;hncoca_sefb.al ;3D HN(CO)CA with gradient sensitivity enhancement ;and minimal H2O saturation ; ;Grzesiek & Bax, JMR(1992), 96, 432-440. ;Kay et al., JMR(1994, series A), 109, 129-133. ; ;Written up by Andrew Lee, alee@lcbvax.cchem.berkeley.edu ;Implemented and tested on DMX-600 and DMX-750 by B. Volkman, ;volkman@nmrfam.wisc.edu. 12/16/95 ; ;Suitable grdprog and *.incl files are appended to ;the end of this pulse program, and should be removed and ;placed in appropriate /pp or /gp directory prior to execution ;of this pulse program. ; ; 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 or University of Wisconsin-Madison ; are liable for any physical or other damage incurred during the ; use of this pulse program. ;BMRB Pulse Sequence Accession Number: 13 ;use gradient program alhncoca_fb - follows pulse program ;adjust cnst30 to find magic angle (ca. 1.8) if equipped ;with 3-axis gradients ; ;******Channel assignments *** ;f1- 1H ;f2- 15N ;f3- 13C' ;f4- 13Ca ; ;******** RF pulses ********* ;p1: high power 1H ;p2: high power 15N ;p3: 90 C' with null at Ca (@ pl3:f3) ;p4: 90 Ca with null at C' ;p9: 2.0m 90 at pl9:f1 (for water flip-back) ;p5: 180 C' with null at Ca (@ pl13:f3) ;p29: 90 on 1H at 6.7 kHz (37.3u 90) for waltz-16(x) ;p30: 90 for SEDUCE-1 on Ca, 1.7 kHz at peak height (320u 90) ;p31: low power pulse at pl16 for N-GARP ; ;******* INEPT delays ******* "d2=2.3m-p11" "d3=d2-d16" "d4=2.3m-p16" "d5=d4-d16" "d6=2.3m-p17" "d7=d6-d16" "d23=6.0m" ;C'/Ca transfer ; ;*** constant-time delays *** "d10=d17" "d20=d17-5.5m-p29-d13" ;"d17=12.4m" ;BV, did you do this? Does it work? "d18=d17-5.5m-p29-d13" "d21=5.5m" "d22=d21-p15-d16-d13" ; ;*** pulse centering delays ** "d26=p2-p5/2" ;BV, which is longer? "d29=p2-p1" ; ;******* other delays ******* "d8=0.5m-p18" "d14=p1" "d15=p2" "d13=10u" "d9=10m" ;(ip, id, rd) "d11=100m" ;(disk i/o) "d16=300u" ;(gradient recovery) ;in0=1/2SW(C') ;in10=in20=1/2SW(N) #include #include #define WLTZ_ON p29:f1 ph1 \n d13 cpds1:f1 #define WLTZ_OFF d13 do:f1 \n p29:f1 ph3 1 ze d9 pl1:f1 pl2:f2 pl13:f3 pl4:f4 2 d11 do:f2 d9 3 d9 d9*3 4 d9 d9*2 5 d9 d9*2 6 20u LOCKH_OFF d1 pl1:f1 pl2:f2 pl13:f3 pl4:f4 p8:c13 20u LOCKH_ON (p2 ph0):f2 GRADIENT10(cnst19) ;g0=0.5m @ 8 G/cm d16 ;********************* Begin HNCO ********************** ;******************************************************* (p1 ph0):f1 GRADIENT11(cnst20) ;g1=0.5m @ 5 G/cm d2 (d29 p1*2 ph0):f1 (p2*2 ph0):f2 d3 GRADIENT11(cnst20) d16 (p1 ph1):f1 10u pl9:f1 (p9 ph0):f1 ;2.0m square selective H2O pulse GRADIENT12(cnst21) ;g2=2.0m @ 15 G/cm d16 pl19:f1 (p2 ph11):f2 d21 WLTZ_ON d18 (d26 p5 ph0):f3 (p2*2 ph0):f2 d17 pl3:f3 ;T(N) (p2 ph0):f2 WLTZ_OFF GRADIENT13(cnst22) ;g3=0.75m @ 20 G/cm d16 (p3 ph0):f3 WLTZ_ON d23 pl13:f3 ;1/2J(Ca/C') ;------------- start t1 ------------ (p4 ph12):f4 d0 ;t1/2 (p5 ph0):f3 d0 ;t1/2 (p4 ph0):f4 ;------------ finish t1 ------------ d23 pl3:f3 ;1/2J(Ca/C') WLTZ_OFF (p3 ph0):f3 GRADIENT14(cnst23) ;g4=0.2m @ 5 G/cm d16 pl13:f3 pl0:f4 WLTZ_ON d13 cpds4:f4 ;turn on SEDUCE-1 on Ca ;------------- start t2 ------------ (p2 ph16):f2 d10 (d26 p5 ph0):f3 (p2*2 ph13):f2 d20 WLTZ_OFF d22 pl1:f1 d13 do:f4 ;turn off SEDUCE-1 GRADIENT15(cnst24) ;g5=1.25m @ 30 G/cm d16 pl4:f4 (p2 ph14):f2 ;------------ finish t2 ------------ d14 (p1 ph0):f1 GRADIENT16(cnst25) ;g6=0.3m @ 5 G/cm d4 (p2*2 ph0):f2 (p1*2 ph0):f1 d5 GRADIENT16(cnst25) d16 d15 (p2 ph1):f2 (p1 ph1):f1 GRADIENT17(cnst26) ;g7=0.2m @ 10 G/cm d6 (d29 p1*2 ph0):f1 (p2*2 ph0):f2 d7 GRADIENT17(cnst26) d16 (p1 ph15):f1 0.5m (p1*2 ph0):f1 GRADIENT18(cnst27) ;g8=0.125m @ 27.8 G/cm d8 pl16:f2 go=2 ph31 cpd2:f2 d11 do:f2 wr #0 if #0 zd d9 ip14*2 lo to 3 times 2 d9 dd10 d9 id20 d9 ip31*2 d9 ip16*2 lo to 4 times l4 ;t1 d9 rd10 d9 rd20 d9 ip12 lo to 5 times 2 d9 id0 d9 ip31 d9 ip31 lo to 6 times l6 ;t2 20u LOCKH_OFF exit ph0=0 ph1=1 ph2=2 ph3=3 ph11=0 2 ph12=0 0 0 0 2 2 2 2 ph13=0 0 2 2 ph14=0 ph15=0 ph16=0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph31=0 2 0 2 2 0 2 0 2 0 2 0 0 2 0 2 ;** alhncoca_fb.r ** ; ;loop ns ;{ ;p10 { (0) | (0) | (0)+(cnst19) } ; { (0) | (0) | (0) } ;p11 { (0) | (0) | (0)+(cnst20) } ; { (0) | (0) | (0) } ;p11 { (0) | (0) | (0)+(cnst20) } ; { (0) | (0) | (0) } ;p12 { (0) | (0) | (0)+(cnst21) } ; { (0) | (0) | (0) } ;p13 { (0) | (0) | (0)+(cnst22) } ; { (0) | (0) | (0) } ;p14 { (0) | (0) | (0)+(cnst23) } ; { (0) | (0) | (0) } ;p15 { (0)+(cnst24*cnst30) | (0) | (0)+(cnst24) } ; { (0) | (0) | (0) } ;p16 { (0) | (0) | (0)+(cnst25) } ; { (0) | (0) | (0) } ;p16 { (0) | (0) | (0)+(cnst25) } ; { (0) | (0) | (0) } ;p17 { (0) | (0) | (0)+(cnst26) } ; { (0) | (0) | (0) } ;p17 { (0) | (0) | (0)+(cnst26) } ; { (0) | (0) | (0) } ;p18 { (0)+(cnst27*cnst30) | (0) | (0)+(cnst27) } ; { (0) | (0) | (0) } ;} ;loop ns ;{ ;p10 { (0) | (0) | (0)+(cnst19) } ; { (0) | (0) | (0) } ;p11 { (0) | (0) | (0)+(cnst20) } ; { (0) | (0) | (0) } ;p11 { (0) | (0) | (0)+(cnst20) } ; { (0) | (0) | (0) } ;p12 { (0) | (0) | (0)+(cnst21) } ; { (0) | (0) | (0) } ;p13 { (0) | (0) | (0)+(cnst22) } ; { (0) | (0) | (0) } ;p14 { (0) | (0) | (0)+(cnst23) } ; { (0) | (0) | (0) } ;p15 { (0)+(cnst24*cnst30) | (0) | (0)+(cnst24) } ; { (0) | (0) | (0) } ;p16 { (0) | (0) | (0)+(cnst25) } ; { (0) | (0) | (0) } ;p16 { (0) | (0) | (0)+(cnst25) } ; { (0) | (0) | (0) } ;p17 { (0) | (0) | (0)+(cnst26) } ; { (0) | (0) | (0) } ;p17 { (0) | (0) | (0)+(cnst26) } ; { (0) | (0) | (0) } ;p18 { (0)+(cnst28*cnst30) | (0) | (0)+(cnst28) } ; { (0) | (0) | (0) } ;} ;**Gradal.incl** ;Gradal.incl - include file for Gradient Spectroscopy ;avance-version ;version 94/06/27 ; ; ;#define GRADIENT10(ampl) p10:ngrad:c34 ;#define GRADIENT11(ampl) p11:ngrad:c34 ;#define GRADIENT12(ampl) p12:ngrad:c34 ;#define GRADIENT13(ampl) p13:ngrad:c34 ;#define GRADIENT14(ampl) p14:ngrad:c34 ;#define GRADIENT15(ampl) p15:ngrad:c34 ;#define GRADIENT16(ampl) p16:ngrad:c34 ;#define GRADIENT17(ampl) p17:ngrad:c34 ;#define GRADIENT18(ampl) p18:ngrad:c34 ;#define GRADIENT19(ampl) p19:ngrad:c34 ;#define GRADIENT20(ampl) p20:ngrad:c34 ;#define BLKGRAD setnmr2^0 setnmr0^34 ;#define UNBLKGRAD setnmr2|0 setnmr0|34 ;#define BLKGRAMP setnmr0^34 ;#define UNBLKGRAMP setnmr0|34