; SCALPEL_idiff ; ; SCALPEL (Spectral Component Acquisition by Localized PARAFAC Extraction of Linear components) ; ; TOCSY-t1 encoding combined with ; double selective iDOSY z-TOCSY ; using DIPSI2 sequence for mixing ; with zero quantum suppression ; and option for water pre-saturation ; ; uses squared steps for sampling in t1-evolution ; and double selective excitation sculpting for iDOSY ; ; THE USE OF WAVEMAKER IS RECOMENDED ; ; Guilherme Dal Poggetto ; University of Manchester ; <2018> ; ; ; (1) M.J. Thrippleton and J. Keeler, Angew. Chem. Int. Ed., 42, 3938 (2003) ; (2) N. Birlirakis and E. Guittet, JACS 118, 13083 (1996) ; (3) P. Howe, Magn. Reson. Chem. 55, 433 (2017) ; (4) L. Braunschweiler and R. R. Ernst, J. Magn. Reson., 53, 521 (1983) ; (5) G. Dal Poggetto, L. Castaņar, R. A. Adams, G. A. Morris and M. Nilsson, Chem. Commun., 53, 7461 (2017) ; ;$CLASS=HighRes ;$DIM=3D ;$TYPE= ;$SUBTYPE= ;$COMMENT= #include #include #include #include ;%%%%%%%%%% WaveMaker Parameters %%%%%%%%%% "d11=30m+1s/(cnst12)-1s/(cnst12)" ;sp12:wvm:gdp_reburp:f1 reburp(cnst12 Hz, PL; NPOINTS=10000) ;%%%%%%%%%% DOSY Parameters %%%%%%%%%% define list diff= "cnst17=0" ;Dtau "cnst18=0.000001*0.000001*p30*p30*(d20-(0.000001*p30/2))" ;Dosytimecubed "DELTA1=((d20/2)-p12-p30-d16)/2" ;%%%%%%%% sel-TOCSY Parameters %%%%%%% "p6=1000000.0/(cnst6*4)" "cnst46= (p6/p1) * (p6/p1)" "plw10=plw1/cnst46" "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" "FACTOR1=(d9/(p6*115.112))/2" "l1=FACTOR1*2" "spoal32=0.5" "spoal34=0.5" "spoff32=0" "spoff34=0" "cnst28=o1" "cnst30=(cnst29*bf1)-cnst28" "cnst31=0" ;%%%%%%%%%% TOCSY-t1 Parameters %%%%%%%%% "d0=0u" "l11=0" "in0=1/2*cnst6" "cnst2=0" "cnst3=((cnst1*in0)*(cnst1*in0))/(td1-1)" ;%%%%%%%%%% Other Parameters %%%%%%%%% "p2=2*p1" "d11=30m" "cnst40=(cnst49*bf1)-cnst28" "acqt0=-p1*2/3.1416" aqseq 312 ;%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%% 1 ze 2 d11 pl1:f1 "cnst2=cnst3*l11" "d0=sqrt(cnst2)" 10u UNBLKGRAD p8 ph21 p8 ph22 p18:gp8 d18 BLKGRAD 1m fq=cnst40:f1 20u pl9:f1 d1 1s cw:f1 ph29 4u do:f1 1m fq=cnst31:f1 20u pl1:f1 50u UNBLKGRAD p18:gp8*-1 d18 p1 ph1 d0 p1 ph4 10u fq=cnst30:f1 5u pl0:f1 100u gron0 (p32:sp32 ph5):f1 20u groff 100u pl10:f1 ;begin DIPSI2 4 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 4 times l1 ;end DIPSI2 p18:gp8*-1 d18 5u pl0:f1 100u gron10 (p34:sp34 ph5):f1 20u groff 20u pl1:f1 10u fq=cnst31:f1 p1 ph4 5 p30:gp1*diff d16 pl0:f1 DELTA1 p12:sp12:f1 ph2 DELTA1 p30:gp1*diff d16 pl1:f1 p2 ph4 p30:gp1*-1*diff d16 pl0:f1 DELTA1 p12:sp12:f1 ph3 DELTA1 p30:gp1*-1*diff d16 pl1:f1 p1 ph6 10u fq=cnst30:f1 5u pl0:f1 100u gron0*-1 (p32:sp32 ph5):f1 20u groff 1m pl10:f1 ;begin DIPSI2 6 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 6 times l1 ;end DIPSI2 3u p18:gp8 d18 5u pl0:f1 100u gron10*-1 (p34:sp34 ph5):f1 20u groff 20u pl1:f1 10u fq=cnst31:f1 100u BLKGRAD p1 ph7 go=2 ph31 d11 mc #0 to 2 F2QF(calgrad(diff)) F1QF(calclc(l11,1)) exit ; Phase cycling ph1= 0 2 ph2= 0 0 1 1 2 2 3 3 ph3= 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ph4= 0 ph5= 0 ph6= 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph7= 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ph21= 0 ph22= 1 ph23= 3 ph25= 1 ph29= 0 ph31= 0 2 2 0 0 2 2 0 2 0 0 2 2 0 0 2 2 0 0 2 2 0 0 2 0 2 2 0 0 2 2 0 ;POWER LEVEL ;pl0 : zero power (0W) ;pl1 : power level for pulse (default) ;pl9 : power level for pre-saturation ;pl10 : power level for TOCSY-spinlock ;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 ;p8 : Spherical randomization pulse [1-1.5 msec] ;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 ;p18 : homospoil gradient [1 msec] ;p30 : DOSY gradient pulse (little delta) [0.5 - 4 msec] ;DELAY ;d0 : increment in TOCSY indirect dimension ;d1 : relaxation delay; [1-10 s] ;d9 : TOCSY mixing time [50-200 ms] ;d11 : delay for disk I/O [30 msec] ;d16 : DOSY gradient pulse recovering delay ;d18 : saturation recovery pulse /TOCSY gradient pulse delay ;d20 : Diffusion encoding period (BIG DELTA) ;PULSE SHAPE ;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 : SINE.100 ;gpnam8 : SMSQ10.100 ;GRADIENT STRENGTH ;gpz0 : first ZQF gradient [3%] ;gpz1 : DOSY gradients [100%] ;gpz8 : homospoil gradient [31%] ;gpz10: last ZQF gradient [4%] ;CONSTANTS ;cnst1: last time increment for t1-TOCSY ;cnst2: first time increment for t1-TOCSY ;cnst3: square of time increment for t1-TOCSY ;cnst6: bandwidth of TOCSY transfer ;cnst12: bandwidth of selective refocussing pulse ;cnst29: offset for TOCSY block (ppm) ;cnst49: water chemical shift (ppm) ;cnst53: GammaB1 of first adiabatic ZQF shaped pulse ;cnst54: GammaB1 of last adiabatic ZQF shaped pulse ;OTHER ;in0 : time evolution for t1-TOCSY ;td1 : number of t1-TOCSY increments ;td2 : number of DOSY increments ;l1 : number of DIPSI-2 loops ;PARMOD = 3D ;NS: 8 * n, total number of scans: NS * TD0 ;DS: 16