;hncocaf.fa ;3D HN(CO)CA with Watergate (3-9-19) reverse INEPT (FHSQC) ; and optional 2H decoupling ;This version uses no ct evolution of Ca ;Yamazaki et al., J.Am. Chem. Soc. 1994, 116, 11655-11666 ;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: hncocaf.fa,v 1.3 2002/03/21 18:39:00 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, f5: 2H (channel assignments may be changed below) ;o1p: 4.7 ppm, ;o2p: 118 ppm, ;o3p: 55 ppm, ;o5p: 4.5 ppm ; ;d1: relaxation delay=d1+0.1s ;p1 90 H1 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 ;p10 90 H at pl10 (H1 composite decoupling) ;p2 90 N at pl2 ;p4 90 Ca at pl4 (for 90 Ca) ;p9 90 Ca at pl9 (for 180 Ca) ;p5 180 CO SEDUCE1 shape at power sp5, offset CO-Ca ;p7 90 CO shaped (square) at power sp7 offset CO-Ca ;p25 90 2H pulse at pl15 (optional) ;pl0 120dB ;d21: 1/(2*dNu), dNu=Nu(NH)-Nu(H2O) ; ;H1 Waltz-16x or DIPSI-2x (cpdprg1), using p90 (PCPD1) at pl11 ;N15 Waltz-16 (cpdprg2), using p90 (PCPD2) at pl12 ;Ca SEDUCE1 decoupling of Ca, using pcpd3 at sp3, ; shape seduce1 offset 0, cpdprg3 waltz16sp3. ;H2 Waltz-16 (cpdprg5), using p90 (PCPD5) at pl15 ;N15 evolution: ; in10=in30, SW(N)=1/2*in10 ; l4 complex points; max. is (d10/in10)+1 ; Process as States (although data is acquired as States-TPPI) ; N15 chemical shift axis is reversed: set reverse to true. ;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). ;ns=8, 16, ..., ds=8, 16,... ; ;Recommendations for triple-axis (single-axis) gradients: ;gpz1: 12% (12%) ;gpz2: 6% (6%) ;gpz3: 15% (15%) ;gpz4: -7% (-7%) ;gpz5: 10% (10%) ;gpz6: -22% (-22%) ;gpz7: 30% (30%) ;gpz8: 44% (44%) ;gpz9: 15% (15%) ;gpz10: 0.6% (0.6%) ;gpz11: 15% (15%) ;gpz12: 10% (10%) ;gpx13: 54% adjust for magic angle (0%) ;gpz13: 30% (55%) ;gpnam1: sine.50 ;gpnam2: sine.50 ;gpnam3: sine.100 ;gpnam4: sine.100 ;gpnam5: sine.100 ;gpnam6: sine.100 ;gpnam7: sine.10 ;gpnam8: sine.10 ;gpnam9: sine.50 ;gpnam10: sine.100 ;gpnam11: sine.50 ;gpnam12: sine.50 ;gpnam13: 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 N15_EVOL ; comment out for 2D w/o N15 evolution #define C13_EVOL ; comment out for 2D w/o C13 evolution #define H2_DEC ; uncomment to enable H2 decoupling #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 #define D f5 ; ;You shouldn't have to worry about anything beyond this point :-) ; ;sanity checks ; #ifdef ONE_D #undef N15_EVOL #undef C13_EVOL #endif ; aqseq 321 ; define delay TAUA define delay TAUA2 define delay TAUA13 define delay TAUB define delay TAUC define delay TAUC1 define delay TAUC2 define delay TAUE define delay TAUE5 define delay TAUE10 define delay TAUW define delay TAUW1 define delay TN 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 GRAD8 define pulse GRAD9 define pulse GRAD10 define pulse GRAD11 define pulse GRAD12 define pulse GRAD13 define pulse H1_90 define pulse H1_180 define pulse H1_S90 define pulse N15_90 define pulse N15_180 define pulse CA_90 define pulse CA_180 define pulse CO_90 define pulse CO_180 "d11=100m" ;disk i/o "d12=10u" ;power switching etc. "d13=5u" ;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" "CA_90=p4" "CA_180=p9*2" "CO_90=p7" "CO_180=p5" "GRAD1=600u" "GRAD2=500u" "GRAD3=1.0m" "GRAD4=1.0m" "GRAD5=1.0m" "GRAD6=700u" "GRAD7=100u" "GRAD8=100u" "GRAD9=600u" "GRAD10=1.0m" "GRAD11=600u" "GRAD12=500u" "GRAD13=700u" "TAUW=d21" "TAUW1=(TAUW/2)-N15_90" "TAUA=2.3m" "TAUB=5.4m" "TAUC=12.0m" "TAUE=4.1m" "TAUA2=TAUA-GRAD2-d16-d13" "TAUA13=TAUA-TAUW*2.5-H1_90*2.385-GRAD13-d16-d13" "TAUC1=TAUC-CO_180-d13" "TAUC2=TAUC-TAUB-p10-d13*2-d12" "TAUE5=TAUE-CA_180-GRAD5-d12-d13*2" "TAUE10=TAUE-CA_180-GRAD10-d12-d13*2" "TN=12.0m" "d10=TN-d13*4-d12*2" "d30=TN-TAUB-CO_180-p10-d12*3-d13*7" #ifdef