# 1 "/u/exp/stan/nmr/lists/pp/gcbcaconhfbBR.nl" ;gcbcaconhfbBR.nl from gcbcaconh3dBR S.Tate 02/08/12 ; ;Avance ;3D CBCA(CO)NH ;phase sensitive using Water Flip Back version ;D. R. Muhandiram and L. E. Kay, J. Magn. Reson. B 103, 203 - 216, (1994) ; ; o1p=~4.7ppm, o2p=43ppm, o3p=117ppm ; o2p is changed in the pulse to 177ppm, D=177-43ppm=20221Hz ; cnst15=20221Hz, If you change o2p, change cnst15 ; set in6=in0 & in7=in10 in xwinnmr manually or by au, set_ctBR ; p19 & p20 is used for 15N coherence seletion, p19:gp12 & p20:gp13*0.5*EA ; modified by D.Kohda 981211 rectangular grad & phcor6 ; modified D.Kohda EA syntax, xwinnmr v2.6PL4 ; modified D.Kohda 000131 water flipback ; (flipback) D. Nietlispach .. E.D.Laue JACS 118, 407-415 (1996) ; modified S.Tate longer 15N evolution 04/03/12 ; modified S.Tate suppress. Bloch-Siegert Effect with Cos-mod Seduce ; modified S.Tate Additional gradient echo at 13ca->13C=o INEPT 040510 ; modified S.Tate Mod. cos-modulation inversion with seduce ; modified S.Tate nus introduced ; ;phase correction: (0deg,0deg) for 15N(t1) ; (0deg,0deg) for 13C(t2) ;fixed delays "d11=30m" ;disk I/O "d12=20u" ;power switching "d13=5u" ;short delay, but used as power switching in this pulse, greater than 4u "p19=1m" ;coherent selection (15N) "p20=200u" ;cohenrece selection (1H) "d17=100u" ;short grad recovery define delay TC define delay TN define delay TAUA1 define delay TAUA2 define delay TAUB define delay TAUC1 define delay TAUC2 define delay TAUC3 define delay TAUD define delay TAUD1 define delay TAUD2 define delay TAUE define delay TAUE1 define delay CEN_HC1 define delay CEN_HN1 define delay CEN_HN2 define delay CEN_CN1 "p2=p1*2" ;1H high power 90 and 180deg pulse "p7=48u" ;13Cab(43ppm) 90deg pulse at PL7=9.0dB @600MHz, null at CO(177ppm) "p8=43u" ;13Cab(43ppm)180deg pulse at PL8=1.7dB @600MHz, null at CO(177ppm) "p23=54u" ;13CO(177ppm) 90deg pulse at PL23=10.15dB @600MHz, null at Ca(57ppm) "p24=48u" ;13CO(177ppm)180deg pulse,p23*2 "p14=310u" ;13CO(177ppm)180deg cos-mod seduce inversion pulse (+/- 20kHz) "p13=48u" ;13Ca(57ppm) 180deg rec96BR SP10=2.9dB offset=-18000 "p22=p21*2" ;15N high power 90 and 180deg pulse at PL3=-6dB "TC=3.6m" ;2TC=constant time of 13C (F2) "TN=12.8m" ;2TN=constant time of 15N (F1) define pulse PULWAL ;pw90 of waltz16 dec on f1 (40u, pcpd1) "PULWAL=40u" ;SL time of waltz16 dec on f1, set to pcpd1, 40u define delay DELT15N