;3.4) Program: CHHC with MAD (Multiple Alternating Depolarization) ;Description: 2D 13C-13C NMR with cross peaks due to 1H spin diffusion ;Requires: !!; long measuring times at long mixing times (2% effic.) ;Reference(s): Hou, Chen, & KSR, Macromolecules 37, 1999-2001 (2004). ;srcp2dMAD.mulech (XWinNMR 2.6) ;from srcp2dMAD.toss, srmulech.plswitch and srmulech.to ;from srcp2dMAD.tppm ;from srcpecho.tppm ;from srcpecho.ksr ;pl2 is power level for contact, pl12 is power level for decoupling on F2 "l20=aq/(p8*2)" ;loop for tppm decoupling define loopcounter td1half "td1half=td1/2" ;for States cosine/sine "d21=l2*(1s/l31)-p2/2-d3-12u" "d22=l2*(1s/l31)-p2/2-d3-d13-3u" "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" 1 ze 2 d1 ;recycle delay 10u pl2:f2 ;preselect pl2 drive power for F2 10u pl11:f1 ;preselect pl11 drive power level for F1 1u:f2 ph1 1u:f1 ph2 p3:f2 ph1 ;proton 90 pulse d19:f2 ph10 ;ca. 1u: allow time for the phase shift on F2 (p24 ph3):f1 (p24 ph2):f2 ;preparation contact pulse, ca. 200 us (p4 ph2):f2 ;t1 evolution of 13C magnetization (p25 ph4):f1 (p25 ph2):f2 ;contact pulse, may alternate on 13C (p4 ph2):f2 ;t1 evolution of 13C magnetization (p25 ph5):f1 (p25 ph2):f2 ;contact pulse, ca. 400 us (p4 ph2):f2 ;t1 evolution of 13C magnetization (p25 ph6):f1 (p25 ph2):f2 ;contact pulse, may alternate on 13C 3 (p4 ph2):f2 ;t1 evolution of 13C magnetization (p25 ph3):f1 (p25 ph2):f2 ;contact pulse, ca. 400 us (p4 ph2):f2 ;t1 evolution of 13C magnetization (p25 ph4):f1 (p25 ph2):f2 ;contact pulse, may alternate on 13C (p4 ph2):f2 ;t1 evolution of 13C magnetization (p25 ph5):f1 (p25 ph2):f2 ;contact pulse, ca. 400 us (p4 ph2):f2 ;t1 evolution of 13C magnetization (p25 ph6):f1 (p25 ph2):f2 ;contact pulse, may alternate on 13C lo to 3 times l4 ;................................................................. p3:f2 ph8 d6 pl1:f1 ;spin diffusion between phases p3:f2 ph9 ;................................................................. (p15 ph12):f1 (p15 ph10):f2 ;contact pulse ;----------------------------------------------------------------- p1:f1 ph17 ;store for z-filter d16 ;z-filter & gamma integral 1u cw:f2 ;turn on F2 decoupling 1u pl12:f2 ;set decoupling drive power level p1:f1 ph18 ;read out ;----------------------------------------------------------------- d25 ; 3u pl23:f2 p2:f1 ph23 ;180 13C #1 d26 ; p2:f1 ph24 ;180 13C #2 3u pl12:f2 d27 ; 3u pl23:f2 p2:f1 ph25 ;180 13C #3 3u pl12:f2 d28 ; 3u pl23:f2 p2:f1 ph26 ;180 13C #4 3u pl12:f2 d29 ; 8u:f1 ph0 ;dead time delay, reset RF phase to detect 1u adc ph31 ;start ADC with ph31 signal routing d21 d13 3u pl23:f2 d3:e (p2 ph13):f1:e ;1st 180 on tr in detection d3:e d13:e 3u pl12:f2 d22 :e 10 d22 :e d13 :e 3u pl23:f2 d3:e (p2 ph13):f1:e ;more 180s for Hahn echoes in detection d3:e d13:e 3u pl12:f2 d22 d22 d13 3u pl23:f2 d3:e (p2 ph14):f1:e ;more 180s for Hahn echoes in detection d3:e d13:e 3u pl12:f2 d22 :e d22 :e d13 :e 3u pl23:f2 d3:e (p2 ph14):f1:e ;more 180s for Hahn echoes in detection d3:e d13:e 3u pl12:f2 d22 d22 d13 3u pl23:f2 d3:e (p2 ph13):f1:e ;more 180s for Hahn echoes in detection d3:e d13:e 3u pl12:f2 d22 :e lo to 10 times l3 20u do:f2 ;turn decoupler off rcyc=2 ;do NS scans id16 ;increment d6 by in6=tr/l5: gamma-average for clean TOSS lo to 2 times l5 ;1D ; wr #0 14 dd16 ;decrement d6 again lo to 14 times l5 ;2D 100m wr #0 if #0 zd ;write file to disk, increment, zero data ip4 ;x -> y for sine (same t1) ip5 ; ip5 ;x -> -x ip6 ip6 ip6 ;x -> -y lo to 2 times 2 10m ipu4 ;increments p4 by inp4 ip4 ;skip -cosine ip4 ;skip -sine ;;;;; ip5 has been reset by 2*2 90 shifts ip6 ip6 lo to 2 times td1half ;number of rows exit ph0= 0 ph1= +y +y -y -y ;First 1H 90 ph2= +x ;1H spin lock in evolution ph3= +x ;13C spin lock in evolution ph4= -x +x ;alternating 13C spin lock in evolution ph5= +x ;13C spin lock in evolution ph6= -x +x ;alternating 13C spin lock in evolution ph8= +y +y +y +y +y +y +y +y ;store for 1H spin diffusion -y -y -y -y -y -y -y -y ph9= +x ;read out from 1H spin diffusion ph10= +y ;1H CP ph12= +x +x +y +y -x -x -y -y ;13C CP ph13= +x +x +y +y -x -x -y -y ;180 in detect (best phase for on-resonance) ph14= -x -x -y -y +x +x +y +y ;180 in detect (best phase for on-resonance) ph17= +y +y -x -x -y -y +x +x ;store for z-filter after CP ph18= -y -y +x +x +y +y -x -x ;read out after z-filter ph20= (360) 10 ;TPPM first pulse ph21= (360) 0 ;TPPM second pulse ph23= +y +y -x -x -y -y +x +x ;180 13C #1 TOSS ph24= -y -y +x +x +y +y -x -x ;180 13C #2 ph25= +y +y -x -x -y -y +x +x ;180 13C #3 -y -y +x +x +y +y -x -x ph26= -x -x +y +y +x +x -y -y ;180 13C #4 +x +x -y -y -x -x +y +y ph31= 0 2 3 1 2 0 1 3 ;RCPH 2 0 1 3 0 2 3 1