# 1 "/u/exp/stan/nmr/lists/pp/hncof.s" ;hncof.fa ;3D HNCO - with Watergate reverse INEPT (FHSQC) and minimal H2O saturation. ;This version makes use of the gp gradient syntax. ;Kay, Xu, and Ymazaki, J. Magn. Reson. A 10l, 129-133 (1994) ;Mori et al., J. Magn. Reson. B 108, 94-98 (1995) ;Bruker Avance/Xwin-nmr version ;Written up by F. Abildgaard, NMRFAM (abild@nmrfam.wisc.edu) ; ; $Id: pulseprogram,v 1.1 2021/02/11 00:42:44 bmrbsvc Exp $ ; ; Disclaimer: This pulse program is provided "as is" for your ; information. Support for the use of this pulse program is only ; provided to users of the National Magnetic Resonance Facility ; at Madison (NMRFAM). Users of this pulse program employ it at ; their own risk. Neither NMRFAM nor University of Wisconsin-Madison ; are liable for any physical or other damage incurred during the ; use of this pulse program. ; ;f1: 1H, f2: 15N, f3: 13C (channel assignments may be changed below) ;o1p: 4.7ppm ;o2p: 118ppm, ;o3p: use fq3list fahncof.C (175ppm,56ppm) ; ;d1: relaxation delay = d1+0.1s ;p1 90 H at pl1 ;p11 90 2.0 ms H1 semi-selective H2O flip-back pulse at power: ; 1) pl21 (zgsel1.fa), with phcor21; ; 2) pl22 (zgsel2.fa), with phcor22. ; Check for a possible phase difference between hard H1 and soft H1 ; pulses and set phcor21 and phcor22 accordingly. ;p10 90 H at pl10 (H1 composite decoupling) ;p2 90 N at pl2. If p5/2 > p2 define SHORT_P2 below. ;p3 90 CO at pl3 ; semi-selective: p90=sqrt(15)/(4*dNu), dNu=(175ppm-55ppm)*bf3); 64.4us at 500MHz ;p5 180 Ca square shaped (spnam5) at power sp5, offset Ca-CO (-120ppm) ; semi-selective: p180=sqrt(3)/(2*dNu), dNu=(175ppm-55ppm)*bf3); 57.6us at 500MHz ;p8 180 CO square shaped (spnam8) at power sp8, offset CO-Ca (120ppm) ; semi-selective: p180=sqrt(15)/(2*dNu), dNu=(175ppm-55ppm)*bf3); 128.8us at 500MHz ;pl0 120dB ;d21: 1/(2*dNu), dNu=(ChSh(NH)-ChSh(H2O))*bf1, 300us at 500MHz ; ;H1 Waltz-16x or DIPSI-2x (cpdprg1), using p90 (PCPD) at pl10 ;N15 Waltz-16 (cpdprg2), 90 dgr pulse (PCPD) at pl12 ;Ca on-resonance SEDUCE1 decoupling of Ca, using p90 (PCPD) at sp3, ; shape seduce1, offset 0, cpdprg3 waltz16sp3. ;N15 evolution: ; in10=in30, SW(N)=1/(2*in10), typ. 35-40 ppm ; l4 complex points; max. is (d10/in10)+1 ; N15 chemical shift axis has reverse orientation ;C13 evolution: ; in0, SW(C)=1/(2*in0), typ. 15 ppm ; l6 complex points ; set cnst0 to 0 (preferably) or 1 to make d0 the smallest possible ; positive delay. cnst0=0 gives (90,-180) phase distortion in F1. ; cnst0=1 