;c_con_sq_bshd_hd_v3.rd ; ;avance-version (14/07/25) ;CON ;2D sequence with ; 13C detected correlation for triple resonance using ; inept transfer steps ; ; F1(C=O) -> F3(N,t1) -> F1(C=O,t2) ; ;on/off resonance 13C pulses using shaped pulses ;phase sensitive (t1) ;with bandselective homodecoupling ;(use parameterset ) ; ;J. Ying, F. Li, J.H. Lee & A. Bax, J. Biomol. NMR , - (2014) ;(L. Castañar, P. Nolis A. Virgili & T. Parella, ; Chem. Eur. J. 19, 17283-17286 (2013)) ;(J. Ying, J. Roche & A. Bax, J. Magn. Reson. 241, 97-102 (2014)) ;(J.O. Struppe, C. Yang, Y. Wang, R.V. Hernandez, L.M. Shamansky ; & L.J. Mueller, J. Magn. Reson. 236, 89-94 (2013)) ;W. Bermel, I. Bertini,L. Duma, I.C. Felli, L. Emsley, R. Pierattelli, ; P.R. Vasos, Angew. Chem. Int. Ed. 44, 3089-3092 (2005) ;(L. Duma, S. Hediger, A. Lesage & L. Emsley, ; J. Magn. Reson. 164, 187-195 (2003) ) ; ; (28/11/17 Rupashree Dass/ Enrico Corliano/Frans Mulder) ; con detection of fast hydrogen exchange, measured by loss of anitphase 2NyHz ; several references to Pelupessy should be given here ; ; change in v2: removed cnst50 and replaced by integer l4 ; ; change in v3: (fm 211217) switched off 15N decoupling during BASHD 13C pulses ; to avoid arcing ; ; remember to set l0 correctly for proper homo-dec ; ;$CLASS=HighRes ;$DIM=2D ;$TYPE= ;$SUBTYPE= ;$COMMENT= prosol relations= #include #include #include #include "p22=p21*2" "d11=30m" "d12=20u" "d22=4.5m" "d23=12.5m" "p29=300u" "d62=aq/(l0*2)" "d63=d62/2" "d0=3u" "in0=inf1/2" "DELTA=d0*2+p8" "DELTA1=d23/2-p12/2" "DELTA2=d23-d22-p12" ;CPMG-block parameters "DELTA5=d25/(2*l4)-p22/2" "spoff7=bf1*((cnst21/2+cnst22/2)/1000000)-o1" "spoff13=bf1*((cnst21/2+cnst22/2)/1000000)-o1" "spoff23=0" "spoff24=0" "spoff25=0" "spoff26=bf1*(cnst22/1000000)-o1" dwellmode explicit 1 ze d11 pl12:f2 2 d11 do:f2 do:f3 4u BLKGRAD d1 pl3:f3 d12 cpd2:f2 50u UNBLKGRAD (p11:sp23 ph1) d23 (center (p12:sp24 ph1) (p22 ph1):f3 ) d23 UNBLKGRAD (p11:sp25 ph2) p16:gp1 d16 ; magnetization here is 2C'zNz d11 do:f2 ; now we put 1H decoupling off ; here comes the compensatory waltz16 block of duration d25 # ifdef LABEL_REF 20u d25 4u # else 20u cpd2:f2 ph1 d25 4u do:f2 # endif ; here ends waltz and starts the CPMG block (p21 ph1):f3 # ifdef LABEL_REF 20u cpd2:f2 ph1 4 DELTA5 (p22 ph2):f3 DELTA5 lo to 4 times l4 20u do:f2 # else 20u 5 DELTA5 (p22 ph2):f3 DELTA5 lo to 5 times l4 20u # endif /*LABEL_REF*/ (p21 ph1):f3 ; here ends the CPMG block and a clean up gradient is given p16:gp5 d16 d12 cpd2:f2 ; resume decouple protons (p21 ph3):f3 d0 (p8:sp13 ph5) d0 (p22 ph1):f3 DELTA (p21 ph4):f3 (p11:sp23 ph1) d23 4u (center (p12:sp24 ph1) (p22 ph1):f3 ) d23 pl16:f3 4u cpd3:f3 ACQ_START(ph30,ph31) 0.1u REC_UNBLK 0.05u DWL_CLK_ON d63:r 0.05u DWL_CLK_OFF 0.1u REC_BLK 6 p29:gp2 d16 4u do:f3 (p24:sp7 ph1):f1 4u cpd3:f3 p29:gp2 d16 p29:gp3 d16 4u do:f3 (p12:sp24 ph6):f1 4u cpd3:f3 p29:gp3 d16 0.1u REC_UNBLK 