# 1 "/u/exp/stan/nmr/lists/pp/ko_cryo_HCCHTOCSY3d.7pr" ;ko_hcchtocsy Ver.12/7/1999 ; modified at 14/2/2001 ;for Avance consoles. ;3D HCCH-TOCSY. ;Kay, L. E. et al., J. Magn. Reson, Ser B 101, 333-337 (1993) ;using DIPSI-3 scheme for 13C isotropic mixing. ;Phase-sensitive mode using States-TPPI(F1,F2). ; ;F1(1H)-ch: ;p1:90deg,pl1, pl1:@-3dB. ;p3: ~7ms ;p4: ~4.3ms ;pl7:~10kHz purge pulse for p3,4 ;pl9:presaturation pulse (<50Hz) ~58dB ;F2(13C)-ch: ;p13:90deg hard pulse,pl2 ;p8:tocsy mixing pulse 90deg,pl8 ;pcpd2:90deg,pl12 ;p11:(2ms spin lock, pl8). ; ;pl2:~18.8u@2.0dB ;pl8:~35u@7.1dB ;pl12:~75u@xx.xdB. ;l1:cycle for mixing time ; p8*54.33*4*l1 ; ;F2(13C')-ch: ;p24:SEDUCE1(i_seduce1_100),sp2 ;sp2:192u@9.5dB. ; ;F3(15N)-ch: ;p21:90deg,pl3 ;pl3:~49u@0dB. ;Gradients (total: 13). ; p15(cnst21)-p15(cnst21) : echo. ; p16(cnst22) : spoil. ; p17(cnst23)-p17(cnst23) : echo. ; p17(cnst23)-p17(cnst23) : echo. ; p18(cnst24) ; spoil. ; p19(cnst25) ; spoil. ; p15(cnst26)-p15(cnst26) : echo. ; p15(cnst27)-p15(cnst27) : echo. # 1 "/u/exp/stan/nmr/lists/pp/Avance.incl" 1 ;Avance.incl ; ;avance-version (03/02/17) ;$Id: pulseprogram,v 1.1 2021/02/10 23:29:19 bmrbsvc Exp $ # 48 "/u/exp/stan/nmr/lists/pp/ko_cryo_HCCHTOCSY3d.7pr" 2 # 1 "/u/exp/stan/nmr/lists/pp/Grad.incl" 1 ;Grad.incl - include file for Gradient Spectroscopy ; ;avance-version (02/05/31) define list EA= ;$Id: pulseprogram,v 1.1 2021/02/10 23:29:19 bmrbsvc Exp $ # 49 "/u/exp/stan/nmr/lists/pp/ko_cryo_HCCHTOCSY3d.7pr" 2 ;defined parameters. ;for gradient ;"p26=400u" ;"p27=100u" ;"p16=2.0m" ;"p28=7.0m" ;"p29=4.4m" ;for adjusting centre of 180 pulses. "d11=p13-p1" ; 13C_90 - 1H_90. ;for 1H->13C INEPT and t1(1H) evolution.. "d0=4u" "d3=1.5m-p26-100u" "d8=8u+p13*2.0" ;for t2(13C) evolition. "d10=4u" "d2=475u-p24*0.5-p21*2.0-p27-100u" "d4=475u-p24*0.5-p1*2.0-p27-100u" "d6=475u-p24*0.5-p27-100u" ;for 13C->1H rev-INEPT. "d5=1.1m-p26-100u" "d13=1.5m-p26-128u-p13*2.0" ;for indirect dimention "l3=td1/2" "l4=td2/2" "spoff2=bf2*(cnst21/1000000)-o2" ;pulse sequence. ;---------- 20u do:f2 20u do:f3 30m setnmr2^0 setnmr0^34^32^33 ze 1 65m do:f2 ; 13C CPD stop. 2 30m 3 30m 4 30m ; relaxation delay = d1 + 150ms. ;---------- INEPT 1H->13C including t1(1H) evolution. 5 20u pl9:f1 d1 cw:f1 ph29 4u do:f1 20u pl1:f1 ; 1H power -> pl1. 20u pl3:f3 ; 15N power -> pl3. 50u setnmr2|0 setnmr0|34|32|33 ;---------- (p1 ph1):f1 ;========== 1st gradient pulse (echo). 5u p26:gp1 95u ;========== d0 d3 pl2:f2 ; 13C power -> pl2. (p13*2.0 ph10):f2 d0 (p1*2.0 ph0):f1 ;========== 2nd gradient pulse (echo). 5u p26:gp1 95u ;========== d8 d3 (p1 ph2):f1 ;========== 3rd gradient pulse (spoil). 5u p16:gp2 95u ;========== 200u ;---------- t2(13C) evolution. (p13 ph11):f2 d10 (p21*2.0 ph20):f3 ;========== 4th gradient pulse (echo). 5u p27:gp3 95u ;========== d2 (p24:sp2 ph10):f2 ;========== 5th gradient pulse (echo). 5u p27:gp3 95u ;========== d4 pl2:f2 ; 13C power -> pl2. (p1*2.0 ph0):f1 d10 (p13*2.0 ph10):f2 ;========== 6th gradient pulse (echo). 