# 1 "/Bruker/35/exp/stan/nmr/lists/pp/ko_NOEHSQCN_Cdec3d.5" ;3D 15N-separated NOESY-HSQC with Water-flip backed HSQC experiment. ;ko_noehsqc3d 980218 ; modified for F3:15N version by koshiba 010503 ; modified for 13C decoupling version by koshiba 010910 ; modified for 13C decoupling using shaped pulses by koshiba 011229 ; modified for 13C decoupling using shaped pulses by koshiba 020208 ; ;F1:1H [p1,pl1@-1db ~10u ; [p5,pl5@40db ~1.0m for WFB ;F3:15N [p21,pl3@ ~40u] ; [pcpd3,pl13@ ~250u,WALTZ16 for decoupling] ; ;Gradient pulses (total: 6). "Sine100" or "Sine50" is used. ; p14:5.0m,gp0(spoil) +30 ; OPT ; p15:2.0m,gp1(spoil) +28 ; p16:3.0m,gp2(spoil) +30 ; p17:2.5m,gp3(spoil) -25 ; p18:1.0m,gp4(spoil) +30 ; p19:400u,gp5(echo) -15 ; p19:400u,gp5(echo) -15 ; ;Loop counter ;l2:1H ;l3:15N ; "l2=td1/2" "l3=td2/2" # 1 "/Bruker/35/exp/stan/nmr/lists/pp/Avance.incl" 1 ;Avance2.incl ; for 1 ; ;avance-version (03/02/17) ;$Id: Avance2.incl,v 1.7.2.3 2003/02/25 14:48:48 ber Exp $ # 30 "/Bruker/35/exp/stan/nmr/lists/pp/ko_NOEHSQCN_Cdec3d.5" 2 # 1 "/Bruker/35/exp/stan/nmr/lists/pp/Grad.incl" 1 ;Grad2.incl - include file for Gradient Spectroscopy ; for 1 ; ;avance-version (02/05/31) define list EA= ;$Id: Grad2.incl,v 1.7 2002/06/12 09:04:22 ber Exp $ # 31 "/Bruker/35/exp/stan/nmr/lists/pp/ko_NOEHSQCN_Cdec3d.5" 2 ;for Gradients ;"p14=5.0m" ;"p15=2.0m" ;"p16=3.0m" ;"p17=2.5m" ;"p18=1.0m" ;"p19=400u" ;defined parameters. "d2=2.25m" "d5=p21-p1" "d15=p23/2.0-p21" "d16=p23/2.0-p1" "d17=p24/2.0-p21" "d24=d2-p19-p5-125u" "d25=d2-p19-p5-p21*2.0-155u" ;"d25=d2-p19-p5-105u" "d23=p24/2.0-p1" ;for t1 evolution "d0=in0*0.5-p1*2.0/3.14" ;phase correction 90(+45),-180 ;"d0=4u" ;for t2(15N) evolution "d10=in10*0.5-p21*2.0/3.14" ; 90/-180 phase collection. ;"d10=4u" ;mixing time(d19=80ms) "d18=d19-p21-p13-p15-p16-2239u" ; mixinig delay ;pulse sequence. 30m setnmr3^0 setnmr0^34^32^33 1 ze 2 75m do:f3 3 15m 15m 4 15m 15m 5 15m 15m 6 20u 20u pl1:f1 20u pl15:f2 20u pl3:f3 d1 ; d1 = relax. delay - 150ms ; (p21 ph10):f3 ;OPTIONAL ;========== ;OPTIONAL ; 20u setnmr3|0 setnmr0|34|32|33 ; ; 5u ; ;OPTIONAL ; p14:gp0 ; PFG (homospoil) ;OPTIONAL ; 100u ;OPTIONAL ;========== ;OPTIONAL ; 500u ;OPTIONAL ;********** t1(1H) evolution. (d16 p1 ph1 d0 d0 p1 ph0 d16):f1 (d0 p23:sp2 ph20):f2 (d0 d15 p21*2.0 ph13):f3 ;********** Mixing period. 