (Ca(gly) && !Cb(!gly))
  • 1/dmf @ dpwr: 13C decoupling during acquisition
  • 1./dmf_co @ dpwrcodec, dresco, pattern - codecseq: low power adiabadic CO decoupling (e.g. WURST-2) during indirect acquisition

2H channel

Carrier at 4.0 ppm (middle of Gly Hα region)

Pulses & power:

  • pwd @ dpwr3_D
  • pwd1 @ dpwr3

PFG

Pulses & levels:

  • gt0 @ gzlvl0
  • gt1 @ gzlvl1
  • gt2 @ gzlvl2
  • gt3 @ gzlvl3
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