;cnmodcsa.mh ;CSA recoupling using SUPER ;use recoupled 13C-15N dipolar coupling to modulate CSA ;Yao XL, Hong M. J. Am. Chem. Soc., volume 124, 2730, 2002 ;p1: 13C 90 pulse ;p3: 1H excitation ;p2: 13C hard 180 pulse ;p4: 15N 180 composite ;p5: 15N 90 composite ;p22: 15N and 13C SUPER rec. =(1/2*12.12wr) ;d3: z-filter for dipolar cosine mod. ;d6: TOSS, gamma integral ;d12: centering delay between 13C and 15N ;l2: C-N modulation, 2(L2+1)*tr ;l4: t1 loop for CSA ;l5: gamma integral, 2 or 4 ;in6: tr/l5 ;pl1: 13C CP power ;pl2: 1H excitation power ;pl3: 1H CP ;pl4: 15N hard power ;pl14: 15N recoupling power ;pl15: 15N CW dec. ;pl11: 13C hard pulse power ;pl21: 13C recoupling power=12.12 wr ;pl22: 1H dec. outside 13C recp. ;pl23: 1H dec. during 13C rec. define loopcounter td1half "td1half=td1/2" ;for States cosine/sine "d3=1s/l31-p1*2-17u" "d11=(1s/l31)*0.2464-1u-p4/2-p5" ;start position of 4*180 pulse "d12=(p4+2*p5-p2)/2" ;centering delay "d21=(1s/l31)*0.2464-1u" ;start position of 4*180 pulse "d22=(0.5s/l31)-4*p22-d21-2u" ;rest of tr/2 in CSA recoupling "d25=(1s/l31)*0.1226-(p2/2)" "d26=(1s/l31)*0.0773-p2" "d27=(1s/l31)*0.2236-p2" "d28=(1s/l31)*1.0433-p2" "d29=(1s/l31)*0.7744-(p2/2)" "l20=aq/(p8*2)" ;loop for tppm dec 1 ze 2 d1 do:f2 rpp12 rpp13 rpp14 rpp15 rpp16 rpp17 rpp18 rpp19 10u pl1:f1 10u pl2:f2 10u pl14:f3 1u:f2 ph1 1u:f1 ph2 3 p3:f2 ph1 0.5u pl3:f2 (p15 ph2):f1 (p15 ph10):f2 ;CP contact 1u cw:f2 pl22:f2 pl11:f1 ;------------- 13C-15N recoupling ------------------ 5 d21 1u pl23:f2 ;higher 1H power during 15N pulses p22:f3 ph12^ ;180 pulse p22:f3 ph13^ p22:f3 ph14^ p22:f3 ph15^ 1u pl22:f2 d22 d22 1u pl23:f2 p22:f3 ph16^ ;180 pulse p22:f3 ph17^ p22:f3 ph18^ p22:f3 ph19^ 1u pl22:f2 d21 lo to 5 times l2 6 d21 1u pl23:f2 ;higher 1H power during 15N pulses p22:f3 ph12^ ;180 pulse p22:f3 ph13^ p22:f3 ph14^ p22:f3 ph15^ 1u pl22:f2 d22 d22 1u pl23:f2 p22:f3 ph16^ ;180 pulse p22:f3 ph17^ p22:f3 ph18^ p22:f3 ph19^ 1u pl22:f2 d11 pl4:f3 ;leave time for 13C, 15N 180 pulses ; recouple C-N, composite 15N pulse (d12 p2 ph22 d12):f1 (p5 ph28 p4 ph29 p5 ph28):f3 7 d11 pl14:f3 ;15N soft pulse power 1u pl23:f2 p22:f3 ph12^ p22:f3 ph13^ p22:f3 ph14^ p22:f3 ph15^ 1u pl22:f2 d22 d22 1u pl23:f2 p22:f3 ph16^ p22:f3 ph17^ p22:f3 ph18^ p22:f3 ph19^ 1u pl22:f2 d21 8 d21 1u pl23:f2 p22:f3 ph12^ p22:f3 ph13^ p22:f3 ph14^ p22:f3 ph15^ 1u pl22:f2 d22 d22 1u pl23:f2 p22:f3 ph16^ p22:f3 ph17^ p22:f3 ph18^ p22:f3 ph19^ 1u pl22:f2 d21 lo to 8 times l2 ;------------ z-filter, select only cosine comp. ----------- 9 p1:f1 ph7 d3 do:f2 2u rpp12 ;reset SUPER phases for 13C 2u rpp13 2u rpp14 2u rpp15 2u rpp16 2u rpp17 2u rpp18 2u rpp19 1u cw:f2 pl12:f2 p1:f1 ph8 ;---------- 13C CSA evolution t1 ------------------------- 1u cw:f3 pl15:f3 ;turn on 15N decoupling 15 d21 pl21:f1 1u pl23:f2 ;higher 1H power during 13C pulses p22:f1 ph12^ p22:f1 ph13^ p22:f1 ph14^ p22:f1 ph15^ 1u pl22:f2 d22 d22 1u pl23:f2 p22:f1 ph16^ p22:f1 ph17^ p22:f1 ph18^ p22:f1 ph19^ 1u pl22:f2 d21 pl11:f1 lo to 15 times l4 ;t1 16 p1:f1 ph9 ;z-filter, cosine and sine 1u do:f3 d6 do:f2 ;gamma integral 1u cw:f2 pl12:f2 p1:f1 ph11 