C13_EVOL "d0=((cnst0*2+1)*in0-CA_90*1.273-CO_180-N15_180-H1_180-d12*2-d13*3)/2" #endif "CEN_HN1=N15_90-H1_90" #define H1_DEC_ON d13 \n d12 pl10:H \n p10:H ph1 \n d13 cpds1:H #define H1_DEC_OFF d13 do:H \n p10:H ph3 \n d13 \n d12 pl1:H #ifdef H2_DEC #define H2_DEC_ON d12 pl15:D \n p25:D ph1 \n d13 cpds5:D #define H2_DEC_OFF d13 do:D \n p25:D ph3 d12 #else #define H2_DEC_ON d13 #define H2_DEC_OFF d13 #endif #define SED_ON d13 \n d12 pl0:C \n d13 cpds3:C #define SED_OFF d13 do:C \n d12 pl0:C \n d13 #ifdef EXPTCORR "d31=2*(GRAD2+TAUA2+TAUB+GRAD5+TAUE5+GRAD10+TAUE10+TAUA13+GRAD13+2*TAUW+TAUW1)+GRAD1+GRAD3+TAUC1+TAUC2+GRAD4+GRAD6+GRAD9+GRAD11+GRAD12" #endif #include #include 1 ze 2 d13 do:N d13 H2_LOCK d11 LOCKH_OFF d14 3 d14 d14 d14 d14 4 d14 d14 d14 5 d14 d14 d14 6 d13 #ifdef EXPTCORR #include #endif d1 pl1:H pl2:N d13 LOCKH_ON d13 UNBLKGRAMP d13 H2_PULSE (N15_90 ph0):N d13 GRAD1:gp1 ;600u, 8G/cm, sine.50 d16 (H1_90 ph0):H d13 GRAD2:gp2 ;500u, 4G/cm, sine.50 d16 TAUA2 (CEN_HN1 H1_180 ph0):H (N15_180 ph0):N TAUA2 d13 GRAD2:gp2 ;500u, 4G/cm, sine.50 d16 (H1_90 ph1):H (d13 d12 pl22 H1_S90 ph22:r d13 d12 pl1):H ;2ms 90 H1 pulse at phase x d13 GRAD3:gp3 ;1.0m, 10G/cm, sine.100 d16 (N15_90 ph0):N TAUB H1_DEC_ON TAUC2 pl0:C (N15_180 ph0):N d13 (CO_180:sp5 ph0):C TAUC1 (N15_90 ph0):N H1_DEC_OFF d13 GRAD4:gp4 ;1.0m, -5G/cm, sine.100 d16 pl0:C (CO_90:sp7 ph11):C d13 d12 pl9:C (CA_180 ph0):C d13 GRAD5:gp5 ;1.0m, 7G/cm, sine.100 TAUE5 pl0:C (CO_180:sp5 ph0):C d13 d12 pl9:C (CA_180 ph0):C d13 GRAD5:gp5 ;1.0m, 7G/cm, sine.100 TAUE5 pl0:C (CO_90:sp7 ph1):C (H1_180 ph0):H d13 GRAD6:gp6 ;1.0m, -15G/cm, sine.100 d16 pl4:C H2_DEC_ON (CA_90 ph12):C #ifdef C13_EVOL d13 d12 pl0:C d0 (CO_180:sp5 ph0):C (d13 N15_180 ph0):N (H1_180 ph0):H d13 d12 pl4:C d0 #else d13 (H1_180 ph0):H d13 #endif (CA_90 ph0):C H2_DEC_OFF d13 GRAD9:gp9 ;600u, 10G/cm, sine.50 d16 pl0:C (CO_90:sp7 ph1):C d13 GRAD10:gp10 ;1.0m, 0.4G/cm, sine.100 TAUE10 pl9:C (CA_180 ph0):C d13 d12 pl0:C (CO_180:sp5 ph0):C d13 GRAD10:gp10 ;1.0m, 0.4G/cm, sine.100 TAUE10 pl9:C (CA_180 ph0):C d13 d12 pl0:C (CO_90:sp7 ph0):C d13 GRAD11:gp11 ;600u, 10G/cm, sine.50 d16 H1_DEC_ON (N15_90 ph13):N SED_ON d10 SED_OFF (N15_180 ph14):N d13 (CO_180:sp5 ph0):C SED_ON d30 H1_DEC_OFF TAUB SED_OFF (N15_90 ph0):N d13 GRAD12:gp12 ;500u, 7G/cm, sine.50 d16 (d13 d12 pl21 H1_S90 ph21:r d13 d12 pl1):H ;2ms 90 H1 pulse at phase x (H1_90 ph2):H d13 GRAD13:gp13 ;700u, 40G/cm, sine.100 d16 TAUA13 (H1_90*0.231 ph1):H TAUW (H1_90*0.692 ph1):H TAUW (H1_90*1.462 ph1):H TAUW1 (N15_180 ph0):N TAUW1 (H1_90*1.462 ph3):H TAUW (H1_90*0.692 ph3):H TAUW (H1_90*0.231 ph3):H TAUA13 GRAD13:gp13 ;700u, 40G/cm, sine.100 d16 pl12:N d13 BLKGRAMP go=2 ph31 cpds2:N #ifdef ONE_D d11 do:N wr #0 #else d11 do:N wr #0 if #0 zd #endif d13 H2_LOCK d13 LOCKH_OFF #ifdef N15_EVOL d14 ip13 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 C13_EVOL d14 ip12 lo to 5 times 2 d14 id0 d14 ip31 d14 ip31 lo to 6 times l6 #endif exit ph0=0 ph1=1 ph2=2 ph3=3 ph11=0 2 ph12=0 0 2 2 ph13=0 ph14=0 0 0 0 2 2 2 2 ph21=0 ph22=0 ph31=0 2 2 0