;noesyi4pr3d ;MANUFACTURER: Bruker ;MODEL: DMX ;AUTHOR: Charles G. Hoogstraten ;DESCRIPTION: avance-version ;BMRB Pulse Sequence Accession Number: 18 ;3D sequence with ; homonuclear correlation via dipolar coupling ; dipolar coupling may be due to noe or chemical exchange. ;phase sensitive using TPPI ;with decoupling during acquisition ;mod to states-tppi cgh 1/5/95 ;mod to BD-NOESY with gradients cgh 1/6/95 ;mod to CD-NOESY 3D cgh 1/31/95 ;Observe cross-relaxation between but not within spectral blocks ;H2O suppression accomplished with gradients and dephasing pulses ;Gradients used in coherence destruction pattern ;Proton Evolution--MENE(BD-NOESY) mixing--INEPT--15N Evolution-- ;Reverse INEPT--Acquire ;Excellent H2O suppression has been obtained, empirically optimize ;gradient strength ratios to optimize ;4-step phase cycle allows 128*x64*x4k in ca. 3 days ;Smaller number of NOE/ROE cycles (l7 counter) will increase S/N but will ;at some point reduce efficiency of editing effect ;Takes full advantage of buffered acquisition, dummy scans at ;beginning of experiment only ;pl11 = power to spin lock entire proton spectrum (use SW/2) ;d7 = precession delay = 1/(8*(gammab1/2pi for spin lock)) ;Setup of NOESY and ROESY delays: ;(1) To first approximation, ROESY delay (p15) is 0.5* NOESY delay (d3) ;For more precise cancellation, calculate ROESY contribution during soft pulse, ;and off-resonance effects on ROE in critical region of spectrum (b-methylenes ;in proteins) and set total cross-relaxation rate at that offset to zero ;(2) Desired "NOESY mixing time" is (d3 + 2.0*p15)*l7, or ; (d3 + (ROESY xrel rate)*p15)*l7 ; this procedure therefore ignores inter-block xrel during soft pulse ;(3) above two equations in two unknowns (p15, d3) may be solved ;uniquely for a given value of l7 #include #include p2=p1*2 ;Proton 180 p4=p3*2 ;Nitrogen 180 d11=30m d13=3u 1 d11 ze 2 d11 do:f2 3 d11 6 d11 7 d11 4 4u d1 pl2:f2 ;Relaxation delay p1 ph3 ;Proton 90 d0 p4:f2 ph0 d0 p1 ph0 GRADIENT(cnst21) ;dephase xy magn. prior to MENE mixing 8 d3 ;longitudinal cross-relaxation p11:sp1:f1 ph5:r ;selective inversion d12 pl1:f1 p1 ph5 ;move spins to transverse plane d7 ;precession delay p1 ph6 ;Griesinger/Ernst type trim pulse d12 pl11:f1 ;power for cw spinlock p15 ph6 ;ROESY, p15= (approx.) 0.5*d3 d12 pl1:f1 p1 ph6 ;trim pulse d7 p1 ph7 ;return spins to z axis d13 p11:sp1:f1 ph5:r ;re-parallelize blocks d12 pl1:f1 lo to 8 times l7 ;loop to total mixing time p1 ph0 GRADIENT(cnst22) ;correct for imperfect 180 d4 pl2:f2 ;d4=2.3 ms - length of grads 2, 5 (p4 ph0):f2 (p2 ph0) GRADIENT(cnst22) d4 p8 ph0 ;p8=1.0ms Messerle-type pulse d13 p1 ph1 GRADIENT(cnst23) ; zz-filter d9 ;settling time (p3 ph4):f2 d10 ;incremented nitrogen delay p2 ph0 d10 p3:f2 ph0 GRADIENT(cnst24) ;cnst24<0 zz-filter d9 p1 ph0 GRADIENT(cnst25) ;cnst25<0 180 correction d4 (p2 ph0) (p4 ph0):f2 GRADIENT(cnst25) d4 pl12:f2 p12 ph0 ;Messerle-type pulse, <>p8 to avoid refocusing d13 go=2 ph31 cpd2:f2 d11 do:f2 wr #0 if #0 ip3 zd lo to 3 times 2 d11 id0 ip31*2 ;States-TPPI in proton dim. lo to 6 times l6 d11 rd0 ip4 lo to 7 times 2 d11 id10 ip31*2 ;States-TPPI in nitrogen dim. lo to 4 times l4 exit ph0=0 ph1=1 ph2=2 ph3=0 0 2 2 ph4=0 2 ph5= 0 ph6= 1 ph7= 2 ph31=0 2 2 0 ;pl1 : f1 channel - power level for pulse (default) ;pl2 : f2 channel - power level for pulse (default) ;pl9 : f1 channel - power level for presaturation ;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 ;p31: - 90 degree pulse for decoupling sequence ;d0 : incremented delay (F1 in 3D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d10: incremented delay (F2 in 3D) [3 usec] ;d11: delay for disk I/O [30 msec] ;d12: delay for power switching [20 usec] ;d13: short delay [3 usec] ;cpd2: decoupling according to sequence defined by cpdprg2