;hncocogp3d1 (19/01/2014) ;avance-version (12/01/11) ;(HN)CO(CO)NH ;3D sequence with ; inverse correlation for triple resonance using multiple ; inept transfer steps and C-C MOCCA-XY16 spinlock ; ; F1(H) -> F3(N) -> F2(C=O,t1) -> F2(C=O, TOCSY) ; -> F3(N,t2) -> F1(H,t3) ; ;on/off resonance Ca and C=O pulses using shaped pulse ;phase sensitive (t1) ;phase sensitive using Echo/Antiecho gradient selection (t2) ;using semi-constant time in t1 for high resolution in IDPs ;using semi-constant time in t2 for high resolution in IDPs ;(use parameterset HNCOCOGP3D) ; ;S. Grzesiek & A. Bax, J. Biomol. NMR 9, 207-211 (1997) ;J.-S. Hu & A. Bax, J. Am. Chem. Soc. 118, 8170-8171 (1996) ;F.A.A. Mulder, R. Otten & R.M. Scheek, J. Biomol. NMR 51, ; 199-207 (2011) ;J. Furrer, F. Kramer, J.P. Marino, S.J. Glaser & B. Luy, J. ; Magn. Reson. 166, 39-46 (2004) ;I.C. Felli, R. Pierattelli, S.J. Glaser & B. Luy, J. Biomol. ; NMR 43, 187-196 (2009) ;Yoshimura Y, Kulminskaya NV, Mulder FAA. ; J Biomol NMR. 2015 Feb;61(2):109-21. doi: 10.1007/s10858-014-9890-7. ; ; (fm 14/11/13 added additional gradient in SE part for artifact suppression) ; (yy 07/01/14 implemented t1 (C') evolution as a semi-CT evolution) ; (yy 07/01/14 implemented t2 (15N) evolution as a semi-CT evolution) ; (yy 07/01/14 changed the isotropic mixing scheme from DIPSI3 to MOCCA-XY16) ; ;$CLASS=HighRes ;$DIM=3D ;$TYPE= ;$SUBTYPE= ;$COMMENT= prosol relations= #include #include #include "p2=p1*2" "p22=p21*2" "d11=30m" "d21=5.5m" "d23=13.5m" "d26=2.3m" "d27=d26-d16-p16-4u" "p17=p16*0.101" "p9=1.732/(4*(o2-cnst22*bf2/1000000))" ; MOCCA-XY16 pulse length "plw15=plw2*(pow((p3/p9),2))" ; MOCCA-XY16 power level "cnst11=d9/p9" "cnst12=(o2/bf2-cnst22)/(1.732*(cnst11+1))"; Maximum offset (in ppm) "d0=3u" "d10=3u" "d20=d23+3u" "d28=3u" "d29=3u" "d30=d23+3u" "in0=inf1/2" "FACTOR1=d23*10000000*2/td1" "in20=FACTOR1/10000000" "in28=larger(in0,in20)-in20" "in20=in0+in28" "FACTOR2=d23*10000000*2/td2" "in10=FACTOR2/10000000" "in29=larger(inf2/2,in10)-in10" "in10=inf2/2-in29" "in30=in10" "DELTA1=p17+d16+8u" "DELTA2=d23-d21-p26" "DELTA3=d23-p22" "DELTA4=d21-p16-d16-4u" "DELTA5=d23-d21-p26-p14*2-10u" "d31=(p9*2+d9*2)*16*l1" "spoff2=0" "spoff3=0" "spoff5=bf2*(cnst22/1000000)-o2" "spoff8=0" aqseq 321 1 d11 ze d31 pl16:f3 2 d11 do:f3 3 d1 pl1:f1 pl2:f2 pl3:f3 20u UNBLKGRAD (center (p3 ph1):f2 (p21 ph1):f3 ) 4u p16:gp3 