define delay DELT13C "DELT15N=1s/(cnst2*4)" ;typical value 1/4*100 = 2.5m, 1/4*110=2.3m "DELT13C=1s/(cnst3*4)" ;typical value 1/4*145 = 1.7m define delay CORSED define delay CORWAL "CORSED=8u" "CORWAL=8u+PULWAL" "d0=5u" "TAUA1=DELT13C-p18-d13-d16" "TAUB=1.1m-p14" ;see Kay's paper "TAUC1=TC-1.1m-p2-(p18+d13+d16)" "d7=TC-(p18+d13+d16)-(p14+d13)+d0" "TAUC2=TC-p14-d13-CORWAL*2-d13-d16-p17" "TAUC3=TC-p14-d13-CORWAL*2-d13-d16-p17" "d10=5u" ;greater than 4u, phase presetting time of p14:sp2 "d6=TN-d10-CORSED*2" "TAUD=4.4m" "TAUD1=TN-TAUD-p13" "TAUD2=TN-p13-d12" "TAUE=5.44m-CORSED-CORWAL" "TAUE1=TN-5.4m-CORSED-d10*2" "TAUA2=DELT15N-p17-p6-d13*2-d12-5u" "CEN_HC1=(p8-p2)/2" "CEN_HN1=(p22-p2)/2" "CEN_HN2=(p21-p1)/2" "CEN_CN1=(p22-p24)/2" ;DECOUPLING DEFINITIONS ;---------------------- ;#define SED_OFF 4u do:f2 \n 4u pl2:f2 ;loop counter assignments "l0=(td1*td2/4)" "l1=(td2)" ;DIMENSIONALITY FLAGS # 1 "/u/exp/stan/nmr/lists/pp//Avance.incl" ;Avance.incl ; ;version 99/08/02 # 116 "/u/exp/stan/nmr/lists/pp/gcbcaconhfbBR.nl" # 1 "/u/exp/stan/nmr/lists/pp//Grad.incl" ;Grad.incl - include file for Gradient Spectroscopy ;avance-version ;version 99/02/19 define list EA= # 117 "/u/exp/stan/nmr/lists/pp/gcbcaconhfbBR.nl" aqseq 312 1 ze 2 d11 do:f3 10m 3 20m 4 15m 5 20m 6 d1 fq=0:f2 ;switch carbon frequency to 13Cab at 43 ppm ;6 d1 fq2:f2 ;switch carbon frequency to 13Cab at 43 ppm ; purging of 13Cab magnetization d12 pl7:f2 ;power for 13C 90deg pulse 50u setnmr2|0 setnmr0|34 (p7 ph0):f2 d13 p19:gp7 ;g1 d16*2 pl1:f1 ;gradient recovery & reset 1H power ; program starts (p1 ph0):f1 d13 p18:gp6 ;g2 d16 TAUA1 pl8:f2 (CEN_HC1 p2 ph0):f1 (p8 ph10):f2 TAUA1 pl3:f3 d13 p18:gp6 ;g3 d16 (p1 ph4):f1 ;begin INEPT transfer H to C d13 p15:gp2 ;g4 Iz filter d16 pl7:f2 (p7 ph1):f2 d0 pl0:f2 ;t1/2 (p14:sp2 ph0):f2 (p22 ph0):f3 TAUB ;taub (p2 ph0):f1 TAUC1 pl8:f2 ;T - TAUB d13 p18:gp16 d16 (p8 ph0):f2 d13 p18:gp16 ;g6 d16 d7 pl0:f2 ;T - t1/2 (corrected by d12+p18+p14+d13) (p14:sp2 ph0):f2 ;Bloch Siegert compensation pulse d13 pl7:f2 (p7 ph0):f2 d13 pl0:f2 (p14:sp2 ph0):f2 ;Bloch Siegert compensation pulse 4u pl19:f1 \n (PULWAL ph21):f1 \n 4u cpds1:f1 ;1H DEC. on TAUC2 pl8:f2 ;begin H decoupling 4u do:f1 \n (PULWAL ph22):f1 \n 4u pl1:f1 ;1H DEC. off d13 ;g7 p17:gp3 d16 (p8 ph0):f2 d13 pl0:f2 (p14:sp2 ph0):f2 d13 ;g7 p17:gp3 d16 4u pl19:f1 \n (PULWAL ph21):f1 \n 4u cpds1:f1 TAUC3 pl7:f2 4u do:f1 \n (PULWAL ph22):f1 \n 4u pl1:f1 ;1H DEC. off (p7 ph0):f2 ;begin transfer Ca to CO d13*2 fq=cnst15:f2 ;Frq. switch p15:gp7 ;g7 Iz filter d16 pl23:f2 4u pl19:f1 \n (PULWAL ph21):f1 \n 4u cpds1:f1 ;H-dec restarts (p23 ph0):f2 TAUD pl0:f2 (p13:sp10 ph0):f2 ;13Ca 180deg SLP pulse TAUD1 pl24:f2 (CEN_CN1 p24 ph0):f2 (p22 ph0):f3 TAUD2 pl0:f2 (p13:sp10 ph0):f2 ;Bloch Siegert compensation pulse d12 pl23:f2 (p23 ph0):f2 ;begin INEPT transfer CO to N 4u do:f1 \n (PULWAL ph22):f1 \n 4u pl1:f1 ; H-dec interrupted p15:gp14 ;g8 IzSz filter d16 pl3:f3 4u pl19:f1 \n (PULWAL ph21):f1 \n 4u cpds1:f1 (p21 ph2):f3 4u pl0:f2 \n 4u cpds6:f2 d6 ;TN - t1/2 ;4u do:f2 \n 4u pl23:f2 4u do:f2 4u pl24:f2 (CEN_CN1 p24 ph0):f2 (p22 ph3):f3 4u pl0:f2 \n 4u cpds6:f2 TAUE1 d10 ;TN + t1/2 - TAUE 4u do:f1 \n (PULWAL ph22):f1 \n 4u pl1:f1 ;end H1 decoupling TAUE 4u do:f2 \n 4u pl23:f2 (p21 ph0):f3 d13 p15:gp10 d16 (p11:sp1 ph11:r):f1 d13 d12 pl1:f1 (p1 ph0):f1 d13 5u p17:gp3 TAUA2 pl6:f1 d13 (p6 ph6:r):f1 d12 pl1:f1 ; Water Gate (CEN_HN1 p2 ph5):f1 (p22 ph0):f3 d12 pl6:f1 (p6 ph6:r):f1 d13 5u ph31 p17:gp3 ;g13 d15 TAUA2 pl16:f3 d13 setnmr2^0 setnmr0^34 go=2 ph31 cpd3:f3 d11 do:f3 wr #0 if #0 zd d12 ip2 ; 15N pulse phase increment d12 lo to 3 times 2 d12 ip1 ; 13C pulse phase increment d12 lo to 5 times 2 ; reset phase & increment d12 rd10 d12 rd6 d12 rd0 d12 rd7 d12 rp2 d12 rp1 d12 rp31 ; increment 15N States-TPPI 95 100u d12 id10 d12 dd6 d12 ip2*2 d12 ip31*2 50m lo to 95 times c d12 ivc ; increment 13C States-TPPI 96 100u d12 id0 d12 dd7 d12 ip1*2 d12 ip31*2 50m lo to 96 times c d12 ivc lo to 4 times l0 ;#ifdef ; 10m ip1 ; lo to 3 times 2 ; 5m id0 ; 5m dd7 ip31*2 ; lo to 4 times l0 ;#endif ;#ifdef ; 10m rd0 ip2 ; 5m rd7 ; lo to 5 times 2 ; 10m id10 ip31*2 ; 10m dd6 ; lo to 6 times l1 ;#endif d12 do:f1 d12 do:f2 d12 do:f3 exit ph0=0 ph10=1 ph1=0 0 2 2 ph2=0 2 ph3=0 0 0 0 2 2 2 2 ph4={1}*8 {3}*8 ph5=2 ph18=0 ph19=(3600) 0 ; tuning ph6=ph18+ph19 ; phcor6 is effective ph20=2 ; water flip back (hgauss) ph11=ph20+ph19 ; phcor11 is effective ph21=1 ;waltz16BR SL at start ph22=3 ;waltz16BR SL at end ph31=0 2 2 0 0 2 2 0 2 0 0 2 2 0 0 2 ;spnam10: rec96BR ;p13: shaped 180 degree for Ca [48u @600] or [108u @600] ;sp10: power for p13 [2.65dB @600] or [9.95dB @600] ;sp2: power for cos-mod dual inversion +/- 20kHZ sedcos0BR (6.3dB = 12.3-6 dB) ;p14: 310u inversion with sedcos0BR ;spnam2: sedocs0BR (cos mod at 