; B_n_i+1 old name: maasnco.pub+/ MA_n_i+1 ; Asparagine selective 15N/1H correlation of the (i+1) residues ; using WATERGATE as water suppression ; phase sensitive with TPPI-States ; last modified by Mario 11.01.2001 ; ref: M. Schubert, M. Smalla, P. Schmieder and H. Oschkinat ; J. Magn. Reson. 1999, 141, 34-43. ; note that this sequence contains 3 gradients in the MUSIC element ; to have an absolutely clean selection, this is an improvement of the ; sequence in the paper! #include ;; PULSES "p2 =2.0*p1" "p6 =2.0*p5" ;;DELAYS "d11 = d1/3" "d12 = 20u" "d13 = 3u" "d5 = 5u" "d0 = 11m" "d15 = (p8 - p2 - d13)/2" "CP4P2 = (p4-p2)/2" "CP3P2 = (p3-p2)/2" "CP6P4 = (p6-p4)/2" "CP5P2 = (p5-p2)/2" "CP8P6 = (p8-p6)/2" "CP10P6 = (p10-p6)/2" "TAU1 = 5.5m - p22 - d22 - d15 -50u" "TAU2 = 2.25m - p21 - d21 - 1.69*d3" "TAU3 = (d3-p6)/2" "TAU4 = 5.5m - p22 - d22 - d15" "TAU5 = TAU4 - 2*d12" "TAU = 5.5m" "DELTA1 = 8m" "DELTA3 = 4.5m" "DELTA4 = 4.5m" "DELTA6 = 11.4m" "DELTA5 = DELTA6 - DELTA4 - p12" "DELTA7 = 22m - TAU - d12 - p19 + p8" "DELTA8 = 11m - p12 - 3u" "l0 = td1/2" 1 ze d12 pl2:f2 d12 fq2:f2 d11 d12 fq2:f2 2 d11 do:f3 3 d11 d11 4 d12 pl3:f3 (p1 ph1):f1 ;--------------------- d15 50u UNBLKGRAD GRADIENT_A(cnst22) d22 TAU1 (CP5P2 p2 ph1):f1 (p5 ph5):f3 TAU4 GRADIENT_A(cnst22) d22 (d15 p1 ph11 d13 p1 ph12):f1 (p8:sp8 ph1):f2 (CP8P6 p6 ph1):f3 d22 GRADIENT_A(cnst22) TAU5 d12 pl19:f1 (d12 cpds1 ph1):f1 DELTA1 (p8:sp8 ph1):f2 (CP8P6 p6 ph1):f3 DELTA1 (p5 ph1):f3 ;---------------------------------------------------------------------------- d13 (p7:sp7 ph1):f2 ; 54u on-res. DELTA6 (p8:sp8 ph1):f2 (CP8P6 p6 ph1):f3 ; 108u on-res. DELTA5 (p12:sp12 ph1):f2 ; 48u -18000 off DELTA4 (p7:sp7 ph4):f2 ; 54u on-res. d12 fq2:f2 ; jump to ca (p3:sp3 ph9):f2 ; 49u on-res. DELTA3 (p10:sp10 ph1):f2 ; 202u sinc 19500 off d13 (p4:sp4 ph1):f2 ; 44u on-res. DELTA3 (p10:sp10 ph1):f2 ; Bloch-Siegert d13 ;----------------------------------------------------------------------------- (p3:sp3 ph1):f2 ; 49u on-res. d13 (p10:sp10 ph1):f2 ; Bloch-Siegert DELTA3 (p4:sp4 ph1):f2 ; 44u on-res. d13 (p10:sp10 ph1):f2 ; 202u sinc 19500 off DELTA3 (p3:sp3 ph1):f2 ; 49u on-res. d12 fq2:f2 ; jump to carbonyl (p7:sp7 ph6):f2 ; 54u on-res. DELTA4 (p12:sp12 ph1):f2 ; 48u -18000 off DELTA5 (p8:sp8 ph1):f2 (CP8P6 p6 ph1):f3 ; 108u on-res. DELTA6 (p7:sp7 ph7):f2 ; 54u on-res. d13 (p5 ph15):f3 (DELTA7 d12 do p19 ph17 TAU):f1 (d0 p8:sp8 ph1 DELTA8 p12:sp12 ph1):f2 (d0 CP8P6 p6 ph8):f3 (p5 ph1):f3 50u GRADIENT_B(cnst23) d22 pl10:f1 (p15:sp1 ph14):f1 d13 d12 pl1:f1 (p1 ph1):f1 50u WTGGRAD(cnst21) d21 TAU2 p1*0.231 ph2 d3 p1*0.692 ph2 d3 p1*1.4621 ph2 TAU3 (p6 ph1):f3 TAU3 p1*1.4621 ph3 d3 p1*0.692 ph3 d3 p1*0.231 ph3 45u WTGGRAD(cnst21) d21 