;noehncof.fa ;3D/4D NOE-HNCO - with Watergate reverse INEPT (3-9-19) and minimal H2O saturation. ;Zhang, Smithgall, Gmeiner, J. Magn. Reson. B 111, 305-309 (1996) ;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: noehncof.fa,v 1.2 1999/08/09 21:42:44 abild Exp abild $ ; ; 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) ;Gradient program: fanoehncof ;o1p: 4.7ppm ;o2p: 118ppm, ;use fq3list fanoehncof.C (56ppm,175ppm,56ppm) ; ;d1: relaxation delay = d1+0.1s ;p1 90 H at pl1 ;p10 90 H1 SEDUCE-1 shape at power sp1, offset 0, 2ms (if SHAPED defined), ; or p10 90 H1 weak regular pulse at power pl10, 2ms (if SHAPED not defined). ; Check for phase difference between hard H1 and soft H1 ; pulses and set ph21 accordingly. ;p11 90 H at pl11 ;p2 90 N at pl2 ;p3 90 CO at pl3 (semi-selective C13 90) ;p4 90 C at pl4 (non-selective C13 90, 16kHz at 500MHz) ;p5 180 Ca square shaped (spnam5) at power sp5, offset Ca-CO (-120ppm) ;p8 180 CO square shaped (spnam8) at power sp8, offset CO-Ca (120ppm) ;pl0 120dB ;d21: 1/(2*dNu), dNu=Nu(NH)-Nu(H2O), 280 us at 500 MHz ;d8: mixing time ; ;H1 Waltz-16x or DIPSI-2x (cpdprg1), using p90 (PCPD) at pl11 ;N15 Waltz-16 (cpdprg2), 90 dgr pulse (PCPD) at pl12 ;Ca on-resonance SEDUCE1 decoupling of Ca, using 90 dgr pulse (PCPD) at sp3, ; shape seduce1, offset 0, cpdprg3 waltz16sp3. ;N15 evolution: ; in10=in30, SW(N)=1/2*in10 ; l4 complex points; max. is (d10/in10)+1 ;C13 evolution: ; in0, SW(C)=1/2*in0 ; 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). ;H1 evolution: ; SW(N)=1/2*in20 ; set cnst2 to 0 (preferably) or 1 to make d20 the smallest possible ; positive delay: d20=((cnst2*2+1)*in20-(p1*1.273+p2*2))/2 ; l8 complex points ;ns=8, 16, ..., ds=8, 16,... ; ;Recommendations for gradients: ;p15=500u ;p16=1.0m ;p17=700u ;p18=1.0m ;p19=600u ;p20=3m ;cnst21=6% (4G/cm z) ;cnst22=15% (10G/cm z) ;cnst23=20% (40G/cm combined x,z) ;cnst24=-8% (-5G/cm z) ;cnst25=15% (10G/cm z) ;cnst26=15% (10G/cm z) ;cnst27=12% (8G/cm z) ;cnst30=1.800 (adjust) for magic angle gradient (Gx/Gz) or 0 for Gz only. ; ;#define ONE_D ; uncomment for 1D experiment ;#define N15_EVOL ; comment out for 2D/3D w/o N15 evolution #define CO_EVOL ; comment out for 2D/3D w/o C13 evolution #define H1_EVOL ; comment out for 2D/3D w/o H1 evolution ;#define SHAPED ; uncomment if using a shaped flip-back pulse ;#define SHORT_P2 ; uncomment if p5/2 > p2 #define EXPTCORR ; uncomment if you want "expt" to report ; ; the correct expt time (works with XWIN-NMR 2.x) ; ; ;Define channel assignments: #define H f1 #define N f2 #define C f3 ; ;You shouldn't have to worry about anything beyond this point :-) ; ;sanity checks ; #ifdef ONE_D #undef N15_EVOL #undef CO_EVOL #undef H1_EVOL #endif ; define delay TAUA1 define delay TAUA2 define delay TAUB define delay TAUC define delay TAUF define delay TAUM define delay TAUW define delay C_H_N define delay CEN_N_C define pulse H1_90 define pulse H1_180 define pulse H1_S90 define pulse N15_90 define pulse N15_180 define pulse C13_90 define pulse C13_180 define pulse CAO_180 define pulse CA_180 define pulse CO_90 define pulse CO_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=p1*2" "H1_S90=p10" "N15_90=p2" "N15_180=p2*2" "C13_90=p4" "C13_180=p4*2" "CAO_180=p5" "CO_90=p3" "CO_180=p3*2" "d6=H1_90" "TAUW=d21" "TAUA2=2.25m-TAUW*2.5-H1_90*2.385-p17-d16-d13" "TAUF=5.5m-p18-d13*2-d16" "TAUA1=2.25m-p15-d13-d16" "TAUB=5.4m" "TAUC=12.4m" "d24=TAUC-TAUB-p11-d13*2-d12" "d10=12.4m" "d30=12.4m-TAUB-p8-p11-d12*3-d13*5" #ifdef