20kHz) ;cpds6: SEDUCE-1 sequence for off-resonance carbonyl decoupling, cosine modulated ;pcpd2: 310u in cpdprg6 ;sp14: 18.9-6=12.9dB, -6 for double in cpdprg6 ;spoffs14: zero ;spnam14: sedcos0BR (cos mod at 20kHz) ;cosine mod is for minimization of Bloch Siegert effects. ;ns: 2*n ;ds: ns*2*n ;in0 = in7: 1 / (2 * SW(F1)=DW(F1) 15N spectral width, ;typically 30 ppm or less ;in10 = in6: 1 / (2 * SW(F2))=DW(F2) 13C spectral width, ;typically 60 - 80 ppm ;nd0: 2 ;nd10: 2 ;MC2(F1): echo-antiecho ;MC2(F2): States ;AQORDER: 3-1-2 ;default#comment#start 2000/1/25 D.Kohda ;------------------------------------------------ ;pl0: power for shutoff [120] ;pl1: power for 1H(f1) hard [5.8] ;pl2: power for 13C(f2) hard [-3] ;pl3: power for 15N(f3) hard [-3.4] ;pl4: power for 2H(f4) hard [120?] ;pl6: power for water selective [~45] ;pl7: power for 48u 13C 90deg, delta=20kHz [8.9] ;pl8: power for 43u 13C 180deg, delta=20kHz [1.55] ;pl23: power for 54u 13C 90deg, delta=18kHz [9.95] ;pl24: power for 48u 13C 180deg, delta=18kHz [2.65] ;pl25: power for 68u 13C 90deg, delta=14kHz [12] ;pl26: power for 61u 13C 180deg, delta=14kHz [5.1] ;pl9: power for 1H presat in h2o [~60] ;pl19: power for 1H(f1) cpd, pcpd1=40u [~18] ;pl12: power for 13C(f2) cpd, WURST [14] ;pl16: power for 15N(f3) cpd, pcpd3=200u [10.1] ;pl27: power for 1H(f1) tocsy or 3-9-19 pulse, 30u [~15] ;pl28: power for 13C(f2) tocsy, 36u [6.3] ; ;p0: variable pulse [0.1u] ;p1: hard pulse, 1H 90deg [~10u] ;p2: hard pulse, 1H 180deg ;p3: hard pulse, 13C 90deg [14.8u] ;p4: hard pulse, 13C 180deg ;p21: hard pulse, 15N 90deg [47u] ;p22: hard pulse, 15N 180deg ;p6: rec. soft pulse, 1H water selective [1m] ;p7: rec. soft pulse, 13C 90deg, delta=20kHz [48u] ;p8: rec. soft pulse, 13C 180deg, delta=20kHz [43u] ;p23: rec. soft pulse, 13C 90deg, delta=18kHz [54u] ;p24: rec. soft pulse, 13C 180deg, delta=18kHz [48u] ;p25: rec. soft pulse, 13C 90deg, delta=14kHz [68u] ;p26: rec. soft pulse, 13C 180deg, delta=14kHz [61u] ;p27: tocsy rec. pulse, 1H tocsy or 3-9-19 pulse [30u] ;p28: tocsy rec. pulse, 13C tocsy [36u] ;p29: wurst filter [700u] ;p11: shaped soft pulse, 1H water selective [2.1m] ;p9: adiabatic pulse, 13C sech5BR [320u] ;p10: shaped pulse, 13C vega1BR [316u] ;p12: adiabatic pulse, 13C wurst_invBR [360u] ;p14: shaped pulse, 13C sinc1BR [200u] ;p13: shaped pulse, 13C sinc1BR, rec128BR [108u] ;p15: gradient pulse, Iz filter [1m] ;p16: