;hn15noe.fa ;2D 1H-15N-NOE, using echo-antiecho gradient coherence selection ;Bruker Avance/Xwin-nmr version. This program requires XWIN-NMR 2.5+ ; NOE and no-NOE (control) experiments are recorded interleaved ;Farrow et al., Biochemistry 33, 5984-6003 (1994). ;Bruker Avance/Xwin-nmr version ;Written up by F. Abildgaard, NMRFAM (abild@nmrfam.wisc.edu) ; ; $Id: hn15noe.fa,v 1.6 2001/08/25 00:25:43 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 (channel assignments may be changed below) ;o1p: 4.7ppm ;o2p: 118ppm ; ;d1: relaxation delay, > d2; typ. 5 s. ;d2: 1H saturation delay, > 3*T1(1H, 15N); typ. 3 s. ;p1 90 H1 at pl1 ;p2 90 N15 at pl2 ;pl0 120dB ; ; ;N15 Waltz-16 PCPD2 at pl12, cpdprg2 ;N15 evolution: ; in0, SW(N)=1/(2*in0) ; l4 complex points in each 2D (ser file holds two 2D files) ; - set "1 td" to 4*l4. ; The reference 2D spectrum is in rows 1,2,5,6,9,10,... ; The NOE enhanced 2D is in rows 3,4,7,8,11,12,... ; Quadrature dection in t1 by echo-antiecho, with axial peaks ; at the edge of the spectrum. ; set cnst0 to 0 (preferably) or 1, 2, 3 .. 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). ; ;ns=8, 16, ..., ds=8, 16, ... ; ;Recommendations for gradients, triple-axis (single-axis): ;gpz1: 12% ;gpz2: 22% ;gpz5: 1.2% (1.2%) ;gpx6: 54% (0%) ;gpz6: 30% (55%) ;gpx7: 14% (0%) ;gpz7: 0% (14%) ;gpy8: 20% (0%) ;gpz8: 0% (20%) ;gpx9: 54% (0%) ;gpz9: 30% (55%) ;gpnam1: sine.50 ;gpnam2: sine.50 ;gpnam6: sine.100 ;gpnam7: sine.50 ;gpnam8: sine.50 ;gpnam9: sine.20 ; ;Coherence selection gradient pair (GRAD6/GRAD9) may be optimized ;by varying p19 (uncomment OPTIM_P19). Theoretical value of p19 is 131.7 us. ; ;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 NOE ; uncomment for NOE in 1D experiment ;#define OPTIM_P19 ; uncomment if you want to optimize p19 (GRAD9) #define EXPTCORR ; uncomment if you want "expt" to report ; ; the correct expt time (works with XWIN-NMR 2.x) ; ;You shouldn't have to worry about anything beyond this point :-) ; ;Define channel assignments: #define H f1 #define N f2 ; ;Sanity checks #ifndef ONE_D #undef NOE #endif ; define delay TAUA define delay TAUA7 define delay TAUA8 define delay TAUB define delay TAUB2 define delay TAUC define delay SATDEL define delay RDEL1 define delay RDEL2 define delay RDEL3 define delay RDEL4 define delay CEN_HN1 define pulse H1_90 define pulse H1_120 define pulse H1_180 define pulse N15_90 define pulse N15_180 define pulse GRAD1 define