;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 ;added tppm15/CW decoupling during fprfdr ;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 CP power level ;pl11 : power level for X pulses ;pl31 : power level for X pulses rfdr ;sp0 : H power level during contact ;pl12 : H dec power level for H 90 ;pl13 : H power level of CW decoupling, 120 dB at high spin rates >15 kHz ;pcpd2 : pulse length in decoupling sequence ;p15 : contact time at pl1 (f1) and pl2 (f2) ;p3 : H 90 degree pulse ;p1 : X 90 degree pulse ;p2 : X 180 degree pulse ;p31 : X 180 degree pulse rfpdr ;cpdprg2 : Sequence used for decoupling in t1 t2 (tppm15, cw, etc.) ;cpdprg1 : cwlg, using pl13 ;spnam0 : file name for variable amplitude CP ;cnst21 : =0, proton offset ;cnst22 : C offset for CP; ppm ;cnst26 : C offset for FPrfdr; ppm ;cnst10 : C offset for detect; ppm ;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 "p31=1s/(3*cnst31)" #endif define delay tau "tau=0.5s/cnst31-p31/2" "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 ;###################################################### ;# 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 rpp17 2u fq=cnst21:H 0.5u fq=cnst22(bf ppm):C ;C jump for CP trigg ;###################################################### ;# Initial excitation # ;###################################################### (p3 pl12 ph1):H (p15 pl1 ph2):C (p15:sp0 ph10):H ;###################################################### ;# t1 evolution # ;# Polarization is on 13C # ;###################################################### 0.5u fq=cnst10(bf ppm):C ;set 13c for dir detect offset d0 cpds2:H ;###################################################### ;# store 13C along Z # ;# turn off 1H briefly for states # ;# TPPM/CW decoupling # ;###################################################### 0.5u fq=cnst26(bf ppm):C do:H ;C jump for rfdr (p1 pl11 ph3):C ;store C on Z 0.1u cpds2:H ; dec on 5 tau ;mixing time with Gullion sequence 0.1u do:H ; dec off (p31 pl31 ph17^):C (p31 pl13 ph0):H ;H cw dec 0.1u cpds2:H ; dec on tau lo to 5 times l1 0.1u do:H ; dec off ;###################################################### ;# recall the 13C along Z # ;###################################################### (p1 pl11 ph5):C 0.5u fq=cnst10(bf ppm):C ;set 13c for dir detect offset ;####################################################### ;# Acquisition # ;####################################################### go=2 ph31 cpds2:H 1m do:H 10m mc #0 to 2 F1PH(ip2,id0) HaltAcqu, 1m 6 exit ;##################################### ;# Phase Cycle # ;##################################### ph0=0 ph1=3 1 ph2=3 ph3= 0 0 0 0 2 2 2 2 ph17=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