;DFtstrnoesyhsqcsi ;avance-version (05/25/05) ;TIME-SHARED NOESY-HSQC ; ;developed for ILV-1H-Me samples (otherwise deuterated): ; use zgoption LABEL_CN ; ; ; ;3D sequence with ; homonuclear correlation via nOe ; correlation may be due to noe or chemical exchange ; Simultaneous H-1/X correlation via time shared inepts or PEP/ST2-PT transfers: ; |Hall(t1)->HN ->N(t2)->HN(t3) ; |Hall(t1)->HMe->C(t2)->HMe(t3) ; ;using sensitivity improvement for 13CMe/HMe and TROSY for 15N/HN ;phase sensitive (t1) ;phase sensitive using Echo/Antiecho-TPPI gradient selection (t2) both N and C ;with decoupling during acquisition on 13C ;using flip-back pulse ;using f3 - channel ;************************************* ;(use parameterset NOESYHSQCFPf3GPSI3D), then addapt as follows: ; ;cnst10: offset (ppm) for shaped inversion pulse on HMe ; have tested : ; cnst10=1: REBURP on HMe (1ppm): OK but 15N relaxation ; cnst10=-2: Q3 on Hali (-2ppm): 600us at 750 MHz (7.56 ppm bwidth) ;cnst11: offset for HMe 90 pulse (1ppm) ; warning: depending on wether water is touched or not ; you will need to add flip-backs as indicated in comments ; in the pulse program ;cnst13: 15N spectral width in ppm ;PROSOL compatible, but : then update the two following pulses: ;p27: TRIM pulse ;p28: HMe 90 pulse ;p29: HMe inversion pulse ;sp8: HMe 90 ;sp9: HMe inversion ;spnam8: 90 HMe: Sinc1.1000 or Q5 or... ;spnam9: 180 HMe, Q3 (or REB) ;Frueh DP, Vosburg DA, Walsh CT, Wagner G, JBNMR 2006 (In press 01/05/06) ;TROSY TS Version Dfrueh 052505 prosol relations= #include #include #include "p2=p1*2" "p22=p21*2" "d0=3u" "d3=1s/(cnst2*2)" "d4=1s/(cnst3*2)-1/(cnst2*2)-p3-p16-d16" "d10=3u" "d20=10u" "d11=30m" "d12=20u" "d13=4u" "d17=d16" "d18=d8-d3-d4-3*p16-2*d16-2*p3 -p21-p11-25u" "d26=1s/(cnst3*4)" ;1/4JNH "d24=1s/(cnst2*4)" ;1/4JCH "d23=d24-p4/2" ;1/4JCH "d25=d26-d24-p4/2" ; "p19=300u" "DELTA1=d13+p19+d16+4u-p28/2" "DELTA3=d23-p16-d16" "DELTA4=d26-p16-d16" "DELTA5=d10" "DELTA7=d20+p29+p3+2*p16+2*d16+2*d10" "DELTA8=d20+p29+2*d10" "DELTA9=(d26+d24)/2" "DELTA10=(d26-d24)/2" "DELTA11=(d26+d24)/2+p22/2" "DELTA12=(d26-d24)/2-p22/2" "DELTA13=(d26-d24)/2-p28/2" "DELTA14=d23-p16-d16" # ifdef LABEL_CN "DELTA=p16+d16+larger(p2,p4)+d10*2" "DELTA2=larger(p4,p22)+d0*2" # else "DELTA=p16+d16+p2+d10*2" "DELTA2=p22+d0*2" # endif /*LABEL_CN*/ "TAU=d8-p16-d16-p19-d16-10u" "in20=1/(2*cnst13*bf3/1000000)-in10" "spoff9=bf1*((cnst10)/1000000)-o1" "spoff8=bf1*((cnst11)/1000000)-o1" aqseq 321 1 ze d11 pl12:f2 2 d11 do:f2 3 d12 d1 pl3:f3 5u pl0:f1 5u (p11:sp1 ph24:r) 5u 5u pl1:f1 5u (p1 ph8) DELTA2 pl2:f2 (p2 ph9) d0 # ifdef LABEL_CN (center (p4 ph1):f2 (p22 ph1):f3 ) # else (p22 ph1):f3 # endif /*LABEL_CN*/ d0 (p1 ph10) ;5u pl0:f1 ;not needed if Radiation dampoing big enough ; 5u ; e.g. cryoprobe, high field ; (p11:sp1 ph26:r) ; 5u ; 5u pl1:f1 d3 (p3 ph1):f2 p16:gp12 ;weak gradient d16 d4 (p21 ph1):f3 p16:gp14 ;weak gradient d16 d18 5u pl0:f1 5u (p11:sp1 ph23:r) 5u 5u pl1:f1 5u (p1 ph11);-----------TS-HSQC-TROSY---- DELTA3 ;d23 p16:gp19 d16 (p4 ph6):f2 d25 (center (p2 ph1) (p22 ph6):f3 ) DELTA4 ;pl10:f1 ;d26 p16:gp19 d16 (p27 ph11) ;5u pl1:f1 (p1 