5u BLKGRAD TAU2 pl16:f3 d5 cpd3:f3 d5 ph10 aq adc ph31 syrec rcyc=2 d11 do:f3 wr #0 if #0 ip15 zd lo to 3 times 2 d11 dd0 ip31 d11 ip31 lo to 4 times l0 exit ph1 = 0 ph2 = 1 ph3 = 3 ph4 = (360) 310 ph5 = 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 ph6 = 0 2 ph7 = (360) 50 ph8 = 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 3 3 3 3 3 3 3 3 ph9 = 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 ph16 = 1 ph17 = 3 3 3 3 1 1 1 1 ph14 = 2 ph10 = (360) 0 ph11 = (360) 0 ph12 = (8) 1 1 3 3 5 5 7 7 ph13 = 0 ph15 = 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 2 0 0 2 2 0 0 2 0 2 2 0 0 2 2 0 0 2 2 0 0 2 2 0 2 0 0 2 2 0 0 2 ; PARAMETER ;p1 :90 deg pulse 1H (power pl1) ;p3 :90 deg pulse 13Cab on-resonance (:sp3) ;p4 :180 deg pulse 13Cab on-resonance (:sp4) ;p5 :90 deg pulse 15N (power pl3) ;p7 :90 deg pulse 13CO on-resonance (:sp7) ;p8 :180 deg pulse 13CO on-resonance (:sp8) ;p10 :180 deg pulse 13CO at 19500 Hz (:sp10) ;p12 :180 deg pulse 13Ca at -18000 Hz (:sp12) ;p15 :water flip back pulse (1000u; sp1) ;p19 :90 deg 1H decoupling pulse (80u; pl19) ;pcpd1 :90 deg 1H decoupling pulse (80u; pl19) ;pcpd3 :90 deg 15N decoupling pulse at pl16 ;CPDPRG3 = cpd program, use "garp" (NOT ASKED IN "ASED" !!) ;d1 :total relaxation delay ;d3 :WATERGATE d. (proteins: 210u at 600MHz) ;l0 :number of complex points in F1 ;pl1 :high power for protons ;pl2 :dummy power for carbon (120 dB) ;pl3 :high power for nitrogen ;pl10 :dummy power (120 dB) ;pl16 :power for 15N cpd-decoupling ;pl19 :power for 1H cpd-decoupling ;GRDPRROG = ma4crushwtg.r (NOT ASKED IN "ASED" !!) ;p21 :watergate gradient (1 msec) ;d21 :recovery for p21 (500 usec) ; set cnst21 = 30 (NOT ASKED IN "ASED" !!) ;p22 :first crusher gradient (0.8 msec) ;d22 :recovery for p22 (500 usec) ; set cnst22 = 10 (NOT ASKED IN "ASED" !!) ;p23 :second crusher gradient (0.8 msec) ;d23 :recovery for p23 (500 usec) ; set cnst23 = 40 (NOT ASKED IN "ASED" !!) ;FQ2LIST = pscbcaconh (NOT ASKED IN "ASED" !!) ;ns :number of scans (ns*64) ;***** Sample Gradient File *************** ;p22 { (0) | (0) | (0)+sin(cnst22,100) } ;40u { (0) | (0) | (0) } ; { (0) | (0) | (0) } ;p22 { (0) | (0) | (0)+sin(cnst22,100) } ;40u { (0) | (0) | (0) } ; { (0) | (0) | (0) } ;p22 { (0) | (0) | (0)+sin(cnst22,100) } ;40u { (0) | (0) | (0) } ; { (0) | (0) | (0) } ;p23 { (0) | (0) | (0)+sin(cnst23,100) } ;40u { (0) | (0) | (0) } ; { (0) | (0) | (0) } ;p21 { (0) | (0) | (0)+sin(cnst21,100) } ;40u { (0) | (0) | (0) } ; { (0) | (0) | (0) } ;p21 { (0) | (0) | (0)+sin(cnst21,100) } ;40u { (0) | (0) | (0) } ; { (0) | (0) | (0) } ;***** SAMPLE FREQUENCE LIST FILE *************** ;O 150.902749 ;BF ;6500 ;alpha/beta region 45ppm ;26000 ;carbonyl 175ppm