5u p27:gp3 95u ;========== 4u d6 ;pl7:f1 (p24:sp2 ph10):f2 ; cancel Bloch-Siegert effect. ;========== 7th gradient pulse (echo). 5u p27:gp3 95u ;========== 4u d6 (p13 ph14):f2 4u p16:gp8 100u pl8:f2 ; 13C power -> pl8 for DIPSI-3. ;---------- 9 (p8*2.722 ph18):f2 ; start DIPSI-3y. (p8*4.389 ph19):f2 (p8*2.778 ph18):f2 (p8*3.056 ph19):f2 (p8*0.333 ph18):f2 (p8*2.556 ph19):f2 (p8*4.000 ph18):f2 (p8*2.722 ph19):f2 (p8*4.111 ph18):f2 (p8*3.778 ph19):f2 (p8*3.889 ph18):f2 (p8*2.889 ph19):f2 (p8*3.000 ph18):f2 (p8*0.333 ph19):f2 (p8*2.500 ph18):f2 (p8*4.050 ph19):f2 (p8*2.830 ph18):f2 (p8*4.389 ph19):f2 (p8*2.722 ph19):f2 (p8*4.389 ph18):f2 (p8*2.778 ph19):f2 (p8*3.056 ph18):f2 (p8*0.333 ph19):f2 (p8*2.556 ph18):f2 (p8*4.000 ph19):f2 (p8*2.722 ph18):f2 (p8*4.111 ph19):f2 (p8*3.778 ph18):f2 (p8*3.889 ph19):f2 (p8*2.889 ph18):f2 (p8*3.000 ph19):f2 (p8*0.333 ph18):f2 (p8*2.500 ph19):f2 (p8*4.050 ph18):f2 (p8*2.830 ph19):f2 (p8*4.389 ph18):f2 (p8*2.722 ph19):f2 (p8*4.389 ph18):f2 (p8*2.778 ph19):f2 (p8*3.056 ph18):f2 (p8*0.333 ph19):f2 (p8*2.556 ph18):f2 (p8*4.000 ph19):f2 (p8*2.722 ph18):f2 (p8*4.111 ph19):f2 (p8*3.778 ph18):f2 (p8*3.889 ph19):f2 (p8*2.889 ph18):f2 (p8*3.000 ph19):f2 (p8*0.333 ph18):f2 (p8*2.500 ph19):f2 (p8*4.050 ph18):f2 (p8*2.830 ph19):f2 (p8*4.389 ph18):f2 (p8*2.722 ph18):f2 (p8*4.389 ph19):f2 (p8*2.778 ph18):f2 (p8*3.056 ph19):f2 (p8*0.333 ph18):f2 (p8*2.556 ph19):f2 (p8*4.000 ph18):f2 (p8*2.722 ph19):f2 (p8*4.111 ph18):f2 (p8*3.778 ph19):f2 (p8*3.889 ph18):f2 (p8*2.889 ph19):f2 (p8*3.000 ph18):f2 (p8*0.333 ph19):f2 (p8*2.500 ph18):f2 (p8*4.050 ph19):f2 (p8*2.830 ph18):f2 (p8*4.389 ph19):f2 ; 4u lo to 9 times l1 ; Mixing time: p8*54.33*4*l1 ;========== 8th gradient pulse (echo). 5u p28:gp4 95u ;========== 200u (p1 ph0):f1 ;========== 9th gradient pulse (echo). 5u p29:gp5 95u ;========== 200u pl2:f2 ; 13C power -> pl2. (p13 ph12):f2 ;========== 10th gradient pulse (echo). 5u p26:gp6 95u ;========== d5 (d11 p1*2.0 ph0):f1 (p13*2.0 ph10):f2 ;========== 11th gradient pulse (echo). 5u p26:gp6 95u ;========== d5 (p13 ph10):f2 (p1 ph0):f1 ;========== 11th gradient pulse (echo). 5u p26:gp7 95u ;========== d3 (d11 p1*2.0 ph0):f1 (p13*2.0 ph10):f2 ;========== 10th gradient pulse (echo). 5u p26:gp7 95u ;========== d13 setnmr2^0 setnmr0^34^32^33 (p13 ph10 4u p13 ph13):f2 4u 20u pl12:f2 ; 13C power -> pl12. (p1 ph0):f1 ;---------- Acquisition. go=1 ph31 cpd2:f2 ;---------- Loop nest for States or States-TPPI. 50m do:f2 wr #0 if #0 zd 15m ip1 lo to 2 times 2 15m id0 15m ip31*2 lo to 3 times l3 15m rd0 15m ip11 lo to 4 times 2 15m id10 15m ip31*2 lo to 5 times l4 ;---------- 30m setnmr2^0 setnmr0^34^32^33 ; gradient-blanking on exit ;phase cycle. ;for 1H ph0=0 ph1=0 2 ph2=1 ph3=(360)0 ph4=(360)90 ;for 13C ph10=0 ph11=0 0 2 2 ph12=1 ph13=0 0 0 0 2 2 2 2 ph14=1 1 1 1 3 3 3 3 ph17=(360)0 ph18=(360)90 ph19=(360)270 ;for 15N ph20=0 ;for 1H presat ph29=0 ;for receiver ph31=0 2 2 0 2 0 0 2 ;for gradient ;p26:400u gp1,6,7 ;p27:100u gp3 ;p16:2.0m gp2,8 ;p28:7.0m gp4 ;p29:4.4m gp5 ;gpz1:25 ;gpz2:45 ;gpz3:25 ;gpz4:45 ;gpz5:45 ;gpz6:20 ;gpz7:25 ;gpz8:20