gradient pulse, Iz filter [2.5m] ;p17: gradient pulse, watergate [500u] ;p18: gradient pulse, 180deg sandwich [500u] ;p19: gradient pulse, purge, coherence selection [1m] ;p20: gradient pulse, variable, coherence selection [200u] ; ;spnam1: halfgaus1BR ;spnam3: gauss ;spnam4: sech5BR ;spnam11: wurst_invBR ;spnam5: sinc1BR ;spnam10: rec128BR ;spnam6: offpresatdownBR ;spnam7: vega1BR ;spnam15: wurst40k_140jBR ;spnam14: sedcos1BR ;spnam8: wurst23k_700uBR (wurst filter) ;spnam9: SSpulseBR ; ;sp1: shape power for water selective [~45] ;sp3: shape power (not used) [120] ;sp4: shape power for sech5BR [-1] ;sp5: shape power for sinc1BR [11.1] ;spoff5: offset [20000Hz] ;sp10: shape power for rec128BR [9.95 if p13=108u] ;spoff10: offset [-18000Hz] ;sp11: shape power for wurst_invBR [0] ;sp6: shape power for offresonane presat [~60] ;sp7: shape power for vega1BR [-3] ;sp15: shape power for wurst cpd [14,wurst40k_140jBR] ;sp14: shape power for sedcos1BR [12.9=18.9 - 6] ;sp8: shape power for wurst filter [12.5] ;sp9: shape power for SSpulseBR [120] ; ;cnst2: practical 1JHN [100Hz] ;cnst3: practical 1JHC [145Hz] ;cnst4: filter 1JHC (aliphatic) [135Hz] ;cnst5: filter 1JHC (aromatic) [175Hz] ;cnst6: exact 1JNH [90Hz] ;cnst12: 13C o2p offset-1 [-20221Hz] 177ppm-43ppm ;cnst13: 13C o2p offset-2 [-18108Hz] 177ppm-57ppm ;csnt14: 13C o2p offset-3 [-8903Hz] 177ppm-115ppm ;cnst15: 13C o2p offset-1 [20221Hz] 177ppm-43ppm ;cnst16: 13C o2p offset-2 [18108Hz] 177ppm-57ppm ;cnst17: 13C o2p offset-3 [8903Hz] 177ppm-57ppm ;cnst20: 16 ;gs mode ;cnst21: 16 ;gs mode ;cnst22: 20 ;gs mode ;cnst23: 20 ;gs mode ;cnst24: 16 ;gs mode ;cnst25: 40 ;coherence selection in gs mode (15N) ;cnst26: 40.5 ;coherence selection in gs mode (1H) echo ;cnst27: -40.5 ;coherence selection in gs mode (1H) antiecho ; ;cpdprg1: 1H cpd, waltz16BR ;cpdprg2: 13C cpd, wurstBR ;cpdprg3: 15N cpd, waltz16BR ;cpdprg4: 2H cpd, waltz16BR ;cpdprg6: 13C cpd, seduce1BR ;cpdprg7: 13C cpd, seduce1aBR ; ;pcpd1: 1H cpd [40u] ;pcpd2: 13C cpd, wrust [1.429m], 310u or 420u for seduce1-shaped WALTZ16 decoupling ;pcpd3: 15N cpd [200u] ;pcpd4: 2H cpd ; ;gpnam0: variable [sine.20] ;gpnam1: Iz fitler-1 [sine.20] ;gpnam2: Iz filter-2 [sine.20] ;gpnam10: Iz filter-3 [sine.20] ;gpnam3: watergate [sine.20] ;gpnam4: water refocus [sine.20] ;gpnam5: purge during mixing [sine.20] ;gpnam6: 180 sandwich-1 [sine.20] ;gpnam16: 180 sandwich-2 [rectangular.1] ;gpnam7: