;cpSPINDIFF ; ;version: 1.0/ TS3 / 6/24/2011 ; ;basic 2D homonuclear exchange experiment ;written by HF and JOS ;updated JOS 6/24/2011 ;checked by JOS 24/6/2011 ; ;General Comment ;2D exchange NMR in rotating solids using PDSD mixing (PL14=120db) ;or DARR/RAD mixing with pl14 set such that the RF field is n*spin rate, n=1-3 ;rotor synchronized, set cnst31=spin rate in Hz ;rotor synchronize in F1 choose n*spin rate for SWH in F1 ;DARR Dipolar assisted rotational resonance (K. Takegoshi et al Chem. Phys. Lett. 2001, 344, 631. ;RAD (RF assisted diffusion) C.R. Morcombe et al., JACS 2004, 126, 7196. ; ;requires modification to run under TS2.1 inquire with applications ; ;Avance III version ;parameters: ;d1 : recycle delay ;p1 : X 90 degree pulse ;p3 : H 90 degree pulse ;p15 : contact time at plw1 (rf-channel f1) and spw0 (rf-channel f2) ;pl11 : rf-power on X for 90 degree pulses ;pl12 : rf-power for 1H pi/2 pulse p3 and standard proton decoupling ;pl13 : e.g. used in tppm13 ;pl14 : rf-power for RAD-DARR mixing pulse, calculate or measure B1 field = 1 * rotation rate ;cnst31 : spinning rate in Hz ;d8 : mixing time,recalculated for multiple rotor period, max. 500 msec ;sp0 : rf-power for contact pulse of 1H channel (rf-channel f2) ;spnam0 : file name for shaped CP pulse ;cpdprg2 : 1H decoupling sequence (spinal64, tppm15, cw, etc.) ;FnMODE: TPPI, States-TPPI or STATES ;ns : 16*n ;SWH[F1]: integer multiple of rotor frequency ;zgoptns: -Dlacq, -Dlcp15, or blank ; ; ;$CLASS=BioSolids ;$DIM=2D ;$TYPE=cross polarisation ;$SUBTYPE=homonuclear correlation ;$COMMENT=exchange NMR in rotating solids using RAD/DARR for improved spin exchange, rotor synchronised prosol relations= #include #include "cnst59=plw14" "d31=1s/cnst31" define pulse mixing define delay darrmix define loopcounter count define loopcounter darr "darr=d8/d31" /*setup for rotor synchronized mixing time */ "mixing=(darr*d31)" "l0=0" /* house keeping for detection in t1, start at t1=0 for flat baseline */ "in0=inf1" "d0=1u" "acqt0=-p1/2" "darrmix=mixing" 1 ze #include #ifndef lcp15 #include ;make sure p15 does not exceed 10 msec ;let supervisor change this pulseprogram if ;more is needed #endif #ifndef lacq ;disable protection file for long acquisition change decoupling power !!! or you risk probe damage ;if you set the label lacq (ZGOPTNS -Dlacq), the protection is disabled #include ;allows max. 50 msec acquisition time, supervisor ;may change to max. 1s at less than 5 % duty cycle ;and reduced decoupling field #endif #include /*allows max. 500 msec mixing time for PDSD, 100m for DARR*/ darrmix d31 2 10m do:f2 d1 1u fq=cnst21:f2 10u pl12:f2 pl1:f1 ;preselect pl2 drive power for F2 trigg p3:f2 ph1 ;proton 90 pulse (p15 ph2):f1 (p15:sp0 ph10):f2 ;contact pulse if "l0==1"{ "d0=in0" } if "l0>0" { ;use cpdprg2=tppm15, SPINAL64 or XiX d0 cpds2:f2 } (p1 pl11 ph3):f1 (1u do):f2 (mixing pl14 ph11):f2 (p1 ph5):f1 (1u cpds2):f2 go=2 ph31 1m do:f2 10m mc #0 to 2 F1PH(ip2,id0 & iu0) HaltAcqu, 1m 6 exit ph1=1 3 ph2=1 ph3={0}*8 {2}*8 ph5=0 0 2 2 1 1 3 3 ph10=0 ph11=0 ph31=0 2 2 0 1 3 3 1 2 0 0 2 3 1 1 3 ;$Id: cpSPINDIFF,v 1.1.6.2 2017/02/22 17:02:01 ber Exp $