;hcch3_tocsy_ydw ;avance-version ;3D sequence with initial inept transfer, ;followed by multiple-quantum(HxCx) evolution for recording 13C chemical shift, ;TOCSY-transfer to methyl carbon (Cm), ; (spin-lock time = 94.224*p9*l1 us) ;constant-time acq mode for Cm chemical shift ; F2(C,t2) -> F1(Cm,t1) -> F3(Hm,t3) ; ; for samples in H2O solution, ajust p17 for better water suppression, ; but it should be less than 0.7ms since probe may not stand for longer time. ; ;phase sensitive using States-TPPI ; Yang et al., J. Am. Chem. Soc., 126. 3710(2004) #include #include #include "d0=3u" "d10=3u" "d20=13.8m" "d11=30m" "d12=20u" "d13=5u" "p2=p1*2" "p4=p3*2" "d4=1.6m" ;taud "d6=1.5m" ;tauc "d5=13.8m-d6-d13-p7-d0" ;bigT "d23=1.15m" ;taub "DELTA1=1.4m-p16-d16-4u-4*p1/3.1416" ;taua "DELTA2=1.4m-p16-d16-4u-p3" ;taua "DELTA3=d23-p29-d16-p14-p1" "DELTA4=d23-p29-d16" "DELTA6=d4-p18-d16-p3*2-7u+p1-p12/2" ;taud "DELTA7=d4-p18-d16-4u-p12/2" ;taud "TAU=(p3*2+3u)-p1" "CEN_HC1=(p3-p1)/2" "CEN_HC2=(p4-p2)/2" "CEN_HC3=(p12-p2)/2" "CEN_HN1=(p14-p2)/2" "CEN_HN2=(p14-p22)/2" "in20=in0" "l3=(td1/2)" "l13=(td2/2)" aqseq 321 1 d11 ze d11 pl12:f2 2 d11 do:f2 d11 3 d11 4 d11 5 d11 6 d1 50u UNBLKGRAD d12 pl1:f1 fq2:f2 (p1 ph1) 4u p16:gp1 d16 DELTA1 pl2:f2 (CEN_HC2 p2 ph1):f1 (p4 ph1):f2 4u p16:gp1 d16 DELTA2 pl3:f3 (p3 ph3):f2 d10 pl0:f2 (CEN_HN1 p2 ph10):f1 (p14:sp5 ph8):f2 (CEN_HN2 p22 ph1):f3 d10 (p1 ph2):f1 p29:gp2 d16 pl2:f2 DELTA3 (CEN_HC2 p2 ph1):f1 (p4 ph1):f2 p29:gp2 d16 DELTA4 (p3 ph2):f2 (p1 ph2):f1 p20:gp5 d16 pl15:f2 7 (p9*0.511 ph14):f2 (p9*1.067 ph16):f2 (p9*1.822 ph17):f2 (p9*1.767 ph28):f2 (p9*1.444 ph15):f2 (p9*1.767 ph28):f2 (p9*1.822 ph17):f2 (p9*1.067 ph16):f2 (p9*0.511 ph14):f2 (p9*0.511 ph22):f2 (p9*1.067 ph24):f2 (p9*1.822 ph25):f2 (p9*1.767 ph20):f2 (p9*1.444 ph23):f2 (p9*1.767 ph20):f2 (p9*1.822 ph25):f2 (p9*1.067 ph24):f2 (p9*0.511 ph22):f2 (p9*0.511 ph22):f2 (p9*1.067 ph24):f2 (p9*1.822 ph25):f2 (p9*1.767 ph20):f2 (p9*1.444 ph23):f2 (p9*1.767 ph20):f2 (p9*1.822 ph25):f2 (p9*1.067 ph24):f2 (p9*0.511 ph22):f2 (p9*0.511 ph14):f2 (p9*1.067 ph16):f2 (p9*1.822 ph17):f2 (p9*1.767 ph28):f2 (p9*1.444 ph15):f2 (p9*1.767 ph28):f2 (p9*1.822 ph17):f2 (p9*1.067 ph16):f2 (p9*0.511 ph14):f2 (p9*0.511 ph14):f2 (p9*1.067 ph16):f2 (p9*1.822 ph17):f2 (p9*1.767 ph28):f2 (p9*1.444 ph15):f2 (p9*1.767 ph28):f2 (p9*1.822 ph17):f2 (p9*1.067 ph16):f2 (p9*0.511 ph14):f2 (p9*0.511 ph14):f2 (p9*1.067 ph16):f2 (p9*1.822 ph17):f2 (p9*1.767 ph28):f2 (p9*1.444 ph15):f2 (p9*1.767 ph28):f2 (p9*1.822 ph17):f2 (p9*1.067 ph16):f2 (p9*0.511 ph14):f2 (p9*0.511 ph22):f2 (p9*1.067 ph24):f2 (p9*1.822 ph25):f2 (p9*1.767 ph20):f2 (p9*1.444 ph23):f2 (p9*1.767 ph20):f2 (p9*1.822 ph25):f2 (p9*1.067 ph24):f2 (p9*0.511 ph22):f2 (p9*0.511 ph22):f2 (p9*1.067 ph24):f2 (p9*1.822 ph25):f2 (p9*1.767 ph20):f2 (p9*1.444 ph23):f2 (p9*1.767 ph20):f2 (p9*1.822 ph25):f2 (p9*1.067 ph24):f2 (p9*0.511 ph22):f2 lo to 7 times l1 (p17 ph1):f1 3u (p17*2 ph2) 4u p30:gp4 d16 fq2:f2 (p1 ph1) 4u p31:gp4 d16 pl2:f2 pl19:f1 (p7 ph7):f1 d13 cpds1:f1 ph1 (p3 ph4):f2 d20 pl0:f2 (p13:sp2 ph6):f2 d0 d5 pl2:f2 d13 do:f1 (p7 ph9):f1 d6 pl1:f1 (CEN_HC1 p1 ph1) (p3 ph1):f2 4u p18:gp1 d16 DELTA7 pl0:f2 (CEN_HC3 p2 ph1) (p12:sp1 ph1):f2 4u p18:gp1 d16 