initial purge [sine.20] ;gpnam8: isotope filter-1 [sine.20] ;gpnam9: isotope filter-2 [sine.20] ;gpnam11: sine.20 ;gpnam12: coherence selection 1 & 2, 15N [rectangular.1] ;gpnam13: coherence selection 1, 1H [rectangular.1] ;gpnam14: coherence selection 2, 1H [rectangular.1] ;gpnam15: coherence selection 2, 1H [rectangular.1] ;gpnam17: coherence selection 3, 13C [rectangular.1] ;gpnam18: coherence selection 3, 1H [rectangular.1] ;gpnam19: coherence selection 3',13C [rectangular.1] ;gpnam20: bipolar gradient-1a [rectangular.1] ;gpnam21: bipolar gradient-1b [rectangular.1] ;gpnam22: bipolar gradient-2a [rectangular.1] ;gpnam23: bipolar gradient-2b [rectangular.1] ;gpnam24: bipolar gradient-3a [rectangular.1] ;gpnam25: bipolar gradient-3b [rectangular.1] ; ;gpx1: [0] ;gpy1: [0] ;gpz1: [33] ;gpx2: [0] ;gpy2: [0] ;gpz2: [-31] ;gpx3: [10] ;gpy3: [10] ;gpz3: [10] ;gpx4: [-10] ;gpy4: [-10] ;gpz4: [-10] ;gpx5: [0] ;gpy5: [0] ;gpz5: [13] ;gpx6: [11] ;gpy6: [-11] ;gpz6: [0] ;gpx16: [7] ;gpy16: [7] ;gpz16: [0] ;gpx7: [20] ;gpy7: [20] ;gpz7: [0] ;gpx8: [0] ;gpy8: [0] ;gpz8: [28] ;gpx9: [17] ;gpy9: [-17] ;gpz9: [17] ;gpx10: [0] ;gpy10: [0] ;gpz10: [17] ;gpx12: [0] ;gpy12: [0] ;gpz12: [40] ;gpx13: [0] ;gpy13: [0] ;gpz13: [40.5] ;gpx14: [9] ;gpy14: [9] ;gpz14: [40.5] ;gpx15: [9] ;gpy15: [9] ;gpz15: [0] ;gpx17: [0] ;gpy17: [0] ;gpz17: [-50] ;gpx18: [0] ;gpy18: [o] ;gpz18: [31.4] ;gpx19: [7] ;gpy19: [7] ;gpz19: [-50] ;gpx20: [1.0] ;gpy20: [1.0] ;gpz20: [1.0] ;gpx21: [-1.0] ;gpy21: [-1.0] ;gpz21: [-1.0] ;gpx22: [0] ;gpy22: [0] ;gpz22: [3.0] ;gpx23: [0] ;gpy23: [0] ;gpz23: [-3.0] ; ;d0: first increment ;d10: second increment ;d20: third increment ;d6: decrement in constant-time with d0 ;d7: decrement in constant-time with d10 ;d9: decrement in semi constant-time with d7,d8 ;d1: relaxation delay [1.2s] ;d4: 1/4JXH ;d8: mixing time (NOESY,TOCSY) ;d21: CT time ;d11: disk I/O [30m] ;d12: long delay [20u] ;d13: short delay [5u] ;d14: very short delay [0.1u] ;d16: gradient recovery [100u] ;d17: short grad recovery [50u] ;d31: internal use or another short delay [2u] ; ;phcor6: phase correction-1 for p6 ;phcor7: phase correction-2 for p6 ;phcor8: phase correction-3 for p6 ;phcor9: phase correction-4 for p6 ;phcor11: phase correction for p11 ; ;l16: define the length of 15N relaxation ;l17: switch for noe on/off etc. [0/1] ;fq1list: not used ;fq2list: not used ;default#comment#end