;cpfprfdr (TopSpin 3.0) ;2D exchange NMR in rotating solids ;rotor synchronized, set cnst31=spin rate, spin rate regulation ;recommended ;see Bennet, Ok, Griffin, Vega J. Chem. Phys. 98, 8624 (1992) ;written by HF, 16.9.98 modified by HF 21.5.07 ;see Yoshitaka Ishii J. Chem. Phys. 114, 8473 (2001) ;fpRFDR included JOS 11/11/2004 ;tested and upgrade to TS2.1 2007 JOS ;tested and upgraded to TS3.0 05/11/2011 JOS ;modified by dan ;Proton offset at LG frequency during mix to avoid HH transfer ;use TPPI for transform, phases will be dispersive ;Avance III version ;parameters: ;d1 : recycle delay ;d0 : =1u t1 evolution period ;in0 : = 1/swh{F1} ;pl1 : X power level ;pl11 : power level for X pulses ;sp0 : carbon power level during contact ;pl2 : proton power level during contact ;pl12 : power level for H 90 ;pl22 : standard proton decoupling ;pl13 : power level of LG decoupling, 120 dB at high spin rates >15 kHz ;pl21 : power level for pi pulse during rfdr ;pcpd2 : pulse length in decoupling sequence ;p15 : contact time at pl1 (f1) and pl2 (f2) ;p10 : pulse length for FSLG shape ;p3 : H 90 degree pulse ;p1 : X 90 degree pulse ;p2 : X 180 degree pulse ;cpdprg2 : Sequence used for decoupling in t1 t2 (tppm15, cw, etc.) ;cpdprg1 : cwlg, using pl13 ;cpdprg3 : Sequence for decoupling in mixing ;spnam0 : file name for variable amplitude CP ;cnst20 : proton RF field to calculate LG parameters ;cnst21 : =0, proton offset ;cnst22 : +ve Lee-Goldburg offset ;cnst23 : -ve Lee-Goldburg offset ;cnst24 : additional Lee-Goldburg offset ;cnst31 : spinning frequency ;l1 : number of rotor cycles for mixing time ;$COMMENT=exchange NMR (RFDR) in rotating solids, rotor synchronized ;$CLASS=Solids ;$DIM=2D ;$TYPE=cross polarisation ;$SUBTYPE=homonuclear correlation ;$OWNER=Bruker #include #ifdef fprfdr "p2=1s/(3*cnst31)" #endif define delay tau "tau=0.5s/cnst31-p2/2" "d31=1s/cnst31" ;"d0=1s/cnst31" define delay mix "mix=l1*d31" ;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt "acqt0=1u*cnst11" "in0=inf1" "d0=0.1u" #include ; defines which channel corresponds to which nucleus #include ;calculates the lg offset cnst22 from cnst20=RF field ;###################################################### ;# Start of Active Pulse Program # ;###################################################### 1 ze #include ;protect for too slow rotation #include ;make sure p15 does not exceed 10 msec ;let supervisor change this pulseprogram if ;more is needed #include ;allows max. 50 msec acquisition time, supervisor ;may change to max. 1s at less than 5 % duty cycle ;and reduced decoupling field mix d31 2 10m do:H d1 rpp4 2u fq=cnst21:H trigg ;###################################################### ;# Initial excitation # ;###################################################### (p3 pl12 ph1):H (p15 pl1 ph2):C (p15:sp0 ph10):H ;###################################################### ;# t1 evolution # ;# Polarization is on 13C # ;###################################################### d0 cpds2:H ;###################################################### ;# store 13C along Z # ;# turn off 1H briefly for states # ;###################################################### (p1 pl11 ph3):C ;something like IzCos + IySin nox 0.1u do:H ;turn off decoupler 2m ;need delay to let IySin term vanish for states 1u cpds3:H 5 tau ;mixing time with Gullion sequence (p2 pl21 ph4^):C tau lo to 5 times l1 0.1u do:H 2m ;###################################################### ;# recall the 13C along Z # ;###################################################### (p1 pl11 ph5):C ;####################################################### ;# Acquisition # ;####################################################### go=2 ph31 cpds2:H 1m do:H 10m mc #0 to 2 F1PH(ip2,id0) HaltAcqu, 1m 6 exit ;##################################### ;# Phase Cycle # ;##################################### ph1=3 1 ph2=3 ph3= 0 0 0 0 2 2 2 2 ph4=0 1 0 1 1 0 1 0 2 3 2 3 3 2 3 2 ;xy16 ph5=0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph10=0 0 2 2 ph31=0 2 2 0 2 0 0 2 2 0 0 2 0 2 2 0