;toccthsqcse.fa ;3D TOCSY relayed constant time HSQC-SE ;Bruker Avance/Xwin-nmr version ;Written up by F. Abildgaard, NMRFAM (abild@nmrfam.wisc.edu) ; ; $Id: toccthsqcse.fa,v 1.3 2001/02/10 00:38:16 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) ;o1p: 4.7ppm or ;use fq1list fatoccthsqc.f1 (6.9,4.70ppm) if F1SWITCH defined below (not with DQD) ;o2p: 118ppm ;o3p: 43ppm (aliphatic) or 126 (aromatic) ; ;p1 90 H1 at pl1 ;p3 90 C13 at pl3 ;p5 180 C' SEDUCE1 shaped at offset CO-43ppm, using sp5 (optional) ;p31 90 H at pl10 for isotropic mixing ;d2: 1/(4Jch), aliph: 1.87ms, arom: 1.5ms ;d4: 1/(4Jch) for CH, 1/(8Jch) for CH, CH2 and CH3 ; i.e. 1.87ms or 0.93ms, resp. ; for arom: 1.5ms ;d3=1/2Jcc or 1/Jcc, aliph: 13.3m or 26.6m, resp., arom: 8ms or 16ms, resp. ;For aromatic residues: comment out N15_DEC and CO_DEC below ;H1 isotropic mixing: p31 and l9. Select l9 to give ~20ms mixing time. ;N15 Waltz-16 PCPD2 at pl12, cpdprg2 (optional) ;C13 GARP decoupling using CPDPRG3 and PCPD3 at pl13 ;H1 evolution: ; SW(H)=1/2*in10, typ. 3 ppm (arom), 8ppm (aliph.) ; set cnst10 to 0 (preferably) or 1 to make d10 the smallest possible ; positive delay: d10=((cnst10*2+1)*in10-(p1*1.273+p3*4+d13*2))/2 ; l6 complex points ;C evolution: ; in0, SW(C)=1/(2*in0), typically 33ppm ; l4 complex points, max l4 = (d3-p5)/in0 (w/ CO_DEC) or d3/in0 (w/o CO_DEC) ; Define C_90180 below for dw/2 initial delay (90,-180 phase) ;ns=16, 32, ..., ds=2*ns*m, m=1, 2, ... ; ;Recommendations for gradients: ;gpz1: 15% ;gpz2: -22% ;gpx3: 54% adjust for magic angle ;gpz3: 30% ;gpz4: 25% ;gpz5: 15% ;gpx6: 54% adjust for magic angle ;gpz6: 30% ;gpnam1: sine.100 ;gpnam2: sine.100 ;gpnam3: sine.100 ;gpnam4: sine.32 ;gpnam5: sine.32 ;gpnam6: sine.20 ; ;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 H1_EVOL ; comment out for 2D w/o H1 evolution #define C13_EVOL ; comment out for 2D w/o C13 evolution #define C_90180 ;#define N15_DEC ; uncomment for N15 decoupling ;#define CO_DEC ; uncomment for C' decoupling ;define F1SWITCH #define OPTIM_P19 ; uncomment if you want to optimize p19 (GRAD6) #define EXPTCORR ; uncomment if you want "expt" to report ; ; the correct expt time (works with XWIN-NMR 2.x) ;Select an isotropic mixing scheme ;#define DIPSI2 ; taum = 115.112*p31*l9 #define DIPSI2RC ; taum = 172.668*p31*l9 ;#define DIPSI3 ; taum = 217.336*p31*l9 ; ;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 H1_EVOL #undef C13_EVOL #undef C_90180 #endif ; define delay RCDELAY define delay DELTA define delay CEN_HC1 define pulse H1_90 define pulse H1_180 define pulse C13_90 define pulse C13_180 define pulse GRAD1 define pulse GRAD2 define pulse GRAD3 define pulse GRAD4 define pulse GRAD5 define pulse