18 d25 ;TOSS p2:f1 ph3 d26 p2:f1 ph4 d27 p2:f1 ph5 d28 p2:f1 ph6 d29 pl12:f2 2u:f1 ph0 ;dead time, reset RF phase 1u adc ph31 ;start ADC with ph31 23 p8:f2 ph20 ;TPPM dec. < 180 p8:f2 ph21 lo to 23 times l20 aq do:f2 rcyc=2 ;do NS scans id6 ;increment d6, clean TOSS lo to 2 times l5 34 dd6 ;decrement d6 again lo to 34 times l5 ;2D 38 100m wr #0 if #0 zd ;write and increment file ip9 lo to 2 times 2 iu4 ;increment l4 (t1) ip9 ip9 lo to 2 times td1half exit ph0= 0 ;reference phase ph1= +y +y +y +y +y +y +y +y ;1H 90 +y +y +y +y +y +y +y +y -y -y -y -y -y -y -y -y -y -y -y -y -y -y -y -y ph10= +x ;1H CP ph2= +x +x +y +y -x -x -y -y ;13C CP ph7= +y +y -x -x -y -y +x +x ;post-dipolar z-filter ph8= -y -y +x +x +y +y -x -x ;post-dipolar z-filter ph9= +y +y -x -x -y -y +x +x ;post CSA z-filter ph11= -y -y +x +x +y +y -x -x ;post CSA z-filter ph22= +x +y +y +x ;13C 180 exorcycle ph28= +y +y -x -x -y -y +x +x ;15N 90 in composite 180 pulse ph29= +x +x +y +y -x -x -y -y ;15N 180 pulse ph31= 0 2 1 3 2 0 3 1 ;receiver 0 2 1 3 2 0 3 1 2 0 3 1 0 2 1 3 ;for 1H inversion 2 0 3 1 0 2 1 3 ph3= +y +y -x -x -y -y +x +x ;180 13C #1 TOSS ph4= -y -y +x +x +y +y -x -x ;180 13C #2 ph5= +y +y -x -x -y -y +x +x ;180 13C #3 -y -y +x +x +y +y -x -x ph6= -x -x +y +y +x +x -y -y ;180 13C #4 +x +x -y -y -x -x +y +y ph20= (360) 10 ;TPPM first pulse ph21= (360) 0 ;TPPM second pulse ph12= +x -x +y -y -x +x -y +y +x +x +y +y -x -x -y -y ;180's for 4*180 "spin-lock" pulses -x +y -x -y +x -y +x +y +x +y -x +y -x -y +x -y -y -x +y -x -y +x -y +x +y +x +y -x +y -x -y +x ;last of previous shifted to first -y +x -x +y -y -x +x -y +y +x +x +y +y -x -x -y ;first line shifted by one ph13= +x +x +y +y -x -x -y -y +x -x +y -y -x +x -y +y +x +y -x +y -x -y +x -y -x +y -x -y +x -y +x +y +y +x +y -x +y -x -y +x -y -x +y -x -y +x -y +x +y +x +x +y +y -x -x -y -y +x -x +y -y -x +x -y ph14= -x +x -y +y +x -x +y -y -x -x -y -y +x +x +y +y +x -y +x +y -x +y -x -y -x -y +x -y +x +y -x +y +y +x -y +x +y -x +y -x -y -x -y +x -y +x +y -x +y -x +x -y +y +x -x +y -y -x -x -y -y +x +x +y ph15= -x -x -y -y +x +x +y +y -x +x -y +y +x -x +y -y -x -y +x -y +x +y -x +y +x -y +x +y -x +y -x -y -y -x -y +x -y +x +y -x +y +x -y +x +y -x +y -x -y -x -x -y -y +x +x +y +y -x +x -y +y +x -x +y ph16= -x +x -y +y +x -x +y -y -x -x -y -y +x +x +y +y ;= ph14 = -ph12 +x -y +x +y -x +y -x -y -x -y +x -y +x +y -x +y +y +x -y +x +y -x +y -x -y -x -y +x -y +x +y -x +y -x +x -y +y +x -x +y -y -x -x -y -y +x +x +y ph17= -x -x -y -y +x +x +y +y -x +x -y +y +x -x +y -y ;= ph15 = -ph13 -x -y +x -y +x +y -x +y +x -y +x +y -x +y -x -y -y -x -y +x -y +x +y -x +y +x -y +x +y -x +y -x -y -x -x -y -y +x +x +y +y -x +x -y +y +x -x +y ph18= +x -x +y -y -x +x -y +y +x +x +y +y -x -x -y -y ;= ph12 = - ph14 -x +y -x -y +x -y +x +y +x +y -x +y -x -y +x -y -y -x +y -x -y +x -y +x +y +x +y -x +y -x -y +x -y +x -x +y -y -x +x -y +y +x +x +y +y -x -x -y ph19= +x +x +y +y -x -x -y -y +x -x +y -y -x +x -y +y ;= ph13 = -ph15 +x +y -x +y -x -y +x -y -x +y -x -y +x -y +x +y +y +x +y -x +y -x -y +x -y -x +y -x -y +x -y +x +y +x +x +y +y -x -x -y -y +x -x +y -y -x +x -y