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cest_caconh.cw
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cest_caconh.cw
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;CA CEST, via (HA)CA(CO)NNH experiment
;
;based on (HA)CA(CO)NH, Jun 2012
;Proton-coupled in Ca-dimension
;Rephasing of Ca-Ha coupling prior to Ca evolution to give in-phase doublets
;Purging equm 13C magnetisation
;With Ca-selective refocusing pulse in rephasing element
;
;cbcaconhgp3d
;avance-version (07/06/20)
;CBCACONH
;3D sequence with
; inverse correlation for triple resonance using inept transfer steps
;
; F1(H) -> F2(Caliph.,t1 -> Ca) -> F2(C=O) -> 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-TPPI gradient selection (t2)
;using constant time in t1
;using constant time in t2
;(use parameterset CBCACONHGP3D)
;
;S. Grzesiek & A. Bax, J. Biomol. NMR 3, 185-204 (1993)
;(D.R. Muhandiram & L.E. Kay, J. Magn. Reson. B 103, 203-216 (1994))
;
;$CLASS=HighRes
;$DIM=3D
;$TYPE=
;$SUBTYPE=
;$COMMENT=
prosol relations=<triple>
#include<Avance.incl>
#include<Grad.incl>
#include<Delay.incl>
;list of CEST saturation frequencies
;first line in file should be zero, indicating the reference plane
;give values in Hz relative to sfo2
define list<frequency> C13sat = <$FQ1LIST>
"p2=p1*2"
"p22=p21*2"
"d11=30m"
"d12=20u"
"d4=1.7m" ;tau a [1/(4*J_CaHa)]
"d21=12.4m" ;T N
"d23=3.6m" ;T C
"d24=4.4m" ;tau d
"d25=5.5m" ;tau f
"d26=2.3m" ;tau g
"d27=12.4m" ;tau e
"d10=d21/2-p14/2"
"d29=d21/2-p14/2-p26-d25-4u"
"d30=d21/2-p14/2"
"in10=inf2/4"
"in29=in10"
"in30=in10"
"DELTA=d26-p16-d16-4u-larger(p1,p21)"
"DELTA1=d4-p16-d16-4u-p14/2"
"DELTA2=d23-p24/2+p14*2"
"DELTA3=d27-d24+4u"
"DELTA4=d25-p16-d16-4u"
"DELTA5=p16+d16+8u+de"
"DELTA6=d4-p24/2-p16-d16-4u"
"spoff2=0"
"spoff3=0"
"spoff5=bf2*((cnst21-cnst22)/1000000)"
"spoff7=bf2*((cnst22-cnst21)/1000000)"
"spoff8=0"
"spoff9=0"
; loop counter for 'reference'
"l2=1"
aqseq 312
1 ze
d11 pl16:f3
2 d11 do:f3
3 d11 fq=cnst22(bf ppm):f2 ; set transmitter to CA
; temperature compensation
if "l2==1"
{
4u LOCKH_ON
;4u fq=cnst19(bf ppm):f1 ; 1H on HA
4u pl8:f1
d18 cpds8:f1
4u do:f1
;4u fq=0:f1
4u LOCKH_OFF
}
; purge water before recycle delay
4u pl1:f1
4u UNBLKGRAD
p16:gp5*0.8
d16
(p1 ph1):f1
p16:gp5
d16
4u BLKGRAD
; recycle delay
d1
50u UNBLKGRAD
d12 pl1:f1 pl2:f2 pl3:f3
; purge eq'm 13C
(p3 ph1):f2
p16:gp5
d16
(p3 ph2):f2
p16:gp5*0.7
d16*2 pl0:f2
; begin main sequence
(p10:sp1 ph2):f1 ; WFD
4u pl1:f1
(p1 ph1):f1 ; HAy --> HAxCAz
4u
p16:gp6
d16
DELTA1
(center (p2 ph1):f1 (p14:sp3 ph1):f2 )
DELTA1
4u
p16:gp6
d16
(p1 ph2):f1
4u
p16:gp7 ; HAzCAz
d16
(p13:sp2 ph11):f2 ; HAzCAy --> CAx
4u
p16:gp8
d16
DELTA6
(center (p2 ph1):f1 (p24:sp9 ph1):f2 ) ; Ca-selective [Reburp]
DELTA6
4u
p16:gp8
d16
(p13:sp8 ph2):f2
4u
p16:gp4*0.7 ; CAz cleaning gradient
d16
; CEST
if "l2==1" goto 77
4u LOCKH_ON
4u C13sat:f2
; 4u fq=cnst19(bf ppm):f1 ; 1H on HA
4u pl8:f1 pl18:f2
d18 cpds8:f1 cw:f2 ph1
4u do:f1 do:f2
; 4u fq=0:f1
4u fq=cnst22(bf ppm):f2
4u LOCKH_OFF
77 4u pl1:f1 pl0:f2
p16:gp4 ; CAz cleaning gradient
d16
(p13:sp2 ph1):f2 ; CAy --> CAxCOz
DELTA2
(p14:sp5 ph1):f2 ; CO
4u
(p24:sp9 ph1):f2 ; Ca-selective [Reburp]
DELTA2
(p14:sp5 ph1):f2 ; CO
4u
(p13:sp8 ph2):f2
