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N15HetNoe_hsqc.cw
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N15HetNoe_hsqc.cw
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; not working nicely at the moment...
; 15N1H HetNoe relaxation experiment with sensitivity enhanced (Rance-Kay) HSQC read-out
; for 15N, 2H15N, 15N13C and 2H15N13C labelled proteins
; written by NL 10/27/11
; see footnotes
#include <Avance.incl>
#include <Grad.incl>
#include <Delay.incl>
;#define LABEL_CN ; switch on for 13C labelled samples
"in0=inf1*0.5"
"l3=td1/2"
"d0=10u"
"d11=30m"
"d26=p7-p1"
"DELTA2=2.65m"
"DELTA3=2.65m"
"DELTA4=p24-p19*0.63"
"DELTA5=2.65m-p25-200u"
"DELTA7=2.65m"
"cnst22=176"
"cnst21=56"
"l1=1"
"l2=1"
# ifdef LABEL_CN
"DELTA6=35u+p4*4"
"d25=20m-p15*0.5-p4*4-5u"
# else
"DELTA6=30u"
"d25=20m-p15*0.5-p4*4-5u"
# endif
"cnst21=176"
"cnst22=56"
"cnst23=8.5"
"spoff4=bf2*((cnst22-cnst21)/1000000)"
"spoff18=bf3*((cnst18)/1000000)"
"d8=p1"
"acqt0=0"
1 ze
1m
2 3m do:f3
d11
1m LOCKH_OFF
3 3m
4 1m
5 1m do:f3
1m BLKGRAD
10u pl1:f1
#ifdef LABEL_CN
10u pl4:f2
#endif
10u pl7:f3
(p7 ph0):f3 ; 90N pulse before d1
d1
;--------------- 1H saturation period-----------------------
10u fq=cnst23(bf ppm):f1
if "l2 == 1" goto 9
8 11m
(p1*2 ph0):f1
11m
lo to 8 times l8
goto 10
9 11m
d8*2
11m
lo to 9 times l8
10 10u fq=0:f1
10u UNBLKGRAD
;---------- Echo- Antiecho encoding------------------------
(p7 ph7):f3
;goto 999
DELTA6 ;compensation for d0 15N evolution
DELTA5
190u
p25:gp5*EA
10u
(center (p1*2 ph0):f1 (p7*2 ph7):f3)
10u
p25:gp5*EA*-1
190u
DELTA5
; t1 evolution ---------------------------------------------
89 d0