; oneshothsqc ; avance-version (05/05/18) ; 3D DOSY-HSQC ; ; Guilheme Dal Poggetto, Laura Castaņar and Peter Kiraly ; University of Manchester ; <2018> ; ; 2D H-1/X correlation via double inept transfer ; phase sensitive using Echo/Antiecho-TPPI gradient selection ; diffusion encoding using Oneshot ; with decoupling during acquisition ; using shaped pulses for inversion and refocussing on f2 - channel ; ; For processing data use MAGNATE, available at: ; http://nmr.chemistry.manchester.ac.uk/ ; ;$CLASS=HighRes ;$DIM=3D ;$TYPE= ;$SUBTYPE= ;$COMMENT= #include #include #include ;;;;;;;;;;;;;;;; DOSY parameters ;;;;;;;;;;;;;;;; define list diff= "cnst14=0.2" "cnst15=1+cnst14" ; 1 + alpha "cnst16=1-cnst14" ; 1 - alpha "cnst17=(2*p1+d16)*0.000001"; Dtau %GDP corrected ;Assuming half-sine gradient pulses [most common on Bruker systems] "cnst18=0.000001*p30*2*0.000001*p30*2*(d20 - (2*0.000001*p30*(5-3*cnst14*cnst14)/16) - (cnst17*(1-cnst14*cnst14)/2) )" ; Dosytimecubed "DELTA1=d20-4.0*p1-4.0*p30-5.0*d16-p19" ; ;;;;;;;;;;;;;;;; HSQC parameters ;;;;;;;;;;;;;;;; "d4=1s/(cnst2*4)" "d0=3u" "in0=inf1/2" "DELTA2=d4-p16-larger(p2,p14)/2-de-8u" "DELTA3=d4-larger(p2,p14)/2" "DELTA4=d4-larger(p2,p14)/2-p1*2/PI" "DELTA=p16+d17+p2+d0*2" "d11=30m+1s/(cnst50)-1s/(cnst50)" "d11=30m+1s/(cnst51)-1s/(cnst51)" "d11=30m+1s/(cnst53)-1s/(cnst53)" "spoff3=0" "spoff7=0" "spoff15=0" "spoal3=0.5" "spoal7=0.5" "spoal15=0.5" ;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;;; "d18=2m" "p2=p1*2" "p4=2*p3" "d11=30m" "acqt0=0" baseopt_echo aqseq 312 1 ze d11 pl12:f2 2 d11 do:f2 1m pl1:f1 1m pl2:f2 10u UNBLKGRAD p8 ph21 p8 ph22 d18 BLKGRAD d1 1m UNBLKGRAD p19:gp2*-1.0 ;Spoiler gradient balancing pulse d16 3 (p1 ph1) ; start of ONESHOT p30:gp1*diff*cnst16 ;1 - alpha d16 p2 ph8 ;First 180 p30:gp1*-1*diff*cnst15 ;1 + alpha d16 p1 ph2 ; 2nd 90 p30:gp1*diff*2*cnst14 ;Lock refocusing pulse pulse d16 p19:gp2 ;Spoiler gradient balancing pulse d16 DELTA1 p30:gp1*diff*2*cnst14 ;Lock refocusing pulse pulse d16 p1 ph3 ; 3rd 90 p30:gp1*diff*cnst16 ; 1 - alpha d16 p2 ph8 p30:gp1*-1*diff*cnst15 ;1 + alpha d16 ; end of ONESHOT ; ; start of HSQC ; DELTA3 4u pl0:f2 (center (p2 ph8) (p14:sp3 ph9):f2 ) 4u pl2:f2 DELTA3 4u (p1 ph4) (p3 ph5):f2 d0 (p2 ph7) d0 p16:gp3*EA d17 4u pl0:f2 (p24:sp7 ph6):f2 4u pl2:f2 DELTA (ralign (p1 ph8) (p3 ph6):f2 ) DELTA4 pl0:f2 (center (p2 ph8) (p14:sp3 ph8):f2 ) 4u p16:gp4 DELTA2 pl12:f2 4u BLKGRAD ; end of HSQC ; go=2 ph31 cpd2:f2 d11 do:f2 mc #0 to 2 F2QF(calgrad(diff)) F1EA(calgrad(EA), caldel(d0, +in0) & calph(ph5, +180) & calph(ph9, +180) & calph(ph31, +180)) exit ph1=0 0 2 2 ph2=0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph3=0 0 0 0 2 2 2 2 ph4=1 ph5=0 2 ph6=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 ph7=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 ph8=0 ph9=0 ph21=0 ph22=1 ph31=0 2 2 0 2 0 0 2 2 0 0 2 0 2 2 0 2 0 0 2 0 2 2 0 0 2 2 0 2 0 0 2 0 2 2 0 2 0 0 2 2 0 0 2 0 2 2 0 2 0 0 2 0 2 2 0 0 2 2 0 2 0 0 2 ;pl0 : 0W ;pl1 : f1 channel - power level for pulse (default) ;pl2 : f2 channel - power level for pulse (default) ;pl12: f2 channel - power level for CPD/BB decoupling ;p1 : f1 channel - 90 degree high power pulse ;p2 : f1 channel - 180 degree high power pulse ;p3 : f2 channel - 90 degree high power pulse ;p4 : f2 channel - 180 degree high power pulse ;p8 : f1 channel - spherical randomization high power pulse [1.5 msec] ;p14: f2 channel - 180 degree shaped pulse for inversion ;p24: f2 channel - 180 degree shaped pulse for refocussing ;p16: gradient encode/decode (HSQC) ;p19: gradient pulse 2 (spoil gradient) [1.2 msec] ;p30: gradient pulse (little DELTA*0.5) ;spnam3: f2 channel - shaped pulse for refocussing ;spnam7: f2 channel - shaped pulse for inversion ;spnam15: f2 channel - shaped pulse cpd2 ;d0 : incremented delay (2D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d4 : 1/(4J)XH ;d11: delay for disk I/O [30 msec] ;d16: delay for gradient recovery (Oneshot) ;d17: delay for gradient recovery (HSQC) ;d18: delay for gradient recovery (Spherical randomization) [2 msec] ;d20: diffusion encoding period (big DELTA) ;cnst2: = J(XH) ;cnst50: sweep-width [kHz] ;cnst51: duration of the low-level W40 pulse [us] ;cnst53: adiabaticity factor of the low-level W40 pulse [Q=2.0] ;inf1: 1/SW(X) = 2 * DW(X) ;in0: 1/(2 * SW(X)) = DW(X) ;nd0: 2 ;ns: 2 * n ;ds: >= 16 ;td1: number of experiments HSQC ;td2: number of experiments Oneshot ;FnMODE(F1): echo-antiecho ;FnMODE(F2): QF ;cpd2: decoupling according to sequence defined by cpdprg2 ;pcpd2: f2 channel - 90 degree pulse for decoupling sequence ;use gradient ratio: gp 3 : gp 4 ; 80 : 20.1 for C-13 ; 80 : 8.1 for N-15 ;for z-only gradients: ;gpz1: 100% ;gpz2: 67% ;gpz3: 80% ;gpz4: 20.1% for C-13, 8.1% for N-15 ;use gradient files: ;gpnam1: SINE.100 ;gpnam2: SINE.100 ;gpnam3: SMSQ10.100 ;gpnam4: SMSQ10.100 ; Instructions for wavemaker: ;sp15(pcpd2,pl12):wvm:kp_W40:f2 cawurst-40(cnst50 kHz, cnst51 us; Q=cnst53 SUCYC=[p5]m4) ss=0.5us;