;hCcHtocsy2D_CT_sel.mj ;2D methyl TOCSY experiment, John et al., 2007 ;format of a constant-time 13C-HSQC spectrum ;selective 13C excitation pulses for reduced 13C-sweepwidth in indirect dimension ;water suppression by 3-9-19 Watergate ;mixing time is d25 #include #include #include ;############# ASED parameters ################## ;in0 = 1/[2*SWH(13Cmethyl)] ;p1 = 90deg high power on 1H (f1, pl1) ;p3 = 90deg high power on 13C (f2, pl2) ;p9 >= 25u low power 90deg on 13C for TOCSY mixing (f2, pl15) ;p13 = 90deg selective 13C on methyl (1.5m Q5) ;spnam13 = Q5 ;spnam15 = Q5tr ;p16 >= 800u gradient pulse ;pcpd2 >80u 13C decoupler (pl12,f2) ;d2 = n/[2J(CC)] = 2*14m (half CT) ;d4 <= 1.8m (C-H evolution on H) ;d14 <= 750u (C-H evolution on C) ;d16 >= 100u (gradient recovery) ;d19 <= 2*DW (for 3-9-19) ;############# fixed parameters, do not change #### "p2=p1*2" "p0=p1*4/3" "p4=p3*2" "d0=3u" "d10=d0+p2+d2" "d11=10m" ;delay for phase and buffer incrementation "d12=d2-d14" "d24=d23-p16-d16" "d25=p9*217*cnst10" ;calculated mixing time define delay d4a ;compensated d4 J-evolution delays define delay d19a "d4a=500u" "d19a=d19-p3" "l10=cnst10" 1 ze d25 2 d1 do:f2 d11 pl1:f1 d11 pl2:f2 ;### Destroy boltzmann 13C polarization ### (p3 ph0):f2 p16:gp1*0.8 d16 ;### INEPT ### (p1 ph1) d4 (center (p2 ph1) (p4 ph1):f2 ) d4 (p1 ph2) 10u ;### Start of t1 on 13C ### (p13:sp13 ph5):f2 d0 d14 (p2 ph0):f1 d12 (p4 ph0):f2 d10 (p13:sp15 ph12):f2 10u p16:gp1*0.5 d16 pl15:f2 ;### Start of DIPSI3 mixing ### 9 (p9*2.722 ph7):f2 (p9*4.389 ph9):f2 (p9*2.778 ph7):f2 (p9*3.056 ph9):f2 (p9*0.333 ph7):f2 (p9*2.556 ph9):f2 (p9*4.000 ph7):f2 (p9*2.722 ph9):f2 (p9*4.111 ph7):f2 (p9*3.778 ph9):f2 (p9*3.889 ph7):f2 (p9*2.889 ph9):f2 (p9*3.000 ph7):f2 (p9*0.333 ph9):f2 (p9*2.500 ph7):f2 (p9*4.050 ph9):f2 (p9*2.830 ph7):f2 (p9*4.389 ph9):f2 (p9*2.722 ph9):f2 (p9*4.389 ph7):f2 (p9*2.778 ph9):f2 (p9*3.056 ph7):f2 (p9*0.333 ph9):f2 (p9*2.556 ph7):f2 (p9*4.000 ph9):f2 (p9*2.722 ph7):f2 (p9*4.111 ph9):f2 (p9*3.778 ph7):f2 (p9*3.889 ph9):f2 (p9*2.889 ph7):f2 (p9*3.000 ph9):f2 (p9*0.333 ph7):f2 (p9*2.500 ph9):f2 (p9*4.050 ph7):f2 (p9*2.830 ph9):f2 (p9*4.389 ph7):f2 (p9*2.722 ph9):f2 (p9*4.389 ph7):f2 (p9*2.778 ph9):f2 (p9*3.056 ph7):f2 (p9*0.333 ph9):f2 (p9*2.556 ph7):f2 (p9*4.000 ph9):f2 (p9*2.722 ph7):f2 (p9*4.111 ph9):f2 (p9*3.778 ph7):f2 (p9*3.889 ph9):f2 (p9*2.889 ph7):f2 (p9*3.000 ph9):f2 (p9*0.333 ph7):f2 (p9*2.500 ph9):f2 (p9*4.050 ph7):f2 (p9*2.830 ph9):f2 (p9*4.389 ph7):f2 (p9*2.722 ph7):f2 (p9*4.389 ph9):f2 (p9*2.778 ph7):f2 (p9*3.056 ph9):f2 (p9*0.333 ph7):f2 (p9*2.556 ph9):f2 (p9*4.000 ph7):f2 (p9*2.722 ph9):f2 (p9*4.111 ph7):f2 (p9*3.778 ph9):f2 (p9*3.889 ph7):f2 (p9*2.889 ph9):f2 (p9*3.000 ph7):f2 (p9*0.333 ph9):f2 (p9*2.500 ph7):f2 (p9*4.050 ph9):f2 (p9*2.830 ph7):f2 (p9*4.389 ph9):f2 lo to 9 times l10 ;### Methyl-selective transfer to 1H ### p16:gp1*0.7 d16 pl2:f2 (p13:sp13 ph0):f2 d14 (center (p2 ph0):f1 (p4 ph0):f2) d14 (p13:sp15 ph1):f2 10u ;### CH rephasing and watergate ### p16:gp1*0.6 ;z-spoil d16 (p1 ph0):f1 d4a p16:gp1*0.4 d16 (p1*0.231 ph14):f1 d19*2 (p1*0.692 ph14):f1 d19*2 (p1*1.462 ph14):f1 d19a (p4 ph0):f2 d19a (p1*1.462 ph15):f1 d19*2 (p1*0.692 ph15):f1 d19*2 (p1*0.231 ph15):f1 p16:gp1*0.4 d16 pl12:f2 d4a BLKGRAD ;### Start of data acquisition ### go=2 ph31 cpd2:f2 d11 do:f2 mc #0 to 2 F1PH(ip5, id0 & dd10) exit ph0= 0 ph1= 1 ph2= 2 ph5= 0 2 ;(C) t1 excitation pulse, States phase ph7= 1 ph9= 3 ph12= 1 1 3 3 ph14= {{0}*4}^2 ph15= {{2}*4}^2 ph20= 0 ph31= 0 2 2 0