;5.3) Program: SUPER (Separation of Undistorted Powderpatterns by Effortless Recoupling) ;Description: Separation of regular chemical-shift anisotropy powder patterns ;of dilute spins (13C, 29Si) with 0.155 scaling factor ;Requires: !!!; 2.5 – 4 kHz MAS, 13C w1 = 12.12 wr, 1H w1 = 30 wr. ;Reference(s): Liu, Mao, & KSR, J. Magn. Reson. 155, 15-28 (2002). ;sr2dcsatoss.tppm (SUPER) ;recoupling of CSA by 2*360 pulses per tr/2 ;choose correct d21 calculation for ;common solutions: ; pulse from 0.2464 to 0.4114 tr (33 us duration at 5 kHz) scalfac=0.15 ; 13C: w1 = gamma B1 = 12.12 wrot, p22 = (1/12.12wrot) / 2 ; 1H: w1 = gamma B1 > 25 wrot ; pulse from 0.197 to 0.447 tr (tr/4 duration) scalfac = 0.19 does not work well ;gamma-integral before TOSS by l5-loop (set l5 = # of sidebands, 4 typically) ;TOtal Sideband Suppression (TOSS) using four 180 13C pulses ;durations between 180 pulses (d25-d29) are calculated from l31 (=SS in Hz) ;pl2 is power level for contact, pl12 is power level for decoupling on F2 ; set in6 to tr/l5 (e.g. tr/4), where l5 is the loop counter for the gamma integral define loopcounter td1half "td1half=td1/2" ;for States cosine/sine "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)-d13" "l20=aq/(p8*2)" ;loop for tppm dec 1 ze 10u pl1:f1 ;preselect pl1 drive power level for F1 2 d1 do:f2 ;recycle delay, turn the decoupler off rpp12 ; reset ph12 rpp13 rpp14 rpp15 rpp16 rpp17 rpp18 rpp19 10u pl2:f2 ;preselect pl2 drive power for F2 10u pl1:f1 ;preselect pl1 drive power level for F1 1u:f2 ph1 1u:f1 ph2 p3:f2 ph1 ;proton 90 pulse d19 ;allow time for the phase shift on F2 (p15 ph2):f1 (p15 ph10):f2 ;contact pulse 1u cw:f2 pl22:f2 ;turn on F2 decoupling 9 d21 pl21:f1 1u pl23:f2 ;increase 1H power during 13C pulses p22:f1 ph12^ ;180 pulse at pl21 p22:f1 ph13^ ;180 pulse p22:f1 ph14^ ;180 pulse p22:f1 ph15^ ;180 pulse 1u pl22:f2 d22 d22 1u pl23:f2 p22:f1 ph16^ ;180 pulse p22:f1 ph17^ ;180 pulse p22:f1 ph18^ ;180 pulse p22:f1 ph19^ ;180 pulse 1u pl22:f2 d21 pl11:f1 ;finish 1 tr lo to 9 times l4 p1:f1 ph7 ;store for z-filter d6 do:f2 ;z-filter & gamma integral 1u cpds2:f2 ;turn on F2 decoupling 1u pl12:f2 ;set decoupling drive power level p1:f1 ph8 ;read out