;noetrosyfb.fa ;3D NOESY-15N-1H-TROSY-SE-FB with 3-9-19 watergate and optional C13 decoupling ;Rance et al., J. Magn. Reson. 136, 92-101 (1999) ;Pervushin et al., Proc. Natl. Acad. Sci. USA 94, 12366-12371 (1997) ;Bruker Avance/Xwin-nmr version. This program requires XWIN-NMR 2.x ;Written up by F. Abildgaard, NMRFAM (abild@nmrfam.wisc.edu) ; ; $Id: noetrosyfb.fa,v 1.5 1999/10/26 22:23:59 abild Exp abild $ ; ; Disclaimer: This pulse program is provided "as is" for your ; information. Support for the use of this pulse program is ; 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: fanoetrosyfb ;o1p: 4.7ppm ;o2p: 118ppm ;o3p: 120ppm ; ;p1 90 H1 at pl1 ;p2 90 N15 at pl2 ;p3 90 C13 at pl3 (for optional C13 decoupling) ;d1: relaxation delay ;d8: mixing time ;d21: 1/(2*dNu), dNu=Nu(NH)-Nu(H2O), 300us at 500MHz, 200us at 750MHz ;N15 evolution: ; SW(N)=1/(2*in0) ; l4 complex points. Set '1 td' to 2*l4. ; Process as echo-antiecho ; set cnst0 to 0 (preferably) or 1 to adjust the initial delay in t2. ; cnst0=0 gives DW(N)/2 initial delay ((90,-180) phase distortion in F2). ; cnst0=1 gives 1.5*DW(N) initial delay ((270,-540) phase distortion in F2 ; (use LP to correct). ;H1 evolution: ; SW(H)=1/2*in10 ; Process as States ; set cnst10 to 0 (preferably) or 1 to make d10 the smallest possible ; positive delay (check with "ased"). ; cnst10=0 gives DW(H)/2 initial delay ((90,-180) phase distortion in F1). ; cnst10=1 gives 1.5*DW(H) initial delay ((270,-540) phase distortion in F1, ; use LP to correct). An additional -45 dgr phase correction is needed. ; l6 complex points. Set '2 td' to 2*l6. ;ns=8,16,... ,ds=8,16,... ; ;Recommendations for gradients: ;p15=500u ;p16=500m ;p17=700u ;p18=1.5m ;cnst21=6% (4G/cm) ;cnst22=8% (6G/cm) ;cnst23=20% (30-40G/cm combined x,z) ;cnst24=0.7-1% (0.5G/cm bipolar gradient) ;cnst25=15% (10G/cm) ;cnst30=1.800 (adjust) for magic angle gradient (Gx/Gz) or 0 for Gz only. ;#define ONE_D ; uncomment for 1D experiment #define H1_EVOL ; comment out for 2D w/o H1 evolution #define N15_EVOL ; comment out for 2D w/o N15 evolution #define C13_LABEL ; uncomment for C13 decoupling #define EXPTCORR ; uncomment if you want "expt" to report ; the correct exp. time (works with XWIN-NMR 2.x) #define XWIN2.6 ; uncomment if running XWIN-NMR 2.6 or higher - ; if XWIN2.6 is undefined, check the value of the ; delay PRESCD below. It should be equal to the prescan ; delay "DE" (e.g. 6.0 us on DMX hardware) ; ;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 H1_EVOL #endif ; define delay TAUA define delay TAUB define delay TAUC define delay TAUW define pulse H1_90 define pulse H1_180 define pulse N15_90 define pulse N15_180 define pulse C13_90 define pulse C13_180 define delay DE2DE1 define delay DEDE2 define delay PRESCD #ifdef XWIN2.6 "PRESCD=de" #else "PRESCD=6.0u" #endif "DE2DE1=de2-de1" "DEDE2=PRESCD-de2" "d11=100m" ;disk