;chredorselndet.mh ;13C-H(N) REDOR with 15N detection ;Schmidt-Ror K, Hong M.J. Am. Chem. Soc., volume 125, 5648, 2003 ;p2: F3 180 REDOR ;p3: 1H excitation ;p8: 1H TPPM pulse ;p11: F1 90 saturate & z-filter, use PL11 ;p12: F1 180 pulse ;p15: LG-CP, short ;p21: 1H MREV-8 t90 ;p22: 1H REDOR 180, same power as for p21 ;d23: MREV-8 small window + t90, tc=12*d23 ;d20: F1 saturation window ;d6: 1H spin diffusion, unused ;d16: 1H z-filter & gamma integral, > tr/2 ;in16: gamma integral, tr/l5 ;l1: TPPM loop ;l3: =tr/tc*2-1, e.g 11 for tr/tc=6 ;l4: C-H REDOR No of tr ;l5: gamma loop ;l6: L6*d23 = soft 13C 180 ;l31: spinning speed in Hz ;pl1: 15N CP, const amplitude ;pl2: 1H excitation power ;pl3: 1H LG-CP, ca. 1.8dB > HHCP ;pl11: 15N TOSS, z-filter, saturation ;pl12: 1H TPPM dec for acq ;pl21: F3 REDOR power ;pl22: 1H MREV-8 power, calc for t90=3us ;pl23: 1H WIM power ;pl31: F3 soft inversion power define delay swi "swi=d23-p21" "p17=d23-p21" ;WIM pulse define delay lwi "lwi=d23+d23-p21" define delay swix ;at 13C 180 pulse "swix=lwi/2" define delay lwir "p5=p2-p21" ;1st part of 180 13C "lwir= d23+d23-p21-p2+p21" ;lwi-p5, rest of long window "d5=p5" define delay tr "tr=1s/l31" define loopcounter lredor "lredor=l4*2" "l17=68-l6" "l1=aq/(p8*2)" ;TPPM loops "p13=p3*353/900" ;35 degree pulse on 1H "d3=1s/l31-p12/2" 1 ze ;zero data tr ;just to calculate tr 2 d1 do:f2 ;recycle time, decoupler off 10u fq1:f2 ;1H on res 10u fq2:f3 ;F3 on res rpp17 rpp25 rpp24 ;WIM phase 10u pl11:f1 ;F1 saturation power p11:f1 ph9 d20 p11:f1 ph10 d20 p11:f1 ph9 d20 p11:f1 ph10 d20 3 10u pl21:f3 ;F3 REDOR power 10u pl2:f2 p3:f2 ph5 ;1H excitation 0.5u pl22:f2 ;high power for MREV8 ;------------------ 1st half of 1H-13C REDOR -------------------- 4 (p5 ph17):f3 ;F3 180 starts (p21 ph25^):f2 (p21 ph17):f3 swi ipp17 ;same as ^ p21:f2 ph25^ lwir ;rest of long window 5 d5 p21:f2 ph25^ swi p21:f2 ph25^ ;tc/4 lwir lo to 5 times l3 ;L3=(No MREV-8 per tr/2)*4 - 1 lo to 4 times lredor ;lredor = No tr for REDOR * 2 ;------------------------------------------------------------ ; 0.2u pl24:f2 (p22 ph19):f2 ;1H 180, middle of REDOR, at ntr=L4*tr ;------------------------------------------------------------ ;---------- WIM on 1H, soft 13C off-res 180 inversion------------- swi pl23:f2 (p21 ph24^):f2 ;WIM swi fq4:f3 ;F3 off res for inversion (p21 ph24^):f2 ;WIM swi pl31:f3 ;soft 13C 180 power 6 (p21 ph24^):f2 (p21 ph4):f3 ;soft 180, and WIM p17:f3 ph4 ;short "window" of WIM, soft 13C still on lo to 6 times l6 ;soft 13C 180 pulse=l6*d23=l6*(p21+p17) 7 (p21 ph24^):f2 ;WIM swi lo to 7 times l17 ;complete tr (p21 ph24^):f2 ;WIM swi fq2:f3 pl21:f3 ;F3 back on res (p21 ph24^):f2 ;WIM ;------------------ 2nd half of 1H-13C REDOR -------------------- 0.2u pl22:f2 8 lwir p21:f2 ph25^ swi p21:f2 ph25^ ;tc/4 d5 lo to 8 times l3 ;L3=(No MREV-8 per tr/2)*4 - 1 9 lwir p21:f2 ph25^ swi (p21 ph25^):f2 (p21 ph17):f3 ;F3 180 (p5 ph17^):f3 lo to 8 times lredor 0.5u pl2:f2 p3:f2 ph6 ;store 1H to z d6 pl1:f1 ;1H spin diffusion p3:f2 ph1 ;flip back to xy plane 10 p13:f2 ph3 ;1H: 35 +y pulse (- offset) 0.5u fq3:f2 1u pl3:f2 ;off res by cos(54.74)x w1 (p15 ph2):f1 (p15 ph11):f2 ;LG-CP 0.5u pl11:f1 p11:f1 ph7 ;store to z d16 do:f2 ;z-filter & gamma integral 5u fq1:f2 ;1H back on resonance 2u cw:f2 pl12:f2 p11:f1 ph8 ;read out d3 ;Hahn echo detect, avoid 0-freq artifact p12:f1 ph27 d3 2u:f1 ph0 ;dead time delay, reset RF phase to detect 1u adc ph31 ;start ADC with ph31 signal routing 18 p8:f2 ph13 ;TPPM decoupling p8:f2 ph14 lo to 18 times l1 1m do:f2 aq rcyc=2 ;do NS scans id16 ;inc by in16=tr/4: gamma-average for clean MAS lo to 2 times l5 ;1D: wr #0 exit ph0=0 ph9= +x ;destroy F1 magnetization ph10=+y ;destroy F1 magnetization ph5= +x +x +x +x +x +x +x +x ;1st 1H 90, excitation +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x +x ph6= -x -x -x -x -x -x -x -x ;2nd 1H 90, after REDOR, 1st z-filter 90 +x +x +x +x +x +x +x +x -x -x -x -x -x -x -x -x +x +x +x +x +x +x +x +x ph17=+x +y +x +y +y +x +y +x ;F3 REDOR 180 in C-H filter -x -y -x -y -y -x -y -x ph19= +y +y +y +y +y +y +y +y ;1H 180 (Hahn echo) middle REDOR -y -y -y -y -y -y -y -y ph25= -x +y -y +x +x +y -y -x ;1H MREV-8 phases ph27= +x +x +y +y -x -x -y -y ;F1 180 Hahn echo -x -x -y -y +x +x +y +y ph24= -y +x -y -y +x -y ;WIM-24 for complete decoupling +y +x +y +y +x +y -y -x -y -y -x -y +y -x +y +y -x +y ph4= +y -y -x +x -y +y +x -x ;F3 soft 180 ph1= +y -y ;3rd 1H 90, flip back after z-filter, before CP ph3= +y ;1H 35 onto tilted SL, - offset ph11= +x ;1H CP ph2= +x +x +y +y -x -x -y -y ;F1 CP ph7= +y +y -x -x -y -y +x +x ;F1 z-filter after CP ph8= -y -y +x +x +y +y -x -x ;F1 read out after z-filter ph13=(360) 0 ;TPPM1 ph14=(360) 10 ;TPPM2 ph31= 0 2 1 3 2 0 3 1 ;RLS 2 0 3 1 0 2 1 3 0 2 1 3 2 0 3 1 2 0 3 1 0 2 1 3 ;ns = 32