d25 ; p2:f1 ph3 ;180 13C #1 d26 ; p2:f1 ph4 ;180 13C #2 d27 ; p2:f1 ph5 ;180 13C #3 d28 ; p2:f1 ph6 ;180 13C #4 d29 pl12:f2 ; 2u:f1 ph0 ;dead time delay, reset RF phase to detect go=2 ph31 1m do:f2 id6 ;increment d6: gamma-average for clean TOSS lo to 2 times l5 ;1D ; wr #0 14 dd6 ;decrement d6 again lo to 14 times l5 ;2D 100m wr #0 if #0 zd ;write and increment file ip7 ;alternate sine & cosine (same t1) lo to 2 times 2 iu4 ;increment l4 (t1) ip7 ;skip -cosine ip7 ;skip -sine lo to 2 times td1half ;number of rows exit ph0= 0 ;reference phase ph1= 1 3 ;1H 90 ph2= 0 0 1 1 2 2 3 3 ;13C CP ph3= 1 1 2 2 3 3 0 0 ;180 13C #1 TOSS ph4= 3 3 0 0 1 1 2 2 ;180 13C #2 ph5= 1 1 2 2 3 3 0 0 ;180 13C #3 3 3 0 0 1 1 2 2 ph6= 2 2 1 1 0 0 3 3 ;180 13C #4 0 0 3 3 2 2 1 1 ph7= 1 1 2 2 3 3 0 0 ;store for z-filter after t1 ph8= 3 3 0 0 1 1 2 2 ;read out after z-filter ph10= 0 ;1H CP ph12= 0 2 1 3 2 0 3 1 0 0 1 1 2 2 3 3 ;180's for 4*180 "spin-lock" pulses 2 1 2 3 0 3 0 1 0 1 2 1 2 3 0 3 3 2 1 2 3 0 3 0 1 0 1 2 1 2 3 0 ;last of previous shifted to first 3 0 2 1 3 2 0 3 1 0 0 1 1 2 2 3 ;first line shifted by one ph13= 0 0 1 1 2 2 3 3 0 2 1 3 2 0 3 1 0 1 2 1 2 3 0 3 2 1 2 3 0 3 0 1 1 0 1 2 1 2 3 0 3 2 1 2 3 0 3 0 1 0 0 1 1 2 2 3 3 0 2 1 3 2 0 3 ph14= 2 0 3 1 0 2 1 3 2 2 3 3 0 0 1 1 0 3 0 1 2 1 2 3 2 3 0 3 0 1 2 1 1 0 3 0 1 2 1 2 3 2 3 0 3 0 1 2 1 2 0 3 1 0 2 1 3 2 2 3 3 0 0 1 ph15= 2 2 3 3 0 0 1 1 2 0 3 1 0 2 1 3 2 3 0 3 0 1 2 1 0 3 0 1 2 1 2 3 3 2 3 0 3 0 1 2 1 0 3 0 1 2 1 2 3 2 2 3 3 0 0 1 1 2 0 3 1 0 2 1 ph16= 2 0 3 1 0 2 1 3 2 2 3 3 0 0 1 1 ;= ph14 = -ph12 0 3 0 1 2 1 2 3 2 3 0 3 0 1 2 1 1 0 3 0 1 2 1 2 3 2 3 0 3 0 1 2 1 2 0 3 1 0 2 1 3 2 2 3 3 0 0 1 ph17= 2 2 3 3 0 0 1 1 2 0 3 1 0 2 1 3 ;= ph15 = -ph13 2 3 0 3 0 1 2 1 0 3 0 1 2 1 2 3 3 2 3 0 3 0 1 2 1 0 3 0 1 2 1 2 3 2 2 3 3 0 0 1 1 2 0 3 1 0 2 1 ph18= 0 2 1 3 2 0 3 1 0 0 1 1 2 2 3 3 ;= ph12 = - ph14 2 1 2 3 0 3 0 1 0 1 2 1 2 3 0 3 3 2 1 2 3 0 3 0 1 0 1 2 1 2 3 0 3 0 2 1 3 2 0 3 1 0 0 1 1 2 2 3 ph19= 0 0 1 1 2 2 3 3 0 2 1 3 2 0 3 1 ;= ph13 = -ph15 0 1 2 1 2 3 0 3 2 1 2 3 0 3 0 1 1 0 1 2 1 2 3 0 3 2 1 2 3 0 3 0 1 0 0 1 1 2 2 3 3 0 2 1 3 2 0 3 ph20= (360) 10 ;TPPM first pulse ph21= (360) 0 ;TPPM second pulse ph31= 0 2 1 3 2 0 3 1 ;RLS