;1.4) Program: Dipolar DEPT for CH-only spectra ;Description: Selects CH (methyne) signals ;Requires: !!!! first set-up; !! run routinely (ca. 15% effic.). Higher power during 2.16 ;tr = 540 us; 4 kHz MAS ;Reference(s): KSR & Mao, J. Am. Chem. Soc. 124, 13938-13948 (2002). ;Applied in: Mao et al., Environ. Sci. Technol. 37, 1751-1757 (2003). ;srcpchsel.4kHz (in spite of name, no CP in this pulse sequence) ;from srcpchsel18.mrev ;use at 4 kHz with p11 = 3.45u and p13 = 3.15u ; MREV TEDOR with tr/6 of MQ excitation, -1/2 tr CH2 suppression ;preceded by trot on 1H for isotropic shift prefocusing ;select CH (spectral editing) by ;different MQ dipolar dephasing of CH and CH2 ;MREV decoupling ;TOSS before detection ;define delay d13rest define delay trot define delay ad3 "d8=p11" ;MREV-8 window "d9=d8/2" "d3=p11*22+p1+p2/2" ; "ad3=p11*46+p2/2+p13" ; ;delays for TOSS with power level switch "d25=(1s/l31)*0.1226-(p2/2)-2u-3u" "d26=(1s/l31)*0.0773-p2" ;too short for power level switch "d27=(1s/l31)*0.2236-p2-6u" "d28=(1s/l31)*1.0433-p2-6u" "d29=(1s/l31)*0.7744-(p2/2)-3u-d13-d14-1u" "l20=aq/(p8*2)" ;loop for tppm decoupling 1 ze 10u ; trot 2 d1 do:f2 ;recycle delay 10u pl11:f1 ;preselect pl1 drive power level for F1 10u pl22:f2 ;preselect pl22 drive power for F2 1u:f2 ph1 1u:f1 ph2 p1:f1 ph18 ;destroy 13C magnetization d20 p1:f1 ph19 d20 p13:f2 ph1 ;+-x 1H excitation to Iy, generates IxzSz 3 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x d8 lo to 3 times 5 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x ;----------------------------------------------------------- p12:f2 ph11 ;+y 1H 180 (tr ) refocuses isotropic shift ;d8 ;mrev-8 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x ;............................................................. p1:f1 ph2 ;+x 13C pulse to start MQ evolution ;tr/6 ; d8 ;MQ evolution p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x ;tr/3 ; d8 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x ;tr/2 p2:f1 ph3 ;13C 180 pulse (tr'/2, center of 13C) ; d8 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x d8 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x d8 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x p13:f2 ph7 ;+-y 1H pulse to end MQ evolution, rotate Ixz onto Beff ;----------------------------------------------------------- ; 1 tr of 1H ; d8 p11:f2 ph22 ;-x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph20 ;x d8 p11:f2 ph20 ;x p11:f2 ph21 ;y d8 p11:f2 ph23 ;-y p11:f2 ph22 ;-x ;............................................................. d3 cpds2:f2 pl12:f2 ;use tppm.mh as cpdprg1(ased) p2:f1 ph4 ;180 on 13C for Hahn echo ad3 ;Hahn echo tau, turn on F2 decoupling p1:f1 ph12 ;Z-filter 2u do:f2 d6 1u cw:f2 pl12:f2 p1:f1 ph13 d25 ; 3u pl22:f2 p2:f1 ph27 ;180 13C #1 d26 ; p2:f1 ph24 ;180 13C #2 3u pl12:f2 d27 ; 3u pl22:f2 p2:f1 ph25 ;180 13C #3 3u pl12:f2 d28 ; 3u pl22:f2 p2:f1 ph26 ;180 13C #4 3u pl12:f2 d29 ; d14 do:f2 1u cpds2:f2 pl12:f2 2u:f1 ph0 ;dead time delay, reset RF phase to detect go=2 ph31 ;do NS scans 1m do:f2 ;turn decoupler off wr #0 exit ph0= 0 ph1= 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ;1H 90 ph2= 0 0 1 1 2 2 3 3 ;13C 90 for transfer ph3= 0 ;13C 180 pulse 1 ph4= 2 ;13C 180 pulse 2 ph5= 1 ph6= 1 ;1H 90 before MQ (not applied) ph7= 3 1 ;1H 90 after MQ ph8= 1 1 2 2 3 3 0 0 ph9= 3 3 0 0 1 1 2 2 ph11= 1 ;1H 180 ph12=1 1 2 2 3 3 0 0 ;Z-filter 1st 90 1 1 2 2 3 3 0 0 3 3 0 0 1 1 2 2 3 3 0 0 1 1 2 2 ph13=3 3 0 0 1 1 2 2 ;Z-filter 2nd 90 ph15= (360) 10 ;TPPM first pulse ph16= (360) 0 ;TPPM second pulse ph18= 0 ;destroy 13C magnetization ph19= 1 ;destroy 13C magnetization ph20=0 ;MREV-8 ph21=1 ph22=2 ph23=3 ph27= 1 1 2 2 3 3 0 0 ;180 13C #1 TOSS ph24= 3 3 0 0 1 1 2 2 ;180 13C #2 ph25= 1 1 2 2 3 3 0 0 ;180 13C #3 3 3 0 0 1 1 2 2 ph26= 2 2 1 1 0 0 3 3 ;180 13C #4 0 0 3 3 2 2 1 1 ph31= 0 2 1 3 2 0 3 1 ;RCPH 2 0 3 1 0 2 1 3 2 0 3 1 0 2 1 3 0 2 1 3 2 0 3 1