i/o ;"d12=10u" ;power switching etc. "d13=5u" ;a short delay "d14=60u" ;ip,id etc. "d16=300u" ;gradient recovery delay "H1_90=p1" "H1_180=p1*2" "N15_90=p2" "N15_180=p2*2" "d6=H1_90" "TAUA=2.7m-p15-d16-d13" "TAUB=2.7m-p16-d16-d13" "TAUW=d21" "TAUC=2.7m-TAUW*2.5-p1*2.385-p17-d16-d13" "d22=(TAUW/2)-N15_90" "d29=N15_90-H1_90" "d18=d8-p16-p18-N15_90-d16*2-d13" #ifdef C13_LABEL "C13_90=p3" "C13_180=p3*2" #endif #ifdef N15_EVOL "d17=50u" ;short gradient recovery delay #ifdef C13_LABEL "d0=((cnst0*2+1)*in0-C13_90*4-d13*7-d17*2)/2" #else "d0=((cnst0*2+1)*in0-d13*5-d17*2)/2" #endif #endif #ifdef H1_EVOL "d10=((cnst10*2+1)*in10-(H1_90*1.273+N15_180))/2" #endif #ifdef EXPTCORR "d31=2*TAUA+2*TAUB+2*TAUC+4*4*TAUW" #endif "l0=0" #include #include 1 ze 2 d11 d14 d14 d14 d14 d14 3 d14 d14 d14 d14 d14 4 d14 d14 d14 5 d14 d14 d14 6 d14 LOCKH_OFF #ifdef EXPTCORR #include #endif d1 pl1:H pl2:N pl3:C d14 LOCKH_ON (N15_90 ph0):N d13 GRADIENT18(cnst21) ;1.5m, 4G/cm d16 #ifdef H1_EVOL (H1_90 ph14):H d10 #ifdef C13_LABEL (N15_180 ph0):N (C13_90 ph0 d13 C13_180 ph1 d13 C13_90 ph0):C #else (N15_180 ph0):N #endif d10 #else (H1_90 ph24):H d13 #endif (H1_90 ph0):H ; Begin mixing time d18 GRADIENT16(cnst25) ;500u, 10G/cm d16 (N15_90 ph0):N d13 GRADIENT18(cnst22) ;1.5ms, 6G/cm d16 ; End mixing time ; Begin TROSY (H1_90 ph0):H d13 GRADIENT15(cnst21) ;500us, 4G/cm d16 TAUA (d29 H1_180 ph3):H (N15_180 ph0):N TAUA d13 GRADIENT15(cnst21) ;500u, 4G/cm d16 (H1_90 ph3):H d13 (N15_90 ph11):N d13 #ifdef N15_EVOL d13:ngrad:c34 ;bipolar gradient, cnst24 0.5G/cm d0 d13:ngrad:c34 d17 #ifdef C13_LABEL (C13_90 ph0 d13 C13_180 ph1 d13 C13_90 ph0):C #endif d13:ngrad:c34 d0 d13:ngrad:c34 d17 #else d13:ngrad:c34 ;bipolar gradient, cnst24 0.5G/cm d13 d13:ngrad:c34 d13:ngrad:c34 d13 d13:ngrad:c34 #endif (H1_90 ph12):H d13 GRADIENT16(cnst22) ;500u, 6G/cm d16 TAUB (d29 H1_180 ph0):H (N15_180 ph0):N TAUB GRADIENT16(cnst22) ;500u, 6G/cm d16 #ifndef N15_EVOL d13*7 #endif (H1_90 ph0):H d13 (N15_90 ph1):N d13 GRADIENT17(cnst23) ;700u, 40G/cm d16 TAUC (H1_90*0.231 ph20):H TAUW (H1_90*0.692 ph20):H TAUW (H1_90*1.462 ph20):H d22 (N15_180 ph0):N d22 (H1_90*1.462 ph21):H TAUW (H1_90*0.692 ph21):H TAUW (H1_90*0.231 ph21):H d13 TAUC d13 GRADIENT17(cnst23) ;700u, 40G/cm d16 (N15_90 ph13):N d6 ; start acquisition de1 DE2DE1 adc ph31 syrec if "l0 %2 == 0" goto 30 29 (DEDE2 ph29):f1 goto 31 30 (DEDE2 ph30):f1 31 aq rcyc=2 #ifdef ONE_D d11 wr #0 #else d11 wr #0 if #0 zd #endif #ifdef N15_EVOL d14 iu0 d14 ip12 d14 ip12 d14 ip13 d14 ip13 lo to 3 times 2 d14 id0 d14 ip11 d14 ip11 d14 ip31 d14 ip31 lo to 4 times l4 d14 rd0 #endif #ifdef H1_EVOL d14 ip14 d14 ip14 lo to 5 times 2 d14 id10 d14 ip31 d14 ip31 lo to 6 times l6 #endif d14 LOCKH_OFF exit ph0=0 ph1=1 ph2=2 ph3=3 ph11=3 1 0 2 ph12=1 ph13=0 ph14=(8) 1 1 1 1 5 5 5 5 ph20=1 ph21=3 ph24=0 0 0 0 2 2 2 2 ph29=2 2 0 0 ph30=0 0 0 0 ph31=0 2 3 1 2 0 1 3