# 1 "/Bruker/35/exp/stan/nmr/lists/pp/ty_CNOESY_wide" ;ko_CHSQC 2D 1H-13C HSQC experiment (DRX version) ; T. Kigawa 960605 ; S. Koshiba 010404 ;2D 1H-13C HSQC experiment for 13C/15N-labelled samples ;dissolved in H2O. ;With 13CO CPD and a 15N 180 pulse ;during t1(13C) evolution period. ;Two spin locking pulses (x,y) immediately after acqu. -> removed ;A 1H 90 degree pulse is added immediately prior to acqu. ;in order to rotate any residual H2O resonances to the z axis. ; ;F1: 1H [p1(90deg,pl1)] ;F2: 15N [p21(90deg,pl4)] ;F3: 13C [p13(90deg,pl2), PCPD2(90deg,pl12,CDP,GARP)] ; [p14(90deg,pl7,SHAPE,SQ)] ;With 6 gradient pulses: ;(400u,+30)*2, (2.5m,+50), (4.0m,-50), (400u,+30)*2 # 1 "/Bruker/35/exp/stan/nmr/lists/pp/Avance.incl" 1 ;Avance2.incl ; for 1 ; ;avance-version (03/02/17) ;$Id: pulseprogram,v 1.1 2021/02/10 23:29:54 bmrbsvc Exp $ # 19 "/Bruker/35/exp/stan/nmr/lists/pp/ty_CNOESY_wide" 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: pulseprogram,v 1.1 2021/02/10 23:29:54 bmrbsvc Exp $ # 20 "/Bruker/35/exp/stan/nmr/lists/pp/ty_CNOESY_wide" 2 # 1 "/Bruker/35/exp/stan/nmr/lists/pp/De.incl" 1 ;De.incl ; ;avance-version (02/05/31) define delay rde1 define delay rde2 define delay rderx define delay rdeadc define delay rdepa "rde1=de-de1" "rde2=de-de2" "rderx=de-derx" "rdeadc=de-deadc" "rdepa=de-depa" ;$Id: pulseprogram,v 1.1 2021/02/10 23:29:54 bmrbsvc Exp $ # 21 "/Bruker/35/exp/stan/nmr/lists/pp/ty_CNOESY_wide" 2 ;"p14=p24/2.0" "d5=p23/2-p1" "d15=p23/2-p21" ;"d8=p14-p1" ;"d9=p14-p21" "d6=(d3-p9-p16-400u-p10-p16-400u)/10-100u-p16" ; ;for gradient pulses ; "p15=400u" ; "p16=2.5m" ; "p17=4.0m" ;for 13C "d4=1.4m" "d2=d4-p15-100u" "d21=d4-p15-5u+p1*2/3.14" ;for AQ ;for t1 evolution ;"d0=in0*3.0-p13*2.0/3.14-p14" "d0=in0/2-p1*2/3.14" "d10=in10/2-p13*2.0/3.14-p1" ;"d0=4u" "l1=td1/2" "l2=td2/2" aqseq 312 ;pulse sequence. 30m do:f2 30m 1 ze 2 75m do:f2 3 30m 4 30m 5 30m 6 20u pl5:f1 (p7 ph0):f1 ; spin lock x (p8 ph7):f1 ; spin lock y 20u pl1:f1 20u pl3:f3 d1 (d5 p1 ph6 d0 d0 p1 ph0 d5):f1 (d0 p23:sp2 ph10):f2 (d0 d15 p21*2 ph10):f3 50u setnmr3|0 setnmr0|34|32|33 11 50u p16:gp0 50u d6 lo to 11 times 10 20u pl9:f1 (p9 ph0):f1 5u p16:gp5 400u pl11:f1 (p10 ph0):f1 5u p16:gp6 400u pl1:f1 ;********** INEPT 1H-15N. (p1 ph0):f1 ;========== 1st gradient pulse. 50u p15:gp1 ; 500u +30% 50u ;========== d2 pl2:f2 ; 13C power -> pl2 (d5 p1*2.0 ph0):f1 (p23:sp2 ph10):f2 ;========== 2nd gradient pulse. 50u p15:gp1 ; 500u +30% 50u ;========== d2 pl3:f3 ; 15N power -> pl3 (p1 ph1):f1 ;========== 3rd gradient pulse (homo-spoil). 50u p16:gp2 ; 2.5m +50% 50u ;========== t1 (15N) evolution. 100u pl2:f2 (p13 ph11):f2 d10 (p1*2.0 ph0):f1 d10 (p13 ph10):f2 ;========== 4th gradient pulse (homo-spoil). 50u p17:gp3 ; 4.0m -50% 50u ;========== 200u (p1 ph3):f1 ;========== 5th gradient pulse. 50u p15:gp4 ; 500u +30% 50u ;========== d2 (d5 p1*2.0 ph0):f1 (p23:sp2 ph10):f2 ;========== 6th gradient pulse (water-gate 2). 5u p15:gp4 ; 500u +30% d21 setnmr3^0 setnmr0^34^32^33 ; optimal for swh=11160.71,de=6 ;========= ;********** ; (p1 ph5):f1 ;------------------------ ; go=2 ph31 cpd2:f2 (de1 rde1 adc ph31 syrec) (de2 rde2 ph30:r):f1 (derx rderx setrtp1|1) (deadc rdeadc setrtp1|0|8) (depa rdepa setrtp1|2) (de) ; ph31 for adc, ph30 for f1 ; DE1 DE2 (de) ;(derx rderx setrtp1|1) (deadc rdeadc setrtp1|0|8) (depa rdepa setrtp1|2) 20u pl2:f2 cpdngs30:f1 (p13 ph10 5u p13 ph13):f2 5u vd (p23:sp2 ph10):f2 vd vd (p23:sp2 ph10):f2 vd 20u pl10:f2 4u cpds2:f2 aq 4u do:f2 4u ivd rcyc=2 60m do:f2 wr #0 if #0 zd 15m ip6 lo to 3 times 2 15m id0 15m ip31*2 lo to 4 times l1 15m rd0 15m ip11 lo to 5 times 2 15m id10 15m ip31*2 lo to 6 times l2 ;********** 30m setnmr3^0 setnmr0^34^32^33 30m exit ;phases for 1H pulses. ph0=0 ph1=1 1 3 3 ph3=0 ph5=0 0 0 0 2 2 2 2 ph6=0 0 0 0 2 2 2 2 ph7=1 ;phases for X pulses. ph10=0 ph11=0 2 ph13=0 0 2 2 ;phases for y pulse. ph20=0 ;phases for receiver. ph30=(360) 0 ph31=0 2 2 0 2 0 0 2 ; ;pl1 : 1H high power for p1 ;pl5 : 1H purge pulse (~25us for 90deg) ;pl3 : 15N high power for p21 ;pl2 : 13C high power for p13 ;pl7 : 13C power for p14,p24 (sp1) ;pl12: 13C CPD pulse for pcpd2 (~50us at 800MHz) ;pcpd2: 13C CPD pulse (~50us for 90deg at 800MHz) ; ;p1 : 1H 90 deg. (pl1) ;p7 : 1H 8ms (pl5) ;p8 : 1H 5ms (pl5) ;p21 : 15N 90 deg. (pl4) ;p13 : 13C 90 deg. (pl2) ;p14 : 13C 90 deg. (pl7,sp1) for 13CO decoupling ;p24 : 13C 180 deg. (pl7) ;d3 : mixing time ;gp0 : very very weak grad ;p9 : 2ms (pl9) ;p10 : 2.8ms (pl11)