0.05u DWL_CLK_ON d62:r 0.05u DWL_CLK_OFF 0.1u REC_BLK p29:gp2 d16 4u do:f3 (p24:sp7 ph1):f1 4u cpd3:f3 p29:gp2 d16 p29:gp3 d16 4u do:f3 (p12:sp24 ph6):f1 4u cpd3:f3 p29:gp3 d16 0.1u REC_UNBLK 0.05u DWL_CLK_ON d62:r 0.05u DWL_CLK_OFF 0.1u REC_BLK lo to 6 times l0 d62 rcyc=2 d11 do:f2 do:f3 mc #0 to 2 F1PH(calph(ph3, +90), caldel(d0, +in0)) exit ph1=0 ph2=1 ph3=0 2 ph4=0 0 0 0 2 2 2 2 ph5=0 0 2 2 ph6=2 ph30=0 ph31=0 2 0 2 2 0 2 0 ;pl1 : f1 channel - power level for pulse (default) ;pl3 : f3 channel - power level for pulse (default) ;pl12: f2 channel - power level for CPD/BB decoupling ;pl16: f3 channel - power level for CPD/BB decoupling ;sp7 : f1 channel - shaped pulse (180degree refocussing) ;spnam7: Crp60comp.4 (Crp80comp.4) ;sp13: f1 channel - shaped pulse 180 degree (adiabatic) ;sp23: f1 channel - shaped pulse 90 degree (on resonance) ;sp24: f1 channel - shaped pulse 180 degree (on resonance) ;sp25: f1 channel - shaped pulse 90 degree (on resonance) ; for time reversed pulse ;sp26: f1 channel - shaped pulse 180 degree (Ca off resonance) ;p8 : f1 channel - 180 degree shaped pulse for inversion (adiabatic) ;p11: f1 channel - 90 degree shaped pulse ;p12: f1 channel - 180 degree shaped pulse ;p16: homospoil/gradient pulse [1 msec] ;p21: f3 channel - 90 degree high power pulse ;p22: f3 channel - 180 degree high power pulse ;p24: f1 channel - 180 degree shaped pulse for refocussing ;p29: gradient pulse 3 [300 usec] ;d0 : incremented delay (F1 in 2D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d11: delay for disk I/O [30 msec] ;d12: delay for power switching [20 usec] ;d16: delay for homospoil/gradient recovery ;d22: 1/(4J(COCa)) [4.5 msec] ;d23: 1/(4J(NCO)) [12.5 msec] ;d25: length of total CPMG period ;d62: length of block between decoupling pulses : = aq/l0 [< 20-40 msec] ;d63: = d62/2 ;cnst21: CO chemical shift (offset, in ppm) ;cnst22: Calpha chemical shift (offset, in ppm) ;l4 : number of 15N 180 pulses during spin lock [2,4,8,16] ;l0 : number of blocks during acquisition time ; adjust to get d62 as required [8 msec] ;o1p: CO chemical shift (cnst21) ;inf1: 1/SW(N) = 2 * DW(N) ;in0: 1/(2 * SW(N)) = DW(N) ;nd0: 2 ;ns: 8 * n ;ds: >= 32 ;td1: number of experiments in F1 * 2 ;FnMODE: States-TPPI (or TPPI) in F1 ;cpd2: decoupling according to sequence defined by cpdprg2 ;cpd3: decoupling according to sequence defined by cpdprg3 ;pcpd2: f2 channel - 90 degree pulse for decoupling sequence ;pcpd3: f3 channel - 90 degree pulse for decoupling sequence ;zgoptns: specify ZGOPTNS = -DLABEL_REF for 1H decoupling during CPMG ;for z-only gradients: ;gpz1: 50% ;gpz2: 5% ;gpz3: 3% ;use gradient files: ;gpnam1: SMSQ10.100 ;gpnam2: SMSQ10.100 ;gpnam3: SMSQ10.100 ;preprocessor-flags-start ;LABEL_REF: when this is defined in ZGOPTNS then a referennce experiment is executed ; option -DLABEL_REF (eda: ZGOPTNS) ;$Id: c_con_sq_bshd,v 1.1 2014/08/22 13:46:21 ber Exp $