;Pulse Program Code for Bruker: ;iINEPT-HSQC ;Shift Correlation version => cnst1= 0 ;J-resolved version =>cnst1= 1 ;F1-heterocoupled iINEPT HSQC by using initial 13C Boltzmann polarization ;for determination of 1J CH via splitting in F1 ;phase sensitive using Echo/Antiecho-TPPI gradient selection ;with decoupling during acquisition ;using shaped pulses for inversion and refocussing on f2 - channel ;using G_BIRD(r) to remove long range couplings in t1 ;with J scaling in t1 ;Measurement of individual 1J(CH) coupling constants in diastereotopic CH2 groups. ;Simultaneous sign-sensitive determination of 1J(CHA), 1J(CHB) and 2J(HH) from a single cross-peak. ;Simultaneous measurement of residual dipolar 1D(CH) and 2D(HH) couplings. ;J. Saurí, L.Castañar, P. Nolis, A. Virgili and T. Parella: Straightforward measurement of individual 1J(CH) and 2J(HH) in diastereotopic CH2 groups. ;J. Magn. Reson. 2014, 242, 33-40. http://dx.doi.org/10.1016/j.jmr.2014.02.003 ;$CLASS=HighRes ;$DIM=2D ;$TYPE= ;$SUBTYPE= ;$COMMENT= ;Avance III ;Topspin3.1 #include #include #include #include "p2=p1*2" "p4=p3*2" "d2=1s/(cnst2*2)" "d4=1s/(cnst2*4)" "d11=30m" "d0=3u" "d20=3u" "in0=inf1/2" "in20=in0*cnst16" "DELTA=d0*2+p2+p16+d16-p3*4/PI" "DELTA1=p16+d16-p3*4/PI" "DELTA2=d4-larger(p2,p14)/2" "DELTA3=d2-larger(p2,p39)/2" "DELTA4=d4-p16-d16-larger(p2,p14)/2" "acqt0=0" baseopt_echo 1 ze d12 do:f1 2 d11 do:f2 d12 pl11:f1 d1 cpd1:f1 d12 do:f1 d12 pl1:f1 d12 pl2:f2 UNBLKGRAD (p3 ph3):f2 if "cnst1==0" { d20 (p1 ph1) DELTA3 (center (p2 ph1) (p39:sp4 ph1):f2 ) DELTA3 (p1 ph1) d20 d0 (p2 ph1) d0 p16:gp1*EA d16 pl0:f2 (p39:sp4 ph14):f2 DELTA pl2:f2 } else { d0 (p1 ph1) DELTA3 (center (p2 ph1) (p39:sp4 ph1):f2 ) DELTA3 (p1 ph1) d0 p16:gp1*EA d16 pl0:f2 (p39:sp4 ph14):f2 DELTA1 pl2:f2 } (ralign (p3 ph4):f2 (p1*0.4 ph1):f1 ) DELTA2 pl0:f2 (center (p2 ph1) (p14:sp3 ph1):f2 ) DELTA4 pl12:f2 p16:gp2 d16 BLKGRAD go=2 ph31 cpd2:f2 d11 do:f2 mc #0 to 2 F1EA(calgrad(EA), caldel(d0, +in0) & caldel(d20, +in20) & calph(ph3, +180) & calph(ph31, +180)) exit ph1=0 ph2=1 ph3=0 2 ph4=0 0 2 2 ph14=0 0 2 2 ph31=0 2 2 0 ;pl0 : 120dB ;pl1 : f1 channel - power level for pulse (default) ;pl2 : f2 channel - power level for pulse (default) ;pl12: f2 channel - power level for CPD/BB decoupling ;sp3: f2 channel - shaped pulse 180 degree for inversion ;sp4: f2 channel - shaped pulse 180 degree for refocussing ;p1 : f1 channel - 90 degree high power pulse ;p2 : f1 channel - 180 degree high power pulse ;p3 : f2 channel - 90 degree high power pulse ;p14: f2 channel - 180 degree shaped pulse for inversion ; Crp60,0.5,20.1 ;p16: homospoil/gradient pulse ;p28: f1 channel - trim pulse ;p39: f2 channel - 180 degree shaped pulse for refocussing ; Bip720,100,10.1 (160us at 600.13 MHz) ;d0 : incremented delay (2D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d2 : 1/(2J)XH ;d4 : 1/(4J)XH ;d11: delay for disk I/O [30 msec] ;d16: delay for homospoil/gradient recovery ;inf1: 1/SW(X) = 2 * DW(X) ;in0: 1/(2 * SW(X)) = DW(X) ;nd0: 2 ;NS: 2 * n ;DS: >= 16 ;td1: number of experiments ;FnMODE: echo-antiecho ;cpd1: Saturation according to sequence defined by cpdprg1 [walt16] ;cpd2: decoupling according to sequence defined by cpdprg2 [p5m4sp180.2] ;pcpd1: f1 channel - 90 degree pulse for decoupling sequence ;pcpd2: f2 channel - 90 degree pulse for decoupling sequence ;cnst1: correlation (0)/J-resolved (1) ;cnst2: = J(XH) ;cnst16: = J(scale) factor ;use gradient ratio: gp 1 : gp 2 ; 80 : 20.1 for C-13 ; 80 : 8.1 for N-15 ;for z-only gradients: ;gpz1: 80% ;gpz2: 20.1% for C-13, 8.1% for N-15 ;use gradient files: ;gpnam1: SINE.100 ;gpnam2: SINE.100 ;preprocessor-flags-start ;LABEL_CN: for C-13 and N-15 labeled samples start experiment with ; option -DLABEL_CN (eda: ZGOPTNS) ;preprocessor-flags-end ;$Id: iINEPT,v 3.1 2014/10/10 16:34:30 lau Exp $