SHORT_P2 "CEN_N_C=p5*0.5-p2" #endif #ifdef CO_EVOL "d0=((cnst0*2+1)*in0-CO_90*1.273-CAO_180-d12*2-d13*2)/2" #endif "d22=(TAUW/2)-N15_90" "C_H_N=N15_90-H1_90" "TAUM=d8-p20-p16-d16*2-C13_90-d13" #ifdef H1_EVOL "d20=((cnst2*2+1)*in20-(H1_90*1.273+N15_180))/2" #endif #define SED_ON d13 \n d12 pl0:C \n d13 cpds3:C #define SED_OFF d13 do:C #define H1_DEC_ON d13 \n d12 pl11:H \n p11:H ph1 \n d13 cpds1:H #define H1_DEC_OFF d13 do:H \n p11:H ph3 \n d13 \n d12 pl1:H #ifdef EXPTCORR "d31=TAUM+2*TAUA1+2*TAUB+TAUC+2*TAUA2+4*TAUW" #endif #include #include 1 ze 2 d11 do:N d14 3 d14 d14 d14 d14 4 d14 d14 d14 5 d14 d14 d14 6 d14 d14 d14 7 d14 d14 d14 8 d14 LOCKH_OFF d1 pl1:H pl2:N ;-------------------- set carbon freq. on Ca --------------- 50u fq3:C 20u LOCKH_ON (N15_90 ph0):N d13 GRADIENT17(cnst26) ;400u, 10G/cm d16 pl4:C (H1_90 ph17):H #ifdef H1_EVOL d20 (N15_180 ph0):N (C13_90 ph0 d13 C13_180 ph1 d13 C13_90 ph0):C d20 #else d13 #endif (H1_90 ph0):H TAUM GRADIENT20(cnst22) ;3ms, 15G/cm d16 (C13_90 ph0):C d13 GRADIENT16(cnst21) ;1ms, 4G/cm d16 ;--------------------- INEPT to N -------------------------- (H1_90 ph0):H d13 GRADIENT15(cnst21) ;500u, 4G/cm d16 TAUA1 (C_H_N H1_180 ph0):H (N15_180 ph0):N TAUA1 d13 GRADIENT15(cnst21) ;500u, 4G/cm d16 (H1_90 ph1):H d13 #ifdef SHAPED d12 pl0:H (H1_S90:sp1 ph21):H ;2ms SEDUCE-1 90 H1 pulse at phase x #else d12 pl10:H (H1_S90 ph21):H ;2ms 90 H1 pulse at phase x #endif ;-------------------- set carbon freq. on CO --------------- d13 50u fq3:C d13 GRADIENT16(cnst22) ;1.0m, 10G/cm d16 ;----------------- INEPT to C' and refocus H --------------- (N15_90 ph11):N TAUB pl3:C H1_DEC_ON d24 (N15_180 ph0):N (TAUC) (CO_180 ph0):C (N15_90 ph0):N H1_DEC_OFF d13 GRADIENT18(cnst24) ;1.0m, -5G/cm d16 (CO_90 ph12):C ;----------------------- C' evolution ------------------------ d13 #ifdef CO_EVOL d0 d12 pl0:C #ifdef SHORT_P2 (CAO_180:sp5 ph0):C (CEN_N_C N15_180 ph0):N #else (CAO_180:sp5 ph0):C (N15_180 ph0):N #endif d0 d12 pl3:C d13 #endif (CO_90 ph0):C d13 GRADIENT19(cnst25) ;600u, 10G/cm ;--------------------- Switch C frequency to Ca -------------- d16 fq3:C d12 pl0:C H1_DEC_ON SED_ON ;------ Refocus C' and constant time evolution on N (t2) ----- (N15_90 ph14):N d10 (N15_180 ph15):N SED_OFF d12 pl0:C (p8:sp8 ph0):C SED_ON d30 H1_DEC_OFF TAUB (N15_90 ph0):N SED_OFF d13 GRADIENT15(cnst27) ;500u, 8G/cm #ifdef SHAPED d16 pl0:H (H1_S90:sp1 ph21):H ;2ms SEDUCE-1 90 H1 pulse at phase x #else d16 pl10:H (H1_S90 ph21):H ;2ms 90 H1 pulse at phase x #endif d13 d12 pl1:H (H1_90 ph2):H d13 TAUA2 GRADIENT17(cnst23) ;700u, 40G/cm d16 (H1_90*0.231 ph1):H TAUW (H1_90*0.692 ph1):H TAUW (H1_90*1.462 ph1):H d22 (N15_180 ph0):N d22 (H1_90*1.462 ph3):H TAUW (H1_90*0.692 ph3):H TAUW (H1_90*0.231 ph3):H d13 GRADIENT17(cnst23) ;700u, 40G/cm d16 pl12:N TAUA2 d6 go=2 ph31 cpd2:N #ifdef ONE_D d11 do:N wr #0 #else d11 do:N wr #0 if #0 zd #endif #ifdef N15_EVOL d14 ip14 lo to 3 times 2 d14 dd10 d14 id30 d14 ip31 d14 ip31 lo to 4 times l4 d14 rd10 d14 rd30 #else d14*7 #endif #ifdef CO_EVOL d14 ip12 lo to 5 times 2 d14 id0 d14 ip31 d14 ip31 lo to 6 times l6 d14 rd0 #else d14*5 #endif #ifdef H1_EVOL d14 ip17 d14 ip17 lo to 7 times 2 d14 id20 d14 ip31 d14 ip31 lo to 8 times l8 #endif d14 LOCKH_OFF exit ph0=0 ph1=1 ph2=2 ph3=3 ph11=0 0 0 0 2 2 2 2 ph12=0 0 2 2 ph14=0 ph15=0 2 ph16=0 ph17=(8) 3 7 ph21=(360) 358 ;Nominal 0, adjust for any phase difference between pl1 and sp1 ph31=0 2 2 0 2 0 0 2