GRAD6 "d11=100m" "d12=10u" "d13=5u" "d14=40u" "d16=300u" "H1_90=p1" "H1_180=H1_90*2" "C13_90=p3" "C13_180=C13_90*2" ; "GRAD1=1.0m" "GRAD2=1.0m" "GRAD3=720u" "GRAD4=250u" "GRAD5=250u" #ifndef OPTIM_P19 "p19=180u" ; configurable: set to the optimum value on your instrument #endif "GRAD6=p19" ; #ifdef H1_EVOL "d10=((cnst10*2+1)*in10-(H1_90*1.273+C13_90*4+d13*2))/2" #endif #ifdef C_90180 "d0=d13+in0/2" #else "d0=d13" #endif "DELTA=GRAD6+d16+d13*2+d12" "CEN_HC1=C13_90-H1_90" "d6=H1_90" "d7=C13_90" #ifdef CO_DEC "d18=d3-d16-GRAD3-p5+C13_180+d12+d13" #else "d18=d3-d16-GRAD3+C13_180+d12+d13" #endif "d22=d2-GRAD5-d13" "d24=d4-GRAD4" #ifdef DIPSI2RC "RCDELAY=p31*1.599" #endif #ifdef N15_DEC #define N15_DEC_ON d12 pl12:N \n d13 cpd2:N #define N15_DEC_OFF d13 do:N #else #define N15_DEC_ON d13 #define N15_DEC_OFF d13 #endif #ifdef EXPTCORR "d31=2*(GRAD4+GRAD5)+GRAD1+GRAD2+GRAD3+GRAD6+DELTA" #endif #include #include 1 ze 2 d13 do:C d11 LOCKH_OFF 3m d14 d14 3 d14 d14 d14 d14 d14 4 d14 d14 5 d14 d14 d14 6 d13 #ifdef EXPTCORR #include #endif #ifdef F1SWITCH d14 fq1:f1 #endif d1 pl1:H pl3:C d13 LOCKH_ON d13 UNBLKGRAMP (C13_90 ph0):C d13 GRAD1:gp1 ;1m, 10G/cm, sine.100 d16 (H1_90 ph10):H #ifdef H1_EVOL d10 (C13_90 ph0 d13 C13_180 ph1 d13 C13_90 ph0):C d10 #else d13 #endif (H1_90 ph1):H d13 d12 pl10:H 9 d13 #ifdef DIPSI2 #include #endif #ifdef DIPSI2RC #include #endif #ifdef DIPSI3 #include #endif lo to 9 times l9 d13 #ifdef F1SWITCH d14 fq1:f1 #endif d12 pl1:H (H1_90 ph0):H d2 (CEN_HC19 H1_180 ph0):H (C13_180 ph0):C d2 (H1_90*55 ph0):H d13 (H1_90 ph1):H d13 GRAD2:gp2 ;1m, -15G/cm, sine.100 d16 N15_DEC_ON (C13_90 ph11):C d13 d12 pl0:C #ifdef CO_DEC (d3) (d0 H1_180 ph0):H (d0 p5:sp5 ph0):C #else (d3) (d0 H1_180 ph0):H #endif d13 d12 pl3:C (d18) (d0 C13_180 ph13):C d13 d12 pl0:C #ifdef CO_DEC (p5:sp5 ph0):C #endif N15_DEC_OFF GRAD3:gp3*EA*-1 ;720u, -/+40G/cm, sine.100 d16 pl3:C N15_DEC_ON (C13_90 ph12):C d6 (H1_90 ph0):H d13 GRAD4:gp4 ;250u, 16G/cm, sine.32 d24 (C13_180 ph0):C (H1_180 ph0):H d13 GRAD4:gp4 ;250u, 16G/cm, sine.32 d24 d7 (C13_90 ph1):C (H1_90 ph1):H d13 GRAD5:gp5 ;250u, 10G/cm, sine.32 d22 N15_DEC_OFF (CEN_HC1 H1_180 ph0):H (C13_180 ph0):C d13 GRAD5:gp5 ;250u, 10G/cm d22 d13 (H1_90 ph0):H DELTA (H1_180 ph0):H d13 GRAD6:gp6 ;180u, 40G/cm, sine.20 d13 d16 BLKGRAMP d12 pl13:C go=2 ph31 cpds3:C #ifdef ONE_D d11 do:C wr #0 #else d11 do:C wr #0 if #0 zd #endif d13 LOCKH_OFF #ifdef C13_EVOL 3m igrad EA d14 ip12 d14 ip12 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 ip10 lo to 5 times 2 d14 id10 d14 ip31 d14 ip31 lo to 6 times l6 #endif exit ph0=0 ph1=1 ph2=2 ph3=3 ph10=1 3 ph11=0 0 2 2 ph12=0 ph13=1 1 1 1 3 3 3 3 2 2 2 2 0 0 0 0 ph31=0 2 2 0 0 2 2 0 2 0 0 2 2 0 0 2