;Pulse Program Code for Bruker: ;pp:hobs_hsqc_tocsy_cpd ;2D Experiment ;HOmodecoupled Band-Selective of refocused F2-decoupled HSQC-TOCSY experiment ;2D H-1/X correlation via double inept transfer ; using sensitivity improvement ; using DIPSI2 for homonuclear Hartman-Hahn mixing ; using trim pulses in inept transfer ; using shaped pulses for all 180 degree inversion pulses on f2 channel ; phase sensitive using Echo/Antiecho-TPPI gradient selection ; with decoupling during acquisition ;Modified by Laura Castaņar (10/11/2014) ;original: hobs_hsqc_cpd ;L. Castaņar, P. Nolis, A. Virgili & T. Parella, ; Chem. Eur. J (2015)21,7682-7685 ; DOI:10.1002/chem.201500521 ;Avance III version (10/11/2014) ;Topspin3.1 #include #include #include #include #define hobs "p2=p1*2" "p4=p3*2" "d11=30m" "d4=1s/(cnst2*4)" "d21=d4*2" "d0=3u" "in0=inf1/2" "FACTOR1=(d9/(p6*115.112))/2" "l1=FACTOR1*2" "DELTA1=p16+d16-p1*0.78+de+8u" "DELTA2=d4-p14/2" "DELTA=p16+d16+p2+d0*2" "DELTA4=d21-p2+p3*2/PI" "DELTA5=d21-p16-d16-p2-d0*2-p3*2/PI" #ifdef hobs dwellmode explicit "d2=aq/l0" "d3=d2/2" "l2=l0-1" #else #endif "acqt0=0" baseopt_echo 1 ze d11 pl12:f2 2 d1 do:f2 10u pl0:f2 #ifdef hobs 10u pl0:f1 3 (p11:sp1 ph1):f1 #else 10u pl1:f1 3 (p1 ph1) #endif DELTA2 pl1:f1 4u (center (p2 ph1) (p14:sp3 ph6):f2 ) 4u DELTA2 pl2:f2 UNBLKGRAD p28 ph1 4u (p1 ph2) (p3 ph3):f2 d0 (p2 ph7) d0 if "cnst24==0" { p16:gp1*EA d16 (p4 ph4):f2 DELTA } else { p16:gp1*EA d16 pl0:f2 DELTA5 (p31:sp18 ph1):f2 (p2 ph1) DELTA4 4u (p31:sp18 ph1):f2 4u pl2:f2 } (center (p1 ph1) (p3 ph4):f2 ) d24 (center (p2 ph1) (p4 ph1):f2 ) d24 (center (p1 ph2) (p3 ph5):f2 ) DELTA2 pl0:f2 (center (p2 ph1) (p14:sp3 ph1):f2 ) DELTA2 pl10:f1 ;begin DIPSI2 4 p6*3.556 ph22 p6*4.556 ph24 p6*3.222 ph22 p6*3.167 ph24 p6*0.333 ph22 p6*2.722 ph24 p6*4.167 ph22 p6*2.944 ph24 p6*4.111 ph22 p6*3.556 ph24 p6*4.556 ph22 p6*3.222 ph24 p6*3.167 ph22 p6*0.333 ph24 p6*2.722 ph22 p6*4.167 ph24 p6*2.944 ph22 p6*4.111 ph24 p6*3.556 ph24 p6*4.556 ph22 p6*3.222 ph24 p6*3.167 ph22 p6*0.333 ph24 p6*2.722 ph22 p6*4.167 ph24 p6*2.944 ph22 p6*4.111 ph24 p6*3.556 ph22 p6*4.556 ph24 p6*3.222 ph22 p6*3.167 ph24 p6*0.333 ph22 p6*2.722 ph24 p6*4.167 ph22 p6*2.944 ph24 p6*4.111 ph22 lo to 4 times l1 ;end DIPSI2 4u pl1:f1 (p1 ph1) DELTA1 (p2 ph1) 4u p16:gp2 d16 pl12:f2 d12 cpd2:f2 #ifdef hobs ACQ_START(ph30,ph31) 0.05u DWL_CLK_ON 0.1u REC_UNBLK d3 0.05u DWL_CLK_OFF 0.1u REC_BLK d12 do:f2 p19:gp8 d16 pl1:f1 (p2 ph8):f1 p19:gp8 d16 p19:gp7 d16 pl0:f1 (p12:sp2 ph9):f1 p19:gp7 d16 5 d12 cpd2:f2 0.05u DWL_CLK_ON 0.1u REC_UNBLK d2:r 0.05u DWL_CLK_OFF 0.1u REC_BLK d12 do:f2 p19:gp8 d16 pl1:f1 (p2 ph8):f1 p19:gp8 d16 p19:gp7 d16 pl0:f1 (p12:sp2 ph9):f1 p19:gp7 d16 lo to 5 times l2 d12 cpd2:f2 0.05u DWL_CLK_ON 0.1u REC_UNBLK d3 15m 0.05u DWL_CLK_OFF 0.1u REC_BLK d12 do:f2 6 rcyc=2 #else go=2 ph31 #endif d1 do:f2 mc #0 to 2 F1EA(calgrad(EA) & calph(ph5, +180), caldel(d0, +in0) & calph(ph3, +180) & calph(ph6, +180) & calph(ph31, +180)) exit ph1=0 ph2=1 ph3=0 2 ph4=0 ph5=1 ph6=0 ph7=0 ph8=0 ph9=0 ph22=3 ph24=1 ph30=0 ph31=0 2 ;pl0 : 0W ;pl1 : f1 channel - power level for pulse (default) ;pl2 : f2 channel - power level for pulse (default) ;pl3 : f3 channel - power level for pulse (default) ;pl10: f1 channel - power level for TOCSY-spinlock ;pl12: f2 channel - power level for CPD/BB decoupling ;pl16: f3 channel - power level for CPD/BB decoupling ;sp1: f1 channel - shaped pulse power level for 90 degree band-selective excitation ;sp2: f1 channel - shaped pulse power level for 180 degree band-selective excitation ;sp3: f2 channel - shaped pulse power level for 180 degree for inversion ;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 ;p6 : f1 channel - 90 degree low power pulse ;p14: f2 channel - 180 degree shaped pulse for inversion [500 us] ;p16: homospoil/gradient pulse [1 msec] ;p19: homospoil/gradient pulse [500 us] ;p22: f3 channel - 180 degree high power pulse ;p28: f1 channel - trim pulse [1 msec] ;p31: f2 channel - 180 degree shaped pulse for refocusing[1730 us] ;d0 : incremented delay (2D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d4 : 1/(4J(XH)) ;d9 : TOCSY mixing time [60-90 ms] ;d11: delay for disk I/O [30 msec] ;d16: delay for homospoil/gradient recovery [20 usec] ;d24: 1/(8J)XH for all multiplicities ; 1/(4J)XH for XH ;cnst2: = J(XH) ;cnst24: = (0) conventional / (1) Multiplicity edited ;l1: loop for DIPSI cycle: ((p6*115.112) * l1) = mixing time ;l2: number of concatenated loops for homodecoupling ;inf1: 1/SW(X) = 2 * DW(X) ;in0: 1/(2 * SW(X)) = DW(X) ;nd0: 2 ;NS: 1 * n ;DS: >= 8 ;td1: number of experiments ;FnMODE: echo-antiecho ;spnam1: shaped pulse for 90 degree selective excitation [EBURP] ;spnam2: shaped pulse for 180 degree selective excitation [REBURP] ;spnam3: shaped pulse for 180 degree for inversion [Crp60,0.5,20.1] ;spnam18: shaped pulse for 180 degree for refocusing [Crp60_xfilt.2] ;cpd2: decoupling according to sequence defined by cpdprg2 ;pcpd2: f2 channel - 90 degree pulse for decoupling sequence ;use gradient ratio: gp 1 : gp 2 ; 80 : 20.1 for C-13 ; 80 : 8.1 for N-15 ;for z-only gradients: ;gpz1: 80% ;gpz2: 20.1% for C-13, 8.1% for N-15 ;gpz7: 63% ;gpz8: 41% ;use gradient files: ;gpnam1: SMSQ10.100 (Topspin3.1) ;gpnam2: SMSQ10.100 (Topspin3.1) ;gpnam7: SMSQ10.100 (Topspin3.1) ;gpnam8: SMSQ10.100 (Topspin3.1)