;hnch2ddfull.mh ;N-H doubled HNCH dipolar correlation to measure phi angle ;1H homonuclear decoupling sequence use cpds2 ;Hong M, Gross JD, Rienstra CM, Griffin RG, Kumashirro KK, Schmidt-Rohr K. ;J. Magn. Reson., volume 129, 85, 1997 ;p1: 13C 90 pulse ;p2: 13C 180 pulse ;p3: 1H excitation ;p8: TPPM 180 pulse length ;p11: 15N 90 pulse ;p12: 15N 180 pulse ;p15: contact time ;p31: 1H MREV-8 pulse ;d0: 15N evolution time ;d21: pulse centering ;pl1: 13C CP power ;pl2: 1H excitation power ;pl3: 1H CP power ;pl4: 15N hard power ;pl11: 13C hard power ;pl12: decoupling power for acq ;pl21: 1H cw dec. during REDOR ;pl22: homo. dec. power ;pl23: MREV-8 dec power ;l0: REDOR mixing time ;l1: TPPM decoupling time "d3=1s/l31-p1*0.5-p11-2u" ;z-filter "d21=(p11-p1)/2" ;pulse centering "d23=0.25s/l31-(p1/2)" ;beginning of REDOR reconvert. "d24=0.25s/l31-p11-2u" ;end of REDOR excitation "d25=0.25s/l31-1.5u" ;REDOR "d26=0.25s/l31-p12/2" ;REDOR delay between 15N pulses "d27=0.25s/l31-p2/2" ;REDOR delay sandwiching 13C pulses "d10=1s/l31+in0-p12/2-2u" ;NH evo. shrinking "d13=1s/l31+in0-p2/2-2u" ;CH evo. shrinking "d12=1s/l31-p2/2-p11-2u" ;CH, ~tr "l1=aq/(p8*2)" ;TPPM define delay dd35 define delay dd36 define delay dd37 define delay dd38 define delay dd39 "dd35=(1s/l31)*0.1226-(p2/2)" "dd36=(1s/l31)*0.0773-p2" "dd37=(1s/l31)*0.2236-p2" "dd38=(1s/l31)*1.0433-p2" "dd39=(1s/l31)*0.7744-(p2/2)-9u" 1 ze 10m dd10 10m dd13 2 d1 ;protect 10u pl1:f1 10u pl2:f2 ;set decoupler power,1H 10u pl4:f3 ;3rd nucleus power,often 15N 2u:f2 ph1 2u:f1 ph2 rpp5 ;reset phase lists for redor rpp7 p3:f2 ph1 ;90 degree proton pulse 0.5u pl3:f2 (p15 ph2):f1 (p15 ph3):f2 ;cross-polarization 1u cw:f2 pl21:f2 ;---------- 13C/15N DQ/ZQ excitation-------------------- d25 ;tr/4 3 d26:f3 ph5 p12:f3 ph5^ ;15N 180 deg. pulse d26 lo to 3 times l0 ;an odd number 0.5u pl11:f1 d27:f1 ph6 ;tr/4 p2:f1 ph6 ;13C 180 deg. pulse d27 4 d26:f3 ph5 p12:f3 ph5^ ;15N 180 deg. pulse d26 lo to 4 times l0 d24 ;-------------- C-H evolution ----------------------------------- 5 1u do:f2 1u cpds2:f2 pl22:f2 ;FSLG decoupling d0 ;d10=tr/2-2u-p2/2 1u do:f2 1u cw:f2 pl21:f2 ;TPPM d13:f1 ph8 ;decrease 6 p2:f1 ph8 ;13C 180 pulse,refocus iso. shift 7 d12:f1 ph9 ;tr ;-------------- N-H x 2 evolution --------------------------------- (d21 p1 d21 ph9):f1 (p11 ph10):f3 ;simultaneous 90 pulses 8 1u do:f2 ;NH 1st tr, 1H homo dec 1u cpds2:f2 pl22:f2 d0:f3 ph8 ;increase p12:f3 ph8 ;15N 180 pulse ; 1u ;still FSLG d10 ;decrease 9 1u do:f2 ;NH 2nd tr, TPPM 1u cw:f2 pl21:f2 ;TPPM d0:f3 ph12 ;increase p12:f3 ph12 ;15N 180 pulse ; 1u d10:f3 ph4 ;decrease ;-------------- z-filter ---------------------------------------- p11:f3 ph4 ;15N 90 d3 do:f2 ;z-filter 1u:f1 ph10 1u cw:f2 pl21:f2 p1:f1 ph10 ;13C 90 ;-------------- 15N-13C REDOR ---------------------------------------- d23 ;tr/4 11 d26:f3 ph7 p12:f3 ph7^ ;15N 180 deg. pulse d26 lo to 11 times l0 ;an odd number d27:f1 ph8 ;tr/4 p2:f1 ph8 ;13C refocus d27 12 d26:f3 ph7 p12:f3 ph7^ ;15N 180 deg. pulse d26 lo to 12 times l0 d25 ;------------ TOSS, not mandatory -------------------------------- dd35:f1 ph23 p2:f1 ph23 ;180 13C #1 dd36:f1 ph24 p2:f1 ph24 ;180 13C #2 dd37:f1 ph25 p2:f1 ph25 ;180 13C #3 dd38:f1 ph26 p2:f1 ph26 ;180 13C #4 dd39 ;-------- detection -------------------------------- 0.5u do:f2 0.5u cw:f2 1u pl12:f2 1u:f1 ph0 ;dead time delay, reset RF phase to detect 1u adc ph31 ;start ADC with ph31 signal routing 13 p8:f2 ph13 p8:f2 ph14 lo to 13 times l1 aq do:f2 ;allow time for data sampling rcyc=2 ;do NS scans ;2D torsion angle 100m wr #0 if #0 zd 1m id0 lo to 1 times td1 exit ph0= 0 ph1= +x -x ;1H excitation ph2= +x +x +y +y -x -x -y -y ;13C CP ph3= +y ;1H CP ph5= +x +y +x +y +y +x +y +x ;15N REDOR pulses -x -y -x -y -y -x -y -x ph6= +x +x +y +y -x -x -y -y ph7= +x +y +x +y +y +x +y +x ;15N REDOR -x -y -x -y -y -x -y -x ph8= +y -y -x +x -y +y +x -x ;15N 180 for doubling ph12=-y +y +x -x +y -y -x +x ;15N 180 for doubling ph9= +x +x +y +y -x -x -y -y ;13C mix ph10= +x +x +y +y -x -x -y -y ;15N read-in ph11= -x -x -y -y +x +x +y +y ;13C flip back ph4= +x -x +y -y -x +x -y +y ;15N read-out -x +x -y +y +x -x +y -y ph13= (360) 10 ph14= (360) 0 ph23= +x -x +y -y -x +x -y +y ;180 13C #1 ph24= -x +x -y +y +x -x +y -y ;180 13C #2 ph25= +x -x +y -y -x +x -y +y ;180 13C #3 +x -x +y -y -x +x -y +y -x +x -y +y +x -x +y -y -x +x -y +y +x -x +y -y ph26= +y -y +x -x -y +y -x +x ;180 13C #4 +y -y +x -x -y +y -x +x -y +y -x +x +y -y +x -x -y +y -x +x +y -y +x -x ph31= 0 0 1 1 2 2 3 3 2 2 3 3 0 0 1 1