# 1 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ; ; title: artsy-qjnh.pp ; summary: ARTSY-2D TROSY for measuring JNH ; author: Nick Fitzkee (nfitzkee@nih.gov) ; date: June 29, 2010 ; version: 6 (final version) ; ; See footer below for notes. ; ; Changes: ; 5.0 - Works w/ simultaenous 180's, confirmed with epsilon ~ 30 us ; 6.0 - Offset the 180 pulses during first inept, corrected delay ; ; converted to prosol standards G.C. 2011 ; *** use this for protonated proteins only! *** ; *** use "artsy_deut" for perdeuterated ones! *** prosol relations= # 1 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Avance.incl" 1 ;Avance3.incl ; for AV III ; ;avance-version (07/12/14) ; ;$CLASS=HighRes Incl ;$COMMENT= # 165 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Avance.incl" ;$Id: pulseprogram,v 1.1 2021/02/11 00:56:23 bmrbsvc Exp $ # 21 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" 2 # 1 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Grad.incl" 1 ;Grad2.incl - include file for Gradient Spectroscopy ; for 1 ; ;avance-version (07/01/17) ; ;$CLASS=HighRes Incl ;$COMMENT= # 27 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Grad.incl" define list EA= # 31 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Grad.incl" ;$Id: pulseprogram,v 1.1 2021/02/11 00:56:23 bmrbsvc Exp $ # 22 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" 2 # 1 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Delay.incl" 1 ;Delay.incl - include file for commonly used delays ; ;version 00/02/07 ; ;$CLASS=HighRes Incl ;$COMMENT= # 9 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Delay.incl" ;general delays define delay DELTA define delay DELTA1 define delay DELTA2 define delay DELTA3 define delay DELTA4 define delay DELTA5 define delay DELTA6 define delay DELTA7 define delay DELTA8 define delay TAU define delay TAU1 define delay TAU2 define delay TAU3 define delay TAU4 define delay TAU5 # 29 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Delay.incl" ;delays for centering pulses define delay CEN_HN1 define delay CEN_HN2 define delay CEN_HN3 define delay CEN_HC1 define delay CEN_HC2 define delay CEN_HC3 define delay CEN_HC4 define delay CEN_HP1 define delay CEN_HP2 define delay CEN_CN1 define delay CEN_CN2 define delay CEN_CN3 define delay CEN_CN4 define delay CEN_CP1 define delay CEN_CP2 # 48 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Delay.incl" ;loop counters define loopcounter COUNTER define loopcounter SCALEF define loopcounter FACTOR1 define loopcounter FACTOR2 define loopcounter FACTOR3 # 58 "/opt/topspin3.0/exp/stan/nmr/lists/pp/Delay.incl" ;$Id: pulseprogram,v 1.1 2021/02/11 00:56:23 bmrbsvc Exp $ # 23 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" 2 # 1 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/bits.gc" 1 ;bits.gc for dexter (AVIII console) # 10 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/bits.gc" define pulse PG1 define pulse PG2 define pulse PG3 define pulse PG4 define pulse PG5 define pulse PG6 define pulse PG7 define pulse PG8 define pulse PG9 define pulse PG10 define pulse PG11 define pulse PG12 define pulse PG13 define pulse PG14 define pulse PG15 define pulse PG16 define pulse PG17 define pulse PG18 define pulse PG19 define pulse PG20 define pulse PG21 define pulse PG22 define pulse PG23 define pulse PG24 