gives (270,-540) phase distortion in F1 (use LP to correct). ; C' chemical shift axis is OK ;ns=8, 16, ..., ds=8, 16,... ; ;Recommendations for triple-axis (single-axis) gradients: ;gpz1: 15% (15%) ;gpz2: 6% (6%) ;gpz3: 15% (15%) ;gpz4: -8% (-8%) ;gpz5: 15% (15%) ;gpz6: 12% (12%) ;gpx7: 54%, adjust for magic-angle (0%) ;gpz7: 30% (55%) ;gpnam1: sine.100 ;gpnam2: sine.50 ;gpnam3: sine.100 ;gpnam4: sine.100 ;gpnam5: sine.50 ;gpnam6: sine.50 ;gpnam7: sine.100 ; ;Define one or more of the following options to tailor this pulse program ; to your specific needs. ; ;#define ONE_D ; uncomment for 1D experiment ;#define SHORT_P2 ; uncomment if p5/2 > p2 ; ; the correct expt time (works with XWIN-NMR 2.x) ; ;Define channel assignments: ; ;You shouldn't have to worry about anything beyond this point :-) ; ;sanity checks ; # 99 "/u/exp/stan/nmr/lists/pp/hncof.s" ; ; define delay TAUA define delay TAUA2 define delay TAUA7 define delay TAUB define delay TAUC define delay TAUW define delay TAUW1 define delay CEN_HN1 define pulse GRAD1 define pulse GRAD2 define pulse GRAD3 define pulse GRAD4 define pulse GRAD5 define pulse GRAD6 define pulse GRAD7 define pulse H1_90 define pulse H1_180 define pulse H1_S90 define pulse N15_90 define pulse N15_180 define pulse CA_180 define pulse CO_90 define pulse CO_180 define pulse CAO_180 define pulse COA_180 "d11=100m" ;disk i/o "d12=10u" ;power switching etc. "d13=5u" ;just a short delay "d14=40u" ;ip,id etc "d16=300u" ;gradient recovery "H1_90=p1" "H1_180=H1_90*2" "H1_S90=p11" "N15_90=p2" "N15_180=N15_90*2" "CO_90=p3" "CO_180=CO_90*2" "CAO_180=p5" "COA_180=p8" "GRAD1=700u" "GRAD2=500u" "GRAD3=1.0m" "GRAD4=1.0m" "GRAD5=600u" "GRAD6=500u" "GRAD7=700u" "d6=H1_90" "TAUW=d21" "TAUW1=(TAUW/2)-N15_90" "TAUA=2.3m" "TAUA2=TAUA-GRAD2-d13-d16" "TAUA7=TAUA-TAUW*2.5-H1_90*2.385-GRAD7-d16-d13" "TAUB=5.4m" "TAUC=12.4m" "d24=TAUC-TAUB-p10-d13*2-d12" "d10=12.4m" "d30=12.4m-TAUB-COA_180-p10-d12*3-d13*5" "d0=((cnst0*2+1)*in0-CO_90*1.273-CAO_180-N15_180-d12*2-d13*2)/2" # 172 "/u/exp/stan/nmr/lists/pp/hncof.s" "CEN_HN1=N15_90-H1_90" "d31=2*(TAUA2+GRAD2+TAUB+TAUA7+GRAD7+2*TAUW+TAUW1)+GRAD1+GRAD3+TAUC+GRAD4+GRAD5+GRAD6" # 1 "/u/exp/stan/nmr/lists/pp//Avance.incl" ;Avance.incl ; ;version 99/08/02 # 191 "/u/exp/stan/nmr/lists/pp/hncof.s" # 1 "/u/exp/stan/nmr/lists/pp//Grad.incl" ;Grad.incl - include file for Gradient Spectroscopy ;avance-version ;version 99/02/19 define list EA= # 192 "/u/exp/stan/nmr/lists/pp/hncof.s" 1 ze 2 d13 do:f2 d11 setnmr2^0 