5u d18 ; mixing time. 20u setnmr3|0 setnmr0|34|32|33 ;========== 5u ; p15:gp1 ; PFG (homospoil) 100u pl2:f2 ;========== 1m (p21 ph10):f3 4u (p13 ph20):f2 ;========== 5u ; p16:gp2 ; PFG (homospoil) 100u pl17:f2 ;========== 1m ;********** INEPT 1H -> 15N. (p1 ph0):f1 d2 (d5 p1*2.0 ph2):f1 (p21*2.0 ph10):f3 d2 (p1 ph4):f1 5u 20u pl5:f1 (p5 ph5:r):f1 ; water-flip back ;========== 5u ; p17:gp3 ; PFG (homospoil) 50u ; ;========== t2 (15N) evolution. 1m pl1:f1 (d17 p21 ph11 d10 d10 p21 ph10 d17):f3 (d10 p24:sp1 ph20):f2 (d10 d23 p1*2.0 ph0):f1 ;========== 5u ; p18:gp4 ; PFG (homospoil) 50u ; ;========== 1m pl5:f1 (p5 ph7:r):f1 ; water-flip back 5u 20u pl1:f1 (p1 ph0):f1 ;========== 5u ; p19:gp5 ; PFG (echo) 95u ; ;========== d24 pl5:f1 (p5 ph8:r):f1 ; water-flip back 5u 20u pl1:f1 ; 1H power -> hl1 (d5 p1*2.0 ph3):f1 (p21*2.0 ph10):f3 5u 20u pl5:f1 ; 1H power -> hl3 (p5 ph8:r):f1 ; water-flip back ;========== 5u ; p19:gp5 ; PFG (echo) 95u ; ;========== d25 setnmr3^0 setnmr0^34^32^33 (p21 ph10 5u p21 ph14):f3 5u 20u pl13:f3 ;---------- Acquisition. go=2 ph31 cpd3:f3 60m do:f3 wr #0 if #0 zd 15m ip1*2 lo to 3 times 2 15m id0 15m ip31*2 lo to 4 times l2 15m rd0 15m ip11 lo to 5 times 2 15m id10 15m ip31*2 lo to 6 times l3 30m setnmr3^0 setnmr0^34^32^33 exit ;phases for 1H pulses. ph0=0 ph1=(8)7 3 ph2=1 ph3=2 ph4=1 1 1 1 3 3 3 3 ph5=(360) 0 ;x ph7=(360) 180 ;-x ph8=(360) 0 ;x ;phases for 15N pulses. ph10=0 ph11=0 0 2 2 ph13=3 1 ph14=0 0 0 0 2 2 2 2 ;phases for 13C pulses. ph20=0 ph21=1 ;--- Reciever Phase --- ph31=0 2 2 0 2 0 0 2 ;for 1H ;p1:1H 90deg hard pulse ~10u ;pl1:1H hard pulse ; ;p5:water flip back pulse ~1ms (phcor5,7,8) ;pl5:water flip back pulse ; ;d19:mixing time ; ;for 15N ;p21:15N 90deg hard pulse (~45us) ;pl3:15N hard pulse ;pl13:15N CPD pulse (pcpd3) ;pcpd3:15N CPD pulse (~250us) ; ;for 13C ;p13:13C 90deg hard pulse (~15us) ;pl2:13C hard pulse ;p23:13C 180deg shape pulse (0-140ppm) ;sp2:13C 180deg shape pulse (p23;ko_CRP80-) ;pl15:13C 180deg shape pulse (p23) (=sp2) ;p24:13C 180deg shape pulse (40-180ppm) ;sp1:13C 180deg shape pulse (p24;ko_CRP80-) ;pl17:13C 180deg shape pulse (p24) (=sp1)