;seldipsy ;13/04/2016 ; ; 1D selective TOCSY PSYCHE ; DIPSI-2 sequence for mixing ; using selective refocussing with a shaped pulse ; and with zero-quantum suppression ; ; Guilherme Dal Poggetto and Laura Castaņar ; University of Manchester ; ;Avance II+/III Version ;Topspin 3.x ; ;Data can be reconstructed using a macro available at http://nmr.chemistry.manchester.ac.uk ; ;References ;(1) Dal Poggetto, G.; Castaņar, L.; Morris, G. A.; Nilsson, M.; RSC Adv. 2016, 6, 100063. ;(2) Foroozandeh, M.; Adams, R. W.; Meharry, N. J.; Jeannerat, D.; Nilsson, M.; Morris, G. A. Angew. Chem. Int. Ed. 2014, 53, 6990. ;(3) Thrippleton, M.J.; Keeler, J.; Angew. Chem. Int. Ed. 2003, 42, 3938. ;(4) Kessler,H.; Oschkinat, H.; Griesinger, C.; Bermel, W.; J. Magn. Reson. 1986, 70, 106. ; ;$CLASS=HighRes ;$DIM=1D ;$TYPE= ;$SUBTYPE= ;$COMMENT= TOPSPIN3.x #include #include #include define delay tauA define delay tauB "in0=inf1/2" "p2=p1*2" "p11=p10" "tauA=in0/2-p16-d16-50u" "tauB=(dw*2*cnst4)+d16+50u" "spoff10=0" "spoff12=bf1*(cnst12/1000000)-o1" "spoff32=0" "spoff34=0" "p33=1000000.0/(cnst53*4)" "cnst33= (p33/p1) * (p33/p1)" "spw32=plw1/cnst33" "p35=1000000.0/(cnst54*4)" "cnst35= (p35/p1) * (p35/p1)" "spw34=plw1/cnst35" "cnst50=(cnst20/360)*sqrt((2*cnst21)/(p10/2000000))" "p30=1000000.0/(cnst50*4)" "cnst31= (p30/p1) * (p30/p1)" "spw10=plw1/cnst31" "FACTOR1=(d9/(p6*115.112))/2" "l1=FACTOR1*2" 1 ze 2 30m 20u pl1:f1 BLKGRAD d1 50u UNBLKGRAD (p1 ph1):f1 3u p17:gp1 d17 pl0:f1 p12:sp12:f1 ph2:r ;selective SE 3u p17:gp1 d17 pl1:f1 ;Begin TOCSY block p1 ph3 10u gron0 (p32:sp32 ph3):f1 20u groff d17 pl10:f1 ;begin DIPSI2 3 p6*3.556 ph23 p6*4.556 ph25 p6*3.222 ph23 p6*3.167 ph25 p6*0.333 ph23 p6*2.722 ph25 p6*4.167 ph23 p6*2.944 ph25 p6*4.111 ph23 p6*3.556 ph25 p6*4.556 ph23 p6*3.222 ph25 p6*3.167 ph23 p6*0.333 ph25 p6*2.722 ph23 p6*4.167 ph25 p6*2.944 ph23 p6*4.111 ph25 p6*3.556 ph25 p6*4.556 ph23 p6*3.222 ph25 p6*3.167 ph23 p6*0.333 ph25 p6*2.722 ph23 p6*4.167 ph25 p6*2.944 ph23 p6*4.111 ph25 p6*3.556 ph23 p6*4.556 ph25 p6*3.222 ph23 p6*3.167 ph25 p6*0.333 ph23 p6*2.722 ph25 p6*4.167 ph23 p6*2.944 ph25 p6*4.111 ph23 lo to 3 times l1 ;end DIPSI2 p17:gp2 d17 10u gron10 (p34:sp34 ph3):f1 20u groff d17 pl1:f1 p1 ph3 ;end TOCSY ;Begin PSYCHE 4 d0 tauA 50u p16:gp3 d16 p2 ph4 50u p16:gp3 d16 tauA p16:gp4 d16 10u pl0:f1 tauB ( center (p10:sp10 ph5):f1 (p11:gp11) ) ;PSYCHE element d16 10u pl1:f1 p16:gp4 d16 50u BLKGRAD d0 ;End PSYCHE go=2 ph31 30m mc #0 to 2 F1QF(id0) exit ph1= 0 2 ph2= 0 0 1 1 2 2 3 3 ph3= 0 ph4= 0 ph5= 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 ph23=3 ph25=1 ph31=0 2 2 0 0 2 