;zTEDOR ; ;version: 2.0 TS3 / 7/14/2011 ; ;transverse echo double resonance experiment ;Tested 12/06 in jos1206 on AV III console ;updated and tested JOS 07/14/2011 ; ;Reference: ;C.P. Jaroniec, C. Filip, and R.G. Griffin, JACS 124, 2002, 10728-10742 ; ;Avance III version ;parameters: ;d1 : recycle delay ;d31 : =1s/cnst31, 1 rotor period, to check correct cnst31 value ;p2 : C 180 degree pulse ;p3 : H 90 degree 1H pulse ;p5 : N 90 deg. ;p12 : N 180 deg. ;p15 : H/C contact pulse ;cnst31 : must be set to the spinning speed (in Hz). ;spnam0 : H file name for variable amplitude CP ;spnam10 : C band selective shape ;pl1 : C CP power ;pl3 : N Hard Power ;pl12 : H power for decoupling; tppm ;pl13 : H power for decoupling during recoupling (for instance using lgcw) ;sp0 : H rf-power for proton contact pulse ;cpdprg2 : H decoupling sequence for data acquisition and t1 evolution period ;pcpd2 : H decoupling pulse width ;cpdprg3 : H decoupling during recoupling block us cw13 or lgcw ;FnMODE: use States-TPPI, States or TPPI ;ZGOPTNS : -DsmallSW for rotor synchronization for spectral width in F1 < sample rotation rate ;l9 : fraction of rotation rate for t1 increment for choice of smallSW else multiple of rotor frequency for larger SW ;ns : n*16 =n*32 with td=phase cycle ;cnst22 : C offset for CP; ppm ;cnst26 : C offset for Band select 180; ppm ;cnst10 : C offset for detect; ppm ; ;$CLASS=Solids ;$DIM=2D ;$TYPE=cross polarisation ;$SUBTYPE=TEDOR ;$COMMENT=heteronuclear correlation prosol relations= "d25=0.25s/cnst31-1u" "d26=0.25s/cnst31-(p12/2)" ; one-quarter rotor cycle ... "d27=0.25s/cnst31-(p1)" "d28=0.25s/cnst31-5u" ;"d29=0.75s/cnst31-(p2/2)" "d29=0.5s/cnst31" ; adjust for selective pi of 600us etc "d31=1s/cnst31" define pulse tauz "tauz=l8*1s/cnst31-p1" "d0=1s/(l9*cnst31)" "acqt0=1u*cnst11" define delay t1incr "l0=0" ;###################################################### ;# delays/t1 defs for SWH #include ;make sure p15 does not exceed 10 msec ;let supervisor change this pulseprogram if ;more is needed #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 ; defines which channel corresponds to which nucleus ;###################################################### ;# Start of Active Pulse Program # ;###################################################### 1 ze t1incr tau mix 2 30m d1 do:H #ifndef smallSW "l11=l10 %l9" "d2=1s*(2*l9-l11)/(l9*cnst31)" #endif 10u pl1:C ;set power level to drive HP amplifier 10u pl12:H ;set decoupler power 10u pl3:N 1m rpp8 ; reset phase list ph8 ... 1m rpp9 1m rpp10 1m rpp11 0.5u fq=cnst22(bf ppm):C ;C jump for CP trigg ;additional trigger available on HP router ;###################################################### ;# Initial excitation # ;###################################################### p3:H ph1 ;90 degree proton pulse (p15 ph2):C (p15:sp0 ph19):H ;cross-polarization ;###################################################### ;# First half REDOR Ix->2IySz; tm/4 # ;# TPPM # ;###################################################### 0.1u cpds2:H d25 ; tppm decoupling at pl12 if synchronized with TPPM use special decoupling sequence 5 d26 ; several F3 pulses ... (p12 ph8^):N ; ... at intervals of ... d26 ; ... one-half rotor cycle d26 (p12 ph8^):N ; ... at intervals of ... d26 ; F1 pulse d26 ; several F3 pulses ... (p12 ph8^):N ; ... at intervals of ... d26 ; ... at intervals of ... d26 ; ... one-half rotor cycle (p12 ph8^):N ; ... at intervals of ... d26 ; F1 pulse lo to 5 times l1 ;###################################################### ;# selective C Pi pulse; 2*m*tr # ;# CW # ;###################################################### 