DELTA6 pl2:f2 (TAU p1 ph1) (p3 ph1 3u p3 ph5):f2 4u pl12:f2 4u BLKGRAD go=2 ph31 cpd2:f2 d11 do:f2 wr #0 if #0 zd d11 ip4 lo to 3 times 2 15m id0 ip31*2 15m dd20 lo to 4 times l3 15m rd0 ip3 15m rd20 lo to 5 times 2 d11 id10 ip31*2 lo to 6 times l13 exit ph1=0 ph2=1 ph3=0 0 0 0 2 2 2 2 ph4=1 ph5=0 0 0 0 2 2 2 2 ph6=0 0 1 1 2 2 3 3 ph7=1 ph8=0 0 2 2 ph9=3 ph10=0 1 2 3 ph14=(16) 0 ph15=(16) 1 ph16=(16) 2 ph17=(16) 3 ph18=(16) 4 ph19=(16) 5 ph20=(16) 6 ph21=(16) 7 ph22=(16) 8 ph23=(16) 9 ph24=(16) 10 ph25=(16) 11 ph26=(16) 12 ph27=(16) 13 ph28=(16) 14 ph29=(16) 15 ph31=0 2 2 0 2 0 0 2 ;pl0 : 120dB ;Channel f1 ;pl1: power level for hard high power pulse ;p1: 90 degree high power pulse ;p2: 180 degree high power pulse ;pl19: power level for 1H decoupling ;p7; 90 degree flank pulse @pl19 (40us) ;p17: trim pulse[~0.5ms for H2O sample,adjustable; ~p1 for D2O sample] ;cpd1: defined by cpdprg1 (DIPSI2) ;pcpd1: 90 degree pulse (40us) ;Channel f2 ;pl2: power level for hard high power pulse ;p3: 90 degree high power pulse ;p4:180 degree high power pulse ;pl12: power level for CPD/BB decoupling ;pl15: power level for TOCSY-spinlock ;p9 : 90 degree TOCSY power pulse ; (~36us @500 MHz; ~33us @600 MHz; ~30us @800 MHz) ;sp1: power level for shaped pulse 180 degree ;p12: 180 degree shaped pulse @sp1 (REBURP, 1500 us@500MHz) ; (~1500us x 500/y, y is the spectrometer frequency in MHz) ;spoff1: offset for sp1 [0] ;sp2: power level for shaped pulse 180 degree ;p13: 180 degree shaped pulse @sp1 (REBURP, 400 us@500MHz) ; (~400us x 500/y, y is the spectrometer frequency in MHz) ;spoff2: offset for sp2 [21ppm x spectrometer frequency, centered at 38ppm] ;sp5: power level for shaped pulse 180 degree ) ;p14: 180 degree shaped pulse @sp1 (SEDUCE, 250 us@500MHz) ; (~250us x 500/y, y is the spectrometer frequency in MHz) ;spoff5: offset for sp5 [135ppm x spectrometer frequency, centered at 176ppm] ;cpd2: defined by cpdprg2 (WALTZ16) ;pcpd2: 90 degree pulse (200us) ;O2p: 17ppm ;FQ2LIST: first at 41 ppm (or 39ppm) and second at 17ppm ;Channel f3 ;pl3: power level for hard high power pulse (120dB without 15N labeling) ;p22: 180 degree high power pulse ;Gradients ;gpnam1: SINE.50 ;gpnam2: SINE.50 ;gpnam4: SINE.50 ;gpnam5: SINE.50 ;p16: gradient pulse 1 @gpz1,[500 usec] ;gpz1: 40% ;p18: gradient pulse 5 @gpz1,[300 usec] ;p20: gradient pulse 3 @gpz5,[1000 usec] ;gpz5: -65% ;p29: gradient pulse 2 @gpz2,[300 usec] ;gpz2: 50% ;p30: gradient pulse 4 @gpz4,[2500 usec] ;gpz4: 60% ;p31: gradient pulse 4'@gpz4,[2200 usec] ;Other parameters ;d0 : incremented delay (F1 in 3D) [3 usec] ;d4 : ~1/(4J(CH)) - taud [1.6 msec] ;d10: incremented delay (F2 in 3D) [3 usec] ;d11: delay for disk I/O [30 msec] ;d12: delay for power switching [20 usec] ;d16: delay for gradient recovery (100us) ;d23: tau b [475 usec] ;l1: loop for DIPSI cycle: ; mixing time = (p9*94.224*p9) * l1) [17 msec] ;l3: loop for phase sensitive 3D using States-TPPI : l3 = td1/2 ;l13: loop for phase sensitive 3D using States-TPPI : l13 = td2/2 ;in0: 1/(2 * SW(Cm)) = DW(Cm) ;nd0: 2 ;in10: 1/(2 * SW(C)) = DW(C) ;nd10: 2 ;NS: 4 * n ;DS: 32 ;td1: number of experiments in F1 ;td2: number of experiments in F2 ;MC2: States-TPPI in F1 ;MC2: States-TPPI in F2