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Biomolecular NMR - Experiments

  • Selectively methyl 13C-labled proteins are used.

 

NMR ExperimentsBruker Sequences
HMQC with 3919 hmqcgpph19.x
Acquires 2D; F2(1H) - F1(13C)
Uses Watergate 3919, (from Y. Xia)
NOESY-HMQC with 3919 noesyhmqc3d19.x2
Acquires 2D; F3(1H) - F2(13C) - F1(1H)
Uses Watergate 3919, (from Y. Xia)
Methyl HMQC CPMG Exchange
H1-C13 DQ relaxation dispersion
Korzhnev et al (2004) JACS 126, 3964
hmqcmerex3dsk
Acquires pseudo3D; F3(1H) - F2(13C) - F1(vdlist) Coded in TopSpin 2
d21; the total relaxation time (<= 0.04)
vd in vdlist; loop counter during d21 and vd max. = d21/1ms
t _cpmg = d21/(vd*4)
n _cpmg = 1/(4* t _cpmg = vd/d21
Ex) vdlist = 2, 4, 6 .... 40 for d21=0.04s
Methyl HSQC CPMG Exchange
C13 SQ relaxation dispersion
Lundstrom et al(2007) JBNMR 38, 79
methyl_rex3dsk
Acquires pseudo3D; F3(1H) - F2(13C) - F1(vdlist) d22; the total relaxation time (<= 0.1)
vd in vdlist; n _cpmg (RF field stregnth), vd max. = 1000
t _cpmg = 1/(vd*4)
Ex) vdlist = 20, 40, 60 .... 1000 for d22=0.1s
Methyl DQ/SQ Relaxation
Sun et al (2011) JPC B 115, 14878
Kay et al (2007) JACS 129, 1743
methyl_DQSQ3d_sk
Acquires Pseudo-3D; F3(1H)-F2(13C)-F1(vdlist)
Uses vdlist for variable relaxation times (s)
Vdlist must have two duplicate values for SQ and DQ signals
Methyl TQ/SQ Relaxation
Sun et al (2011) JPC B 115, 14878
Kay et al (2007) JACS 129, 1743
methyl_TQSQ3d_sk
Acquires Pseudo-3D; F3(1H)-F2(13C)-F1(vdlist)
Uses vdlist for variable relaxation times (s)
Vdlist must have two duplicate values for SQ and TQ signals
Minimum NS is 48 to satisfy 16 for SQ and 24 for TQ.
Methyl zz-exchange methyl_zzex3d_sk
Acquires Pseudo-3D; F3(1H)-F2(13C)-F1(vdlist)
Uses vdlist for variable relaxation times (s)
L2=1; relaxation (zzex) period before 13C t1-evolution, no zzex peaks
L2=2; relaxation (zzex) period after 13C t1-evolution, zzex peaks

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molecule v3

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