0.5u fq=cnst26(bf ppm):C ;C jump for rfdr d29 ; 0.5tr ; d26=0.25tr ; 0.1u do:H ; DEC OFF (p2:sp10 ph6):C (p2 pl13 ph0):H ; make p2=(2*n+0.5)*tr; 8.5tr is ok 0.1u cpds2:H ; DEC ON ; d29 ; 0.5tr ; d26=0.25tr ;###################################################### ;# REDOR second tm/4 # ;# TPPM # ;###################################################### 6 d26 ; several F3 pulses ... (p12 ph9^):N ; ... at intervals of ... d26 ; ... at intervals of ... d26 ; ... one-half rotor cycle (p12 ph9^):N ; ... at intervals of ... d26 ; d26 ; several F3 pulses ... (p12 ph9^):N ; ... at intervals of ... d26 ; ... at intervals of ... d26 ; ... one-half rotor cycle (p12 ph9^):N ; ... at intervals of ... d26 ; F1 pulse lo to 6 times l1 d27 ;####################################################### ;# IySz -> IzSy 90s # ;####################################################### 0.1u fq=cnst10(bf ppm):C ;set 13c for dir detect offset (p1 ph6):C (0.1u do):H ; end of integer rotor period (p5 ph6):N ; begin rotor period at beginning of pulse ;###################################################### ;# t1 evolution # ;# Polarization is on 15N # ;# TPPM # ;###################################################### if "l0==1"{ "d0=in0" } if "l0>0"{ d0 cpds2:H } ;###################################################### ;# IzSy -> IySz 90s # ;# CW # ;###################################################### (p5 ph3):N (0.1u do):H d2 cpds3:H ;CW and rotor synchronization (p1 ph4):C ; rotor period done at end of p1! 0.1u do:H ; DEC OFF 0.1u cpds2:H ; DEC ON ;###################################################### ;# First half REDOR 2IySz->Sx # ;# TPPM # ;###################################################### d25 ; tppm decoupling at pl12 7 d26 ; several F3 pulses ... (p12 ph10^):N ; ... at intervals of ... d26 ; ... one-half rotor cycle d26 (p12 ph10^):N ; ... at intervals of ... d26 d26 ; several F3 pulses ... (p12 ph10^):N ; ... at intervals of ... d26 ; ... one-half rotor cycle d26 (p12 ph10^):N ; ... at intervals of ... d26 lo to 7 times l1 ;###################################################### ;# selective C Pi pulse; 2*m*tr # ;# CW # ;###################################################### 0.1u fq=cnst26(bf ppm):C ;C jump for rfdr d29 ; 0.5tr ; d26=0.25tr ; 0.1u do:H ; DEC OFF (p2:sp10 ph6):C (p2 pl13 ph0):H ; make p2=(2*n+0.5)*tr; 8.5tr is ok 0.1u cpds2:H ; DEC ON ; d29 ; 0.5tr ; d26=0.25tr ;###################################################### ;# REDOR second tm/4 # ;# TPPM # ;###################################################### 8 d26 ; several F3 pulses ... (p12 ph11^):N ; ... at intervals of ... d26 ; ... one-half rotor cycle d26 (p12 ph11^):N ; ... at intervals of ... d26 d26 ; several F3 pulses ... (p12 ph11^):N ; ... at intervals of ... d26 ; ... one-half rotor cycle d26 (p12 ph11^):N ; ... at intervals of ... d26 lo to 8 times l1 d27 ; Hahn echo occurs about now ;####################################################### ;# Acquisition # ;# Polarization is on 13C # ;# TPPM # ;####################################################### 0.1u fq=cnst10(bf ppm):C ;set 13c for dir detect offset go=2 ph31 1m do:H 30m mc #0 to 2 F1PH(ip3,id0 & iu10 & iu0) HaltAcqu, 1m exit ;##################################### ;# Phase Cycle # ;##################################### ph1= {0}*8 {2}*8 ph0= 0 ph2= 0 ph3= 0 2 ph4= 0 0 1 1 2 2 3 3 ph6= 0 ph8= 0 1 0 1 1 0 1 0 2 3 2 3 3 2 3 2 ;xy16 ph9= 0 1 0 1 1 0 1 0 2 3 2 3 3 2 3 2 ph10= 0 1 0 1 1 0 1 0 2 3 2 3 3 2 3 2 ph11= 0 1 0 1 1 0 1 0 2 3 2 3 3 2 3 2 ph19= 1 ph31= 2 0 1 3 0 2 3 1 0 2 3 1 2 0 1 3 ;$Id: zTEDOR,v 1.2.2.2 2017/02/22 17:02:22 ber Exp $