d12 pl19:f1
p16:gp1 ; CAzCOz
d16 fq=cnst21(bf ppm):f2 ; move transmitter to CO
(p26 ph2):f1
20u cpds1:f1 ph1
(p13:sp2 ph1):f2
d24
(p14:sp7 ph1):f2
DELTA3
(center (p14:sp3 ph1):f2 (p22 ph1):f3 )
d27
(p14:sp7 ph1):f2
4u
(p13:sp8 ph1):f2
(p21 ph12):f3
d30
(p14:sp7 ph1):f2
d30
(center (p14:sp3 ph1):f2 (p22 ph1):f3 )
d10
(p14:sp7 ph1):f2
d29
4u do:f1
(p26 ph7):f1
4u
p16:gp2*EA
d16
DELTA4 pl1:f1
(center (p1 ph1):f1 (p21 ph13):f3 )
4u
p16:gp9
d16
DELTA
(center (p2 ph1):f1 (p22 ph1):f3 )
DELTA
4u
p16:gp9
d16
(center (p1 ph2):f1 (p21 ph2):f3 )
4u
p16:gp10
d16
DELTA
(center (p2 ph1):f1 (p22 ph1):f3 )
DELTA
4u
p16:gp10
d16
(p1 ph1):f1
DELTA5
(p2 ph1):f1
4u
p16:gp3
d16 pl16:f3
4u BLKGRAD
go=2 ph31 cpd3:f3
d11 do:f3 mc #0 to 2
F1QF(C13sat.inc & iu2)
F2EA(ru2 & igrad EA & ip13*2, id10 & id29 & dd30 & ip12*2 & ip31*2)
; F1PH(rd10 & rd29 & rd30 & rp11 & rp31 & ip3, id0 & dd20)
exit
ph1=0
ph2=1
ph7=3
ph11=0 2
ph12=0 0 2 2
ph13=0
ph31=0 2 2 0
;pl0 : 120dB
;pl1 : f1 channel - power level for pulse (default)
;pl3 : f3 channel - power level for pulse (default)
;pl16: f3 channel - power level for CPD/BB decoupling
;pl19: f1 channel - power level for CPD/BB decoupling
;sp2: f2 channel - shaped pulse 90 degree (on resonance)
;sp3: f2 channel - shaped pulse 180 degree (on resonance)
;sp5: f2 channel - shaped pulse 180 degree (C=O off resonance)
;sp7: f2 channel - shaped pulse 180 degree (Ca off resonance)
;sp8: f2 channel - shaped pulse 90 degree (on resonance)
; for time reversed pulse
;sp9: f2 channel - Ca-selective shaped pulse 180 degree (Reburp.1000)
;p1 : f1 channel - 90 degree high power pulse
;p2 : f1 channel - 180 degree high power pulse
;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
;p24: f2 channel - Ca-selective 180 degree shaped pulse
;p26: f1 channel - 90 degree pulse at pl19
;d1 : relaxation delay; 1-5 * T1
;d3 : tau b : 1.1m-p14
;d4 : 1/(4J(CH)) - tau a [1.7 msec]
;d10: incremented delay (F2 in 3D) = d21/2-p14/2
;d11: delay for disk I/O [30 msec]
;d12: delay for power switching [20 usec]
;d16: delay for homospoil/gradient recovery
;d21: T(N) [12.4 msec]
;d22: T(C) [3.6 msec]
;d23: tau c [3.6 msec]
;d24: tau d [4.4 msec]
;d25: tau f [5.5 msec]
;d26: 1/(4J(NH)) - tau g [2.3 msec]
;d27: tau e [12.4 msec]
;d29: incremented delay (F2 in 3D) = d21/2-p14/2-p26-d25-4u
;d30: decremented delay (F2 in 3D) = d21/2-p14/2
;cnst21: CO chemical shift (offset, in ppm) [174 ppm]
;cnst22: Calpha chemical shift (offset, in ppm) [55 ppm]
;o2p: Calpha chemical shift (cnst22) [55 ppm]
;inf2: 1/SW(N) = 2 * DW(N)
;in10: 1/(4 * SW(N)) = (1/2) DW(N)
;nd10: 4
;in29: = in10
;in30: = in10
;NS: 4 * n
;DS: >= 16
;td2: number of experiments in F2 td2 max = 2 * d30 / in30
;FnMODE: States-TPPI (or TPPI) in F1
;FnMODE: echo-antiecho in F2
;cpds1: decoupling according to sequence defined by cpdprg1
;cpd3: decoupling according to sequence defined by cpdprg3
;pcpd1: 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
; 30 : 80 : 8.1
;for z-only gradients
;gpz1: 30%
;gpz2: 80%
;gpz3: 8.1%
;gpz4: 17.13%
;gpz5: 47%
;use gradient files:
;gpnam1: SINE.100
;gpnam2: SINE.100
;gpnam3: SINE.100
;gpnam4: SINE.100
;gpnam5: SINE.100
;$Id: cbcaconhgp3d,v 1.13.2.1 2007/07/04 13:41:19 ber Exp $