;sronepcsafilsp2A.echo ;from sronepcsafilsp2A.cpd ;from srcsafilsp2A.cpd ;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 detection by l5-loop (set l5 = # of sidebands, 4 typically) ;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-p1/2" ; tr-tau in CSA recoupling ;add -p2/2 Dec.01 "d13=1s/l31-p2/2-p1/2-1u" "d15=d13-d14" "d3=d13-10u" 1 ze 10u pl1:f1 ;preselect pl1 drive power level for F1 2 d1 do:f2 ;recycle delay, turn the decoupler off 10u pl22:f2 ;preselect pl2 drive power for F2 10u pl11:f1 ;preselect pl11 drive power level for F1 1u cw:f2 ;turn on F2 decoupling p1:f1 ph1 ;X 90 pulse d21 ;tau of CSA dephasing (max. dephasing if d21 = tr/2) p2:f1 ph12 ;180 pulse at tau, along initial magnetization d22 ;finish 1 tr p2:f1 ph13 ;180 pulse at tr d22 ; p2:f1 ph14 ;180 pulse at 2tr - tau d21 p1:f1 ph7 ;store for z-filter d6 do:f2 ;z-filter & gamma integral 1u pl12:f2 ;set decoupling drive power level p1:f1 ph8 ;read out d14 ;gated decoupling 1u cpds2:f2 d15 p2:f1 ph3 ;180 13C #1 d3 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 ;X 90 excitation ph3= 0 0 1 1 2 2 3 3 ;180 before detection 0 0 1 1 2 2 3 3 0 0 1 1 2 2 3 3 0 0 1 1 2 2 3 3 ; 1 1 2 2 3 3 0 0 ;put back in ; 1 1 2 2 3 3 0 0 ; 1 1 2 2 3 3 0 0 ; 1 1 2 2 3 3 0 0 ; 2 2 3 3 0 0 1 1 ; 2 2 3 3 0 0 1 1 ; 2 2 3 3 0 0 1 1 ; 2 2 3 3 0 0 1 1 ; 3 3 0 0 1 1 2 2 ; 3 3 0 0 1 1 2 2 ; 3 3 0 0 1 1 2 2 ; 3 3 0 0 1 1 2 2 ph7= 1 1 ;store for z-filter after t1 ph8= 3 3 0 0 1 1 2 2 ;read out after z-filter ph12= 0 ;180 at tau for csa filter along magnetization 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 ;third 180 ph31= 0 2 1 3 2 0 3 1 ;RLS 2 0 3 1 0 2 1 3 ;ph13 exorcycle 0 2 1 3 2 0 3 1 ; 2 0 3 1 0 2 1 3 ; ;32 scans fine for near resonance ; 2 0 3 1 0 2 1 3 ;ph3 exorcycle ; 0 2 1 3 2 0 3 1 ; ; 2 0 3 1 0 2 1 3 ; ; 0 2 1 3 2 0 3 1 ;