d16 pl0:f2 p1 ph1 d26 (center (p2 ph1) (p22 ph1):f3 ) d26 (p1 ph2):f1 4u pl0:f1 (p11:sp1 ph1:r):f1 4u p16:gp1 d16 (p21 ph3):f3 d21 pl19:f1 (p26 ph2):f1 DELTA2 cpds1:f1 ph1 (center (p14:sp3 ph1):f2 (p22 ph1):f3 ) d23 (p21 ph1):f3 4u do:f1 (p26 ph7):f1 4u p16:gp6 d16 (p26 ph2):f1 4u cpds2:f1 ph1 (p13:sp2 ph4):f2 d0 (p14:sp5 ph1):f2 DELTA3 (p22 ph1):f3 d28 (p14:sp3 ph1):f2 d20 (p14:sp5 ph1):f2 3u (p13:sp8 ph2):f2 4u do:f1 (p26 ph7):f1 4u p16:gp7 ;begin MOCCA-XY16 4 d9 pl15:f2 (p9*2 ph21):f2 d9*2 (p9*2 ph22):f2 d9*2 (p9*2 ph21):f2 d9*2 (p9*2 ph22):f2 d9*2 (p9*2 ph22):f2 d9*2 (p9*2 ph21):f2 d9*2 (p9*2 ph22):f2 d9*2 (p9*2 ph21):f2 d9*2 (p9*2 ph23):f2 d9*2 (p9*2 ph24):f2 d9*2 (p9*2 ph23):f2 d9*2 (p9*2 ph24):f2 d9*2 (p9*2 ph24):f2 d9*2 (p9*2 ph23):f2 d9*2 (p9*2 ph24):f2 d9*2 (p9*2 ph23):f2 d9 lo to 4 times l1 ;end MOCCA-XY16 p16:gp9 d16 pl0:f2 (p13:sp2 ph2):f2 d23 (center (p14:sp3 ph1):f2 (p22 ph1):f3 ) d23 (p13:sp8 ph9):f2 4u p16:gp8 d16 (p26 ph2):f1 4u cpds1:f1 ph1 (p21 ph1):f3 d30 (center (p14:sp5 ph1):f2 (p22 ph1):f3 ) d29 (p14:sp3 ph1):f2 d10 (p14:sp5 ph1):f2 d29 DELTA5 4u do:f1 (p26 ph7):f1 4u p16:gp2*EA d16 DELTA4 pl1:f1 (center (p1 ph1) (p21 ph5):f3 ) 4u p16:gp4 d16 d27 (center (p2 ph1) (p22 ph1):f3 ) 4u d27 p16:gp4 d16 (center (p1 ph2) (p21 ph6):f3 ) 4u p16:gp5 d16 d27 (center (p2 ph1) (p22 ph1):f3 ) 4u d27 p16:gp5 d16 (p1 ph1) DELTA1 (p2 ph1) 4u p17:gp2 d16 pl16:f3 4u BLKGRAD go=2 ph31 cpd3:f3 d11 do:f3 mc #0 to 2 F1PH(calph(ph4, +90), caldel(d0, +in0) & caldel(d20, -in20) & caldel(d28, +in28)) F2EA(calgrad(EA) & calph(ph6, +180), caldel(d10, +in10) & caldel(d29, +in29) & caldel(d30, -in30)) exit ph1=0 ph2=1 ph3=0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph4=0 2 ph5=0 0 2 2 ph6=3 3 1 1 ph7=3 ph9=0 0 0 0 2 2 2 2 ph21=0 ph22=1 ph23=2 ph24=3 ph31=0 2 2 0 2 0 0 2 2 0 0 2 0 2 2 0 ;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) ;pl15: f2 channel - power level for MOCCA-XY16 ;pl16: f3 channel - power level for CPD/BB decoupling ;pl19: f1 channel - power level for CPD/BB decoupling ;sp1: f1 channel - shaped pulse 90 degree (H2O on resonance) ;sp2: f2 channel - shaped pulse 90 degree (C=O on resonance) ;sp3: f2 channel - shaped pulse 180 degree (C=O on resonance) ;sp5: f2 channel - shaped pulse 180 degree (Ca off resonance) ;sp8: f2 channel - shaped pulse 90 degree (C=O on resonance) ; for time reversed pulse ;p1 : f1 channel - 90 degree high power pulse ;p2 : f1 channel - 180 degree high power pulse ;p3 : f2 channel - 90 degree high power pulse ;p9 : f2 channel - 90 degree low power pulse ;p11: f1 channel - 90 degree shaped pulse [2 msec] ;p13: f2 channel - 90 degree shaped pulse ;p14: f2 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 ;p26: f1 channel - 90 degree pulse at pl19 ;d0 : incremented delay (F1 in 3D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d9 : delay in MOCCA-XY16 scheme (DELTA/2) ;d10: incremented delay (F2 in 3D) ;d11: delay for disk I/O [30 msec] ;d16: delay for homospoil/gradient recovery ;d20: decremented delay (F1 in 3D) ;d21: 1/(2J(NH) [5.5 msec] ;d23: 1/(4J(NCO) [13.5 msec] ;d26: 1/(4J'(NH) [2.3 msec] ;d28: incremented delay (F1 in 3D) ;d29: incremented delay (F2 in 3D) ;d30: decremented delay (F2 in 3D) ;d31: length of MOCCA-XY16 cycle as executed = (p9*2+d9*2)*16*l1 ;cnst11: d9/p9 ;cnst12: Maximum offset (in ppm) ;cnst21: CO chemical shift (offset, in ppm) ;cnst22: Calpha chemical shift (offset, in ppm) ;o2p: CO chemical shift (cnst21) ;l1: loop for MOCCA-XY16 cycle: ; mixing time = (p9*2+d9*2)*16*l1 ;inf1: 1/SW(CO) = 2 * DW(CO) ;inf2: 1/SW(N) = 2 * DW(N) ;in0: 1/(2 * SW(CO)) = DW(CO) ;nd0: 2 ;in10: = d23*2/td2 ;nd10: 2 ;in20: = d23*2/td1 ;in28: = inf1/2-in20 ;in29: = inf2/2-in10 ;in30: = in10 ;ns: 8 * n ;ds: >= 64 ;td1: number of experiments in F1 (t1 max > 1/2JNCO) ;td2: number of experiments in F2 (t2 max > 1/2JNCO) ;FnMODE: States-TPPI (or TPPI) in F1 ;FnMODE: echo-antiecho in F2 ;cpds1: decoupling according to sequence defined by cpdprg1 ;cpds2: decoupling according to sequence defined by cpdprg2 ;cpd3: decoupling according to sequence defined by cpdprg3 ;pcpd1: f1 channel - 90 degree pulse for decoupling sequence ;pcpd2: f1 channel - 90 degree pulse for decoupling sequence ;pcpd3: f3 channel - 90 degree pulse for decoupling sequence ;use gradient ratio: gp 1 : gp 2 : gp 3 : gp 4 : gp 5 : gp 6 : gp 7 : gp 8 : gp 9 ; 30 : 80 : 24 : 60 : 12 : 20 : 35 : 28 : 45 ;for z-only gradients: ;gpz1: 30% ;gpz2: 80% ;gpz3: 24% ;gpz4: 60% ;gpz5: 12% ;gpz6: 20% ;gpz7: 35% ;gpz8: 28% ;gpz9: 45% ;use gradient files: ;gpnam1: SINE.100 ;gpnam2: SINE.100 ;gpnam3: SINE.100 ;gpnam4: SINE.100 ;gpnam5: SINE.100 ;gpnam6: SINE.100 ;gpnam7: SINE.100 ;gpnam8: SINE.100 ;gpnam9: SINE.100 ;$Id: hncocogp3d,v 1.6.6.1 2012/01/31 17:56:27 ber Exp $