2 0 2 0 0 2 2 0 0 2 ;POWER LEVEL ;pl0 : zero power (0W) ;pl1 : power level for pulse (default) ;pl10 : power level for TOCSY-spinlock ;sp10 : power level of double-chirp PSYCHE pulse element ;sp12 : power level of refocusing shaped pulse ;sp32 : power level of adiabatic pulse of first ZQF element ;sp34 : power level of adiabatic pulse of last ZQF element ;PULSE DURATION ;p1 : 90 degree high power pulse ;p2 : 180 degree high power pulse ;p6 : 90 degree low power pulse ;p10 : duration of double-chirp PSYCHE pulse element [30 ms] ;p12 : 180 degree refocusing shaped pulse ; choose p12 according to desired selectivity ;p32 : first ZQF 180 degree inversion shaped pulse (adiabatic) [10 msec] ;p34 : second ZQF 180 degree inversion shaped pulse (adiabatic) [30 msec] ;GRADIENT DURATION ;p11 : duration of weak gradient during PSYCHE pulse element [p11=p10] ;p16 : duration of CTP gradients for PSYCHE [1 ms] ;p17 : duration of CTP gradients for Selective-TOCSY [0.9 ms] ;DELAY ;d0 : incremented delay ;d1 : relaxation delay [5*T1 s] ;d9 : TOCSY mixing time [50-200 ms] ;d16 : recovery delay for gradients in PSYCHE block [1 ms] ;d17 : selective spin-echo delay in selective-TOCSY block [200 us] ;PULSE SHAPE ;spnam10 : file name for PSYCHE pulse element [SALTIRE] ;spnam12 : file name for the selective 180 refocusing shaped pulse [RSNOB or REBURP] ;spnam32 : file name for the adiabatic shaped pulse using in first ZQF [CHIRP] ; smoothed chirp (low to high, 20% smoothing, 1000 points, 20KHz) ;spnam34 : file name for the adiabatic shaped pulse using in last ZQF [CHIRP] ; smoothed chirp (low to high, 20% smoothing, 1000 points, 20KHz) ;GRADIENT SHAPE ;gpnam1 : SMSQ10.100 ;gpnam2 : SMSQ10.100 ;gpnam3 : SINE.100 ;gpnam4 : SINE.100 ;gpnam11: RECT.1 ;GRADIENT STRENGTH ;gpz0 : first ZQF gradient [3%] ;gpz1 : CTP gradient [13%] ;gpz2 : CTP gradient [31%] ;gpz3 : CTP gradient [77%] ;gpz4 : CTP gradient [49%] ;gpz10: last ZQF gradient [2%] ;gpz11: weak gradient during PSYCHE element [1-3%] ;CONSTANTS ;cnst4 : number of drop points from FID ;cnst12: chemical shift for selective pulse (offset, in ppm) ;cnst20: desired flip angle for PSYCHE pulse element (degree) [10-25] ;cnst21: bandwidth of each chirp in PSYCHE pulse element (Hz) [10000 Hz] ;cnst53: GammaB1 of first adiabatic ZQF shaped pulse ;cnst54: GammaB1 of last adiabatic ZQF shaped pulse ;OTHER ;ns : 8 * n, total number of scans: NS * TD0 ;ds : 8 ;td1 : number of t1 increments [16-64] ;sw1 : sw2/n (n has to be an integer number) [40-100 Hz] ;in0 : 1/(2 * SW) = DW ;nd0 : 2 ;l1 : loop for DIPSI cycle: ((p6*115.112) * l1) = mixing time ;MC2 : QF