ph23) 4u pl0:f1 ; (p11:sp1 ph12:r):f1 4u pl3:f3 p16:gp2 d16 pl1:f1 (p21 ph3):f3 ;TShared DELTA7 ;(p2 ph1):f1 DELTA8 (p22 ph4):f3 d20 ;(p2 ph22):f1 d20 (p3 ph3):f2 p16:gp3*EA d16 DELTA5 (p29:sp9 ph22):f1 ;REB on Hc-Me: 4ppm @ 1 ppm DELTA5 (p4 ph4):f2 d10 (p29:sp9 ph7):f1 d10 p16:gp13*EA d16 (center (p1 ph17) (p3 ph16):f2 ) ;---include flip-backs if p28 does not excite water DELTA11 pl3:f3 (p4 ph1):f2 DELTA12 (center (p2 ph1) (p22 ph1):f3 ) DELTA9 (p4 ph1):f2 DELTA10 (center (p1 ph1) (p21 ph2):f3 (p3 ph2):f2 ) DELTA11 pl3:f3 (p4 ph1):f2 DELTA12 (center (p2 ph1) (p22 ph1):f3 ) DELTA9 (p4 ph1):f2 DELTA13 (center (p28:sp8 ph2):f1 (p21 ph16):f3) ;(p21 ph1):f3 DELTA1 (p2 ph1) d13 p19:gp6 d17 pl12:f2 4u BLKGRAD go=2 ph31 cpd2:f2 d11 do:f2 mc #0 to 2 F1PH(rd10 & rd20 & ip8 & ip9 & ip24, id0) F2EA(igrad EA & ip16*2 & ip17*2, id10 &id20 & ip3*2 & ip31*2) exit ph1=0 ph2=1 ph3=0 2 ph4=0 0 ph5=1 1 ph15=3 3 ph6=0 ph7=0 0 2 2 ph8=0 0 0 0 2 2 2 2 ph9=1 1 1 1 3 3 3 3 ph10=0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ph11=0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph12=2 2 2 2 2 2 2 2 0 0 0 0 0 0 0 0 ph16=0 ph17=1 ph22=2 ph23=1 ph24=2 2 2 2 0 0 0 0 ph25=3 3 3 3 1 1 1 1 ph26=2 2 0 0 0 0 2 2 ph31=0 2 0 2 2 0 2 0 2 0 2 0 0 2 0 2 2 0 2 0 0 2 0 2 0 2 0 2 2 0 2 0 ;pl0 : 120dB ;pl1 : f1 channel - power level for pulse (default) ;pl3 : f3 channel - power level for pulse (default) ;sp1 : f1 channel - shaped pulse 90 degree ;p1 : f1 channel - 90 degree high power pulse ;p2 : f1 channel - 180 degree high power pulse ;p11: f1 channel - 90 degree shaped pulse ;p16: homospoil/gradient pulse [1 msec] ;p19: homospoil/gradient pulse [300 usec] ;p21: f3 channel - 90 degree high power pulse ;p22: f3 channel - 180 degree high power pulse ;d0 : incremented delay (F1 in 3D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d8 : mixing time ;d10: incremented delay (f3 in 3D) [3 usec] ;d11: delay for disk I/O [30 msec] ;d12: delay for power switching [20 usec] ;d13: short delay [4 usec] ;d16: delay for homospoil/gradient recovery ;d24: 1/(4J)CH for CH ; 1/(8J)CH for all multiplicities ;d26: 1/(4J(NH)) ;cnst2: = J(CH) ;cnst3: = J(NH) ;in0: 1/(2 * SW(H)) = DW(H) ;nd0: 2 ;in10: 1/(2 * SW(C)) = DW(C) ;nd10: 2 ;NS: 8 * n ;DS: >= 16 ;td1: number of experiments in F1 ;td2: number of experiments in f3 ;FnMODE: States-TPPI (or TPPI) in F1 ;FnMODE: echo-antiecho in f3 ;cpd2: decoupling according to sequence defined by cpdprg2 ;pcpd2: f2 channel - 90 degree pulse for decoupling sequence ;use gradient ratio: gpz3=-3(p19)(gpz6)/p16 ; gpz13=-7(p19)(gpz6)/p16 ; ;for z-only gradients: ;gpz1: 30% ;gpz2: -50% ;gpz3: -23.9% ;gpz4: 11% ;gpz5: 5% ;gpz6: 27% ;gpz12: 7% ;gpz13: -56.1% ;gpz14: 11% ;use gradient files: ;gpnam1: SINE.100 ;gpnam2: SINE.100 ;gpnam3: SINE.100 ;gpnam4: SINE.100 ;gpnam5: SINE.100 ;gpnam6: SINE.50 ;gpnam12: SINE.100 ;gpnam13: SINE.100 ;gpnam14: SINE.100 ;preprocessor-flags-start ;LABEL_CN: for C-13 and N-15 labeled samples start experiment with ; option -DLABEL_CN (eda: ZGOPTNS) ;preprocessor-flags-end ;modified from: $Id: noesyhsqcfpf3gpsi3d,v 1.1.2.3 2003/06/18 15:27:56 ber Exp $