;t1_15n_sefb.bv ;2D 15N T1 (HSQC) with water along +Z ;Farrow, N.A. et al, Biochemistry (1994), 33, 5984-6003. ;Implemented and tested on DMX-600 and DMX-750 by B. Volkman, ;volkman@nmrfam.wisc.edu. 4/15/96 ;added additional steps to ph12 ;to eliminate quad artifacts in t1 5/9/96 BFV ; ;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. ; ;use gradient program bv_t1_15n(m).r (m for magic angle ;gradients, if equipped with triple-axis gradients) ; ;**Set these parameters manually** ;RF pulses ;F1= proton at H2O ;F2=15N at amides (~116ppm) ;p1 - 1H high power 90 @ pl1 ;p2 - 15N high power 90 @ pl2 ;p25 - shaped 180 shifted to center of NH's, ; with null at water ;pcpd2 - 15N aliphatic decoupling 90 @ pl12 ;cpdprg2 - waltz16 or garp ;L3 - loop for T delay ;T= 5m * (L3+1) "p21=p1*2" "p22=p2*2" "d11=100m" "d16=300u" "d2=2.25m-p12" ;p12=GRADIENT12 pulse length "d3=d2-d16" "d4=2.75m" "d5=500u" "d6=p1" "d7=p2" "d12=20u" "d13=d4-p14" ;for tau-b "d14=d13-d16" ;for tau-b "d15=d4-d12-p17" ;p17=GRADIENT17 pulse length "d17=d4+(p1*2)+6u" ;for tau-b''' "d21=2.5m-p25/2" "d22=d21-p16-d16" "d25=d5-p18" "d29=p2-p1" #include #include 1 ze d11 pl1:f1 pl2:f2 2 d11 do:f2 d9 5 d9 d9 d9 6 d9 d12 LOCKH_OFF d1 pl1:f1 pl2:f2 (p2 ph0):f2 d12 LOCKH_ON GRADIENT11(cnst20) ;g1=1.0m @ 5 G/cm d16 ;****************** Experiment Beginning ****************** (p1 ph0):f1 GRADIENT12(cnst21) ;g2=0.5m @ 4 G/cm d2 (d29 p1*2 ph0):f1 (p2*2 ph0):f2 d3 GRADIENT12(cnst21) d16 (p1 ph1):f1 d12 pl9:f1 (p9 ph9):f1 ;2m 1H 90 pulse => water along -Z GRADIENT13(cnst22) ;g3=1.0m @ 10 G/cm - x-axis d16 pl1:f1 (p2 ph11):f2 GRADIENT14(cnst23) ;g4=0.5m @ 8 G/cm d13 (d29 p1*2 ph0):f1 (p2*2 ph0):f2 d14 GRADIENT14(cnst23) d16 LOCKH_OFF (p2 ph1):f2 ;=============== begin T1 relaxation period ============ 8 d21 pl0:f1 (p25:sp1 ph0):f1 d21 pl0:f1 lo to 8 times l3 ; l3 must be odd d21 LOCKH_ON (p25:sp1 ph0):f1 d22 pl1:f1 GRADIENT16(cnst24) ;g4=0.5m @ 8 G/cm d16 ;================ end T1 relaxation period ============= (p2 ph12):f2 d17 (p2*2 ph13):f2 ;------------------ t1 evolution period ----------------- d0 ;t1/2 (p1*2 ph0):f1 d12 GRADIENT17(cnst25) ;g5=1.25m @ 30 G/cm for coh. selection d15 d0 ;t1/2 ;------------ start RINEPT with gradient SE ------------ (p2 ph14):f2 d6 (p1 ph0):f1 GRADIENT12(cnst21) ;g6=g2=0.5hm @ 4 G/cm d2 (p2*2 ph0):f2 (p1*2 ph0):f1 d3 GRADIENT12(cnst21) d16 d7 (p2 ph1):f2 (p1 ph1):f1 GRADIENT12(cnst21) ;g7=g2=0.5hm @ 4 G/cm d2 (d29 p1*2 ph0):f1 (p2*2 ph0):f2 d3 GRADIENT12(cnst21) d16 (p1 ph2):f1 d5 (p1*2 ph0):f1 GRADIENT18(cnst27) ;g8=0.125m @ 27.8 G/cm for refocusing d25 pl12:f2 go=2 ph31 cpd2:f2 ;******************* Experiment Ending ******************* d11 do:f2 wr #0 if #0 zd d9 ip14*2 lo to 5 times 2 d9 id0 d9 ip12*2 d9 ip31*2 lo to 6 times l4 d11 LOCKH_OFF exit ph0=0 ph1=1 ph2=2 ph3=3 ph9=190 ;optimize for water flipback ph11=0 2 ph12=1 1 3 3 ph13=0 0 0 0 1 1 1 1 2 2 2 2 3 3 3 3 ph14=0 ph31=0 2 2 0 2 0 0 2 ;**bv_t1_15nm.r loop ns { p11 { (0) | (0) | (0)+(cnst20) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p13 { (0)+(cnst22) | (0) | (0) } { (0) | (0) | (0) } p14 { (0) | (0) | (0)+(cnst23) } { (0) | (0) | (0) } p14 { (0) | (0) | (0)+(cnst23) } { (0) | (0) | (0) } p16 { (0) | (0) | (0)+(cnst24) } { (0) | (0) | (0) } p17 { (0)+(cnst25*1.800) | (0) | (0)+(cnst25) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p18 { (0)+(cnst27*1.800) | (0) | (0)+(cnst27) } { (0) | (0) | (0) } } loop ns { p11 { (0) | (0) | (0)+(cnst20) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p13 { (0)+(cnst22) | (0) | (0) } { (0) | (0) | (0) } p14 { (0) | (0) | (0)+(cnst23) } { (0) | (0) | (0) } p14 { (0) | (0) | (0)+(cnst23) } { (0) | (0) | (0) } p16 { (0) | (0) | (0)+(cnst24) } { (0) | (0) | (0) } p17 { (0)+(cnst25*1.800) | (0) | (0)+(cnst25) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p12 { (0) | (0) | (0)+(cnst21) } { (0) | (0) | (0) } p18 { (0)+(cnst28*1.800) | (0) | (0)+(cnst28) } { (0) | (0) | (0) } } ;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