pulse GRAD2 define pulse GRAD5 define pulse GRAD6 define pulse GRAD7 define pulse GRAD8 define pulse GRAD9 "d11=100m" ;disk i/o ;"d12=10u" ;power switching etc. "d13=5u" ;a short delay "d14=60u" ;ip,id etc. "d16=300u" ;gradient recovery "d17=30u" ;short gradient recovery "H1_90=p1" "H1_120=H1_90*4/3" "H1_180=H1_90*2" "N15_90=p2" "N15_180=N15_90*2" ; "GRAD1=400u" "GRAD2=400u" "GRAD5=1.5m" "GRAD6=2.2m" "GRAD7=500u" "GRAD8=500u" #ifndef OPTIM_P19 "p19=111.4u" #endif "GRAD9=p19" "TAUA=2.25m" ;1/(4Jnh) w/ relax. comp. "TAUA7=TAUA-GRAD7-d13-d16" "TAUA8=TAUA-GRAD8-d13-d16" "TAUB=2.75m" "TAUB2=TAUB-GRAD6-d16-H1_180-d17*2-d13*4" "TAUC=GRAD9+d16+d13" "d6=H1_90" "d7=N15_90" "CEN_HN1=N15_90-H1_90" "SATDEL=d2" "RDEL3=5m" "l1=SATDEL/(H1_120+RDEL3)" "RDEL2=d1-(l1*(H1_120+RDEL3))" "RDEL1=d1+GRAD1+GRAD2+d16*2+H1_90+d13" "RDEL4=d1*5/3" #ifdef ONE_D "d0=d13" #else "d0=d13+((cnst0*2+1)*in0)/2" "d28=RDEL4" #endif #ifdef NOE "l2=1" #else "l2=0" #endif #ifdef EXPTCORR "d31=2*(TAUA7+GRAD7+TAUA8+GRAD8+GRAD9)+RDEL1+TAUB+TAUB2+TAUC+GRAD6" #endif #include #include 1 ze 2 d13 do:N d11 LOCKH_OFF 3m d14 d14 3 d14 d14 d14 d14 d14 4 d13 #ifdef EXPTCORR #include #endif d14 pl1:H pl2:N ; Proton saturation and 15N relaxation if "l2 %2 == 0" goto 9 ; Let N15 relax and saturate H1 RDEL2 8 (H1_120 ph0):H RDEL3 lo to 8 times l1 d13 d13 LOCKH_ON d13 UNBLKGRAMP ; Purge H1 GRAD1:gp1 ;400us, 8G/cm, sine.50 d16 (H1_90 ph0):H d13 GRAD2:gp2 ;400us, 15G/cm, sine.50 d16 goto 10 ; Or let the N15 relax 9 RDEL1 d13 d13 LOCKH_ON d13 UNBLKGRAMP 10 d13 (N15_90 ph12):N TAUB (N15_180 ph13):N d13 d0 gron5*-1 d17 groff (H1_180 ph0):H d13 GRAD6:gp6*EA ;1.3m, +/-30G/cm d16 TAUB2 d0 gron5 d17 groff (N15_90 ph14):N d6 (H1_90 ph0):H d13 GRAD7:gp7 ;500u, 7G/cm d16 TAUA7 (N15_180 ph0):N (H1_180 ph0):H d13 TAUA7 GRAD7:gp7 ;500u, 7G/cm d16 d7 (N15_90 ph1):N (H1_90 ph1):H d13 GRAD8:gp8 ;500u, 7G/cm d16 TAUA8 (CEN_HN1 H1_180 ph0):H (N15_180 ph0):N d13 TAUA8 GRAD8:gp8 ;500u, 7G/cm d16 (H1_90 ph2):H d13 GRAD9:gp9*-1 ;130u, 30G/cm d16 pl12:N (H1_180 ph0):H d13 GRAD9:gp9 ;130u, 30G/cm d16 BLKGRAMP go=2 ph31 cpd2:N #ifdef ONE_D d11 do:N wr #0 d13 LOCKH_OFF #else d11 do:N wr #0 if #0 zd d13 LOCKH_OFF 3m igrad EA d14 ip14 d14 ip14 lo to 3 times 2 ; insert extra delay to let 1H relax before NO-NOE ; RDEL4 iu2 d28 iu2 lo to 3 times 2 d14 id0 d14 ip12 d14 ip12 d14 ip31 d14 ip31 lo to 4 times l4 #endif exit ph0=0 ph1=1 ph2=2 ph3=3 ph12=1 3 ph13=0 0 1 1 2 2 3 3 ph14=0 ph31=0 2 2 0