;1.8) Program: CSA filter ;Description: Selects alkyl (i.e. sp3-hybridized) C, e.g. O-C-O (which overlap with aromatic ;C) by three- or five-pulse CSA dephasing ;Requires: !; ca. 5 kHz MAS; short CP for O-CH-O selection; long CP & gated decoupling for ;O-Cq-O selection ;Reference(s): Mao & KSR, Solid State NMR 26, 36-45 (2004); compare SUPER sequence (5.3) for ;measurement of all three CSA principal values ;srcsafilsp2A.cpd ;from srcsafilsp2A.deph on SGI ;type "eda", set "CPDPRG2" to "tppm15", set p30=p31=9u (180 on 1H at pl12) ;2 tr duration ;recoupling of CSA by 3 180 pulses ;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 "d22=(1s/l31)-d21-p2-p2/2-3u" ; tr-tau in CSA recoupling ;add -p2/2 Dec.01 "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" 1 ze 10u pl1:f1 ;preselect pl1 drive power level for F1 2 d1 do:f2 ;recycle delay, turn the decoupler off 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 (p15 ph2):f1 (p15 ph10):f2 ;contact pulse 1u cw:f2 pl22:f2 ;turn on F2 decoupling 9 d21 pl11:f1 ;tau of CSA dephasing (max. dephasing if d21 = tr/2) p2:f1 ph12 ;180 pulse at tau 1u pl12:f2 d22 ;finish 1 tr 1u pl22:f2 ;off (120 dB) or double 13C B1 p2:f1 ph13 ;180 pulse at tr 1u pl12:f2 d22 ; 1u pl22:f2 p2:f1 ph14 ;180 pulse at 2tr - tau d21 p1:f1 ph7 ;store for z-filter d6 do:f2 ;z-filter & gamma integral 1u cw:f2 ;turn on F2 decoupling 1u pl12:f2 ;set decoupling drive power level p1:f1 ph8 ;read out d25 ; 3u pl22:f2 p2:f1 ph3 ;180 13C #1 d26 ; p2:f1 ph4 ;180 13C #2 3u pl12:f2 d27 ; 3u pl22:f2 p2:f1 ph5 ;180 13C #3 3u pl12:f2 d28 ; 3u pl22:f2 p2:f1 ph6 ;180 13C #4 3u pl12:f2 d29 ; d14 do:f2; gated decoupling 1u cpds2:f2 2u:f1 ph0 ;dead time delay, reset RF phase to detect go=2 ph31 ;do NS scans 1m do:f2 id6 ;increment d6 by in6=tr/4: gamma-average for clean TOSS lo to 2 times l5 ;1D wr #0 14 dd6 ;decrement d6 again lo to 14 times l5 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 TOSS ph5= 1 1 2 2 3 3 0 0 ;180 13C #3 TOSS 3 3 0 0 1 1 2 2 ph6= 2 2 1 1 0 0 3 3 ;;180 13C #4 TOSS 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 0 1 1 2 2 3 3 ;180 at tau for csa filter along CP ph13= 2 2 2 2 2 2 2 2 ;180 pulse at tr, exorcycle 3 3 3 3 3 3 3 3 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 ph14= 2 2 3 3 0 0 1 1 ;third 180 ph31= 0 2 3 1 2 0 1 3 ;RLS 2 0 1 3 0 2 3 1