d14 3 d14 d14 d14 d14 4 d14 d14 d14 5 d14 d14 d14 6 d14 # 1 "/u/exp/stan/nmr/lists/pp//faexptcorr.incl" ; This is here to trick "expt" to calculate the experiment time ; correctly. if "1 == 1" goto nod31 d31 nod31, d13 # 210 "/u/exp/stan/nmr/lists/pp/hncof.s" d1 pl1:f1 pl2:f2 ;-------------------- set carbon freq. on CO --------------- 50u fq3:f3 d13 setnmr2|0 d13 setnmr0|34 (N15_90 ph0):f2 d13 GRAD1:gp1 ;400u, 10G/cm d16 pl3:f3 ;--------------------- INEPT to f2 -------------------------- (H1_90 ph0):f1 d13 GRAD2:gp2 ;500u, 4G/cm d16 TAUA2 (CEN_HN1 H1_180 ph0):f1 (N15_180 ph0):f2 TAUA2 d13 GRAD2:gp2 ;500u, 4G/cm d16 (H1_90 ph1):f1 d13 d12 pl22:f1 (H1_S90 ph22:r):f1 ;2ms 90 H1 pulse at phase x d13 GRAD3:gp3 ;1.0m, 10G/cm d16 ;----------------- INEPT to f3' and refocus H --------------- (N15_90 ph11):f2 TAUB d13 \n d12 pl10:f1 \n p10:f1 ph1 \n d13 cpds1:f1 d24 (N15_180 ph0):f2 (TAUC) (d13 CO_180 ph0):f3 (N15_90 ph0):f2 d13 do:f1 \n p10:f1 ph3 \n d13 \n d12 pl1:f1 d13 GRAD4:gp4 ;1.0m, -5G/cm d16 ;----------------------- f3' evolution ------------------------ (CO_90 ph12):f3 d13 d12 pl0:f3 (d0 CAO_180:sp5 ph0):f3 (d13 N15_180 ph0 d0):f2 d12 pl3:f3 # 263 "/u/exp/stan/nmr/lists/pp/hncof.s" (CO_90 ph0):f3 d13 GRAD5:gp5 ;600u, 10G/cm ;--------------------- Switch f3 frequency to Ca -------------- d16 fq3:f3 d12 pl0:f3 d13 \n d12 pl10:f1 \n p10:f1 ph1 \n d13 cpds1:f1 d13 \n d12 pl0:f3 \n d13 cpds3:f3 ;------ Refocus f3' and constant time evolution on N (t2) ----- (N15_90 ph14):f2 d10 (N15_180 ph15):f2 d13 do:f3 d12 pl0:f3 (COA_180:sp8 ph0):f3 d13 \n d12 pl0:f3 \n d13 cpds3:f3 d30 d13 do:f1 \n p10:f1 ph3 \n d13 \n d12 pl1:f1 TAUB (N15_90 ph0):f2 d13 do:f3 d13 GRAD6:gp6 ;500u, 8G/cm d16 pl21:f1 (H1_S90 ph21:r):f1 ;2ms 90 H1 pulse at phase x d13 d12 pl1:f1 (H1_90 ph2):f1 d13 TAUA7 GRAD7:gp7 ;700u, 40G/cm d16 (H1_90*0.231 ph1):f1 TAUW (H1_90*0.692 ph1):f1 TAUW (H1_90*1.462 ph1):f1 TAUW1 (N15_180 ph0):f2 TAUW1 (H1_90*1.462 ph3):f1 TAUW (H1_90*0.692 ph3):f1 TAUW (H1_90*0.231 ph3):f1 d13 GRAD7:gp7 ;700u, 40G/cm d16 pl12:f2 TAUA7 d6 setnmr0^34 go=2 ph31 cpds2:f2 # 319 "/u/exp/stan/nmr/lists/pp/hncof.s" d11 do:f2 wr #0 if #0 zd d13 setnmr2^0 d14 ip14 lo to 3 times 2 d14 dd10 d14 id30 d14 ip31 d14 ip31 lo to 4 times l4 d14 rd10 d14 rd30 # 335 "/u/exp/stan/nmr/lists/pp/hncof.s" d14 ip12 lo to 5 times 2 d14 id0 d14 ip31 d14 ip31 lo to 6 times l6 exit ph0=0 ph1=1 ph2=2 ph3=3 ph11=0 2 ph12=0 0 0 0 2 2 2 2 ph14=0 ph15=0 0 2 2 ph16=0 ph21=0 ph22=0 ph31=0 2 0 2 2 0 2 0