define pulse PG25 define pulse PG26 define pulse PG27 define pulse PG28 define pulse PG29 define pulse PG30 define pulse PG31 # 24 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" 2 # 26 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ;--- SWITCH ----- # 30 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ;Gradient Pulses "PG1=1m" ;half-encoding "PG3=500u" "PG4=500u" ;half-encoding "PG5=250u" "PG6=800u" ;"PG7=101.3u" ;decoding "PG7=99.9u" ;decoding - optimize for max. signal "l5=1" "l6=1" "d0=3u" ;use if set up for (0,0) 15N phase # 45 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" "DELTA4=p14*2+4u+d0*2+p21*1.274-p1" ;phc0=0 phc1=0 aliased peaks same sign ;"d0=in0*0.5-p21*0.637-2u-p14+p1*0.5" ;ph0=90deg ph1=-180deg # 51 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ;note well: will still require a little ; phase correction in 15N and; ; will not likely be perfect for ; all peaks. This is due to ; sequence design. "p2=p1*2" "p22=p21*2" "d11=30m" "d12=100u" "d16=190u" ;Gradient recovery "d28=p51+5u+p1-p21" ; Delays to compensate composite 15N 180 "d29=p21*4.34" # 67 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ; Adjust for Clean TROSY (with phcor14) - total time for 1st S3E element ;"d25=2.71m" "d25=2.345m" ; Total time of 1st transfer step (1/JNH) ; Adjust this so 2nd FID is a null for isotropic sample ; In the attenuated spectrum, the coupling will evolve for d27, and in ; the reference spectrum, it will evolve for d27*0.5 + 0.637*p1. "d27=9.4m" "DELTA1=d27-d29*3-p1*1.237-80u" "DELTA2=d25-PG5-p50-d16" "DELTA3=2.71m-PG6-p51-205u" "DELTA5=300u-PG7-20u-p1-3u" # 82 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" "cnst21=174" "cnst22=54" "spoff3=bf2*((cnst22-cnst21)/1000000)" "spoff5=0" # 1 "mc_line 88 file /opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam dc-measurement inserted automatically" dccorr # 88 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" 1 ze 1m 2 10u do:f2 1m setnmr3^0 setnmr0^34^32^33 ctrlgrad 7 d11 fq=cnst21(bf ppm):f2 ;f2 on CO d12*6 3 d12*6 4 d12*6 5 d1 1m setnmr3|0 setnmr0|34|32|33 ctrlgrad 0 10u pl0:f1 10u pl3:f3 10u pl0:f2 10u # 103 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" (p21 ph0):f3 ; along with cycling ph5, 3u ; this thoroughly eliminates PG1:gp1 ; 15N Boltzmann magnetization 500u ;- start 90-degree on hn -------------------------------------- (p50:sp50 ph6:r):f1 3u 3u pl1:f1 10 (p1 ph5):f1 5u 5u gron2 DELTA1*0.25 10u groff d29*2 5u pl0:f1 5u gron2 DELTA1*0.25 10u groff # 124 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" if "l6==1" goto 20 (center (p52:sp54 ph0):f1 (p21 ph0 p21*2.34 ph1 p21 ph0):f3) 5u 5u gron2 DELTA1*0.25 10u groff d29 goto 25 20 (p52:sp54 ph0):f1 d29*0.75 5u 5u gron2 DELTA1*0.25 10u groff (p21 ph0 p21*2.34 ph1 p21 ph0):f3 d29*0.25 25 5u pl1:f1 5u gron2 DELTA1*0.25 10u groff (p1 ph1):f1 30 3u 3u pl0:f1 (p50:sp53 ph11:r):f1 3u 3u pl1:f1 # 153 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ;goto 100 ;WARNING - make sure pl14 is set properly for f2' dec ; or comment out f2' AQ cpd before using this ; statement. Ditto for all 'goto 100's'. PG3:gp3 d16 ;- quantitative-J finished, start 15N evolution --------------- # 162 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" if "l5==1" { (p21 ph17):f3 } else { (p21 ph7):f3 } d0 (p14:sp3 ph0):f2 4u (p14:sp5 ph0):f2 # 176 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" d0 PG4:gp4*EA ;half-encoding pulse 200u if "l5==1" { (p22 ph17):f3 } else { (p22 ph7):f3 } PG4:gp4*EA*-1 ;half-encoding pulse 200u DELTA4 ;comment out if 90,180 delay selected ;- start final TROSY back-transfer ---------------------------- # 191 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" (p1 ph12):f1 3u 2u pl0:f1 (p50:sp51 ph21:r):f1 ;goto 100 5u PG5:gp5 DELTA2 d16 pl1:f1 (center (p2 ph0):f1 (p22 ph0):f3) 5u DELTA2 PG5:gp5 d16 pl0:f1 (p50:sp52 ph22:r):f1 3u 2u pl1:f1 (p1 ph0):f1 (p21 ph15):f3 5u ;goto 100 PG6:gp6 195u pl6:f1 DELTA3 (150u p51 ph10:r 3u 2u pl1 p2 ph0 3u 2u pl6 p51 ph10:r):f1 (d28 p22 ph15):f3 3u 2u pl1:f1 ;goto 100 PG6:gp6 DELTA3 45u (p21 ph14:r):f3 3u PG7:gp7 ;decoding gradient DELTA5 100 5u 5u pl14:f2 10u setnmr3^0 setnmr0^34^32^33 ctrlgrad 7 go=2 ph31 cpds2:f2 # 233 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" 10u do:f2 1m setnmr3^0 setnmr0^34^32^33 ctrlgrad 7 d11 wr #0 if #0 zd d12*6 iu6 lo to 3 times 2 # 242 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" d12 igrad EA d12 ip12*2 d12 ip21*2 d12 ip14*2 d12 iu5 d12 ru6 lo to 4 times 2 d12 ip7*2 d12 ip17*2 d12 ip31*2 d12 id0 d12 ru5 d12 lo to 5 times l3 ; l3 = nr. of increments in each spectrum, 1 td = 2*l3 (for the pair) 1m do:f2 1m do:f3 1m setnmr3^0 setnmr0^34^32^33 ctrlgrad 7 exit ph0=0 ph1=1 ph2=2 ph3=3 ph5=0 2 ph6=2 0 ph7=1 1 3 3 ph10=2 ph11=3 ph12=3 ph14=3 3 3 3 1 1 1 1 ph15=0 0 0 0 2 2 2 2 ph17=1 1 3 3 ph21=1 ph22=0 ph31=1 3 3 1 3 1 1 3 # 281 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ;---- NOTES ----- ; tested on Bruker AVIII TS2-PL3 consoles ; Note: when used on older dmx/drx consoles, add 3u between pulses ; in the 15N composite pulse (and adjust d29, d30) ; All "goto 100" statements are at points where water flip-backs can ; be tuned. See note above at first statement. # 290 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ;1H pulses (f1=f1, center on H2O): ;p1 = 90 deg (10us) hard 1H pulse @ pl1 ;p51 = 1.2ms soft 90 deg pulse @ pl6 ;p50 = 1.9m @ sp50, sp51, sp52, sp53 (spnam50,51,52,53 = sinc1.0) - fine adjusted flipbacks ;p52 = 1.5m @ sp54 (spnam54 = reburp.1000) spoffs54= 2100 Hz (HN 3ppm off resonance) spoal54=0.5 ;15N pulses (f3=f3, carrier=119ppm): ;p21 = 90 deg (~50us) 15N pulse @pl3 ;13C pulses (f2=f2, carrier=174ppm): ;p14 @ sp3 180 Ca spnam3=Q3.1000 256u@600 spoffs3= -120ppm (Ca off resonance) spoal3=0.5 ;sp3: f2 channel - shaped pulse 180 degree (Ca off resonance) ;p14 @ sp5 180 CO spnam5=Q3.1000 256u@600 spoffs5= 0 (f2=O on resonance) spoal5=0.5 ;sp5: f2 channel - shaped pulse 180 degree (CO on resonance) ;p61: C13 (f2) 90 deg low power dec on CO (p61=120u@600) @pl14 ;pcpd2: f2 channel - 90 degree pulse for decoupling sequence ;cpd2: aq f2' dec program for 13C samples cpdprg2: garp.p61 ;pl14: C13 (f2) - power level (low) for CPD/BB decoupling # 309 "/opt/topspin3.0/exp/stan/nmr/lists/pp/user/pr_artsy_prot_fam" ;f3 SW = 1/(2*in0) ;echo-antiecho in N15 ;l3 = nr. of increments in each spectrum, 1 td = 2*l3 (for the pair) ;RECT pulse pairs do not work well on an AVIII ;gpz1 = +33% sine.100 Boltzmann killer ;gpz2 = +0.5 (gron2) ;gpz3 = +17% sine.100 zz crusher gradient ;gpz4 = +70% sine.20 encoding gradient ;gpz5 = +15% sine.50 ;gpz6 = +23% sine.50 ;gpz7 = +70% sine.10 decoding gradient