;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 ;pcpd2 : pulse length in decoupling sequence ;p15 : contact time at pl1 (f1) and pl2 (H) ;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 ;cnst31 : spinning frequency ;$COMMENT=exchange NMR (RFDR) in rotating solids, rotor synchronized ;$CLASS=Solids ;$DIM=2D ;$TYPE=cross polarisation ;$SUBTYPE=homonuclear correlation ;$OWNER=Bruker #include #include ; defines which channel corresponds to which nucleus ;###################################################### ;# Define CORD # ;###################################################### "d31=1s/cnst31" "p11=(1s/cnst31)/2" define delay cordmix define loopcounter cord define pulse mixing "cord=d8/(24*d31)" "l11=cord" "mixing=(cord*24*d31)" "cordmix=mixing" ;###################################################### "in0=inf1" ;########################## "d0=1u" ;# t1_init => 0, 0 # ;########################## "l0=0" ; #/* house keeping for detection in t1, start at t1=0 for flat baseline */ "acqt0=-p1/2" ;###################################################### ;# Start of Active Pulse Program # ;###################################################### #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 1 ze cordmix d31 2 10m do:H d1 rpp17 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 0.1u do:H ;decoupler off ;###################################################### ;# store 13C along Z # ;# turn off 1H briefly for states # ;###################################################### (p1 pl11 ph3):C ;something like IzCos + IySin nox 5 (p11 pl14 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11*2 pl15 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H (p11 pl14 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11*2 pl15 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H (p11 pl14 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11*2 pl15 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H (p11 pl14 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11 ph17^):H (p11*2 pl15 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H (p11*2 ph17^):H lo to 5 times l11 0.1u do:H ;decoupler off ;###################################################### ;# 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 ph17= 1 3 2 2 1 3 2 2 2 0 3 3 2 0 3 3 3 1 0 0 3 1 0 0 0 2 1 1 0 2 1 1 ;XY814 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 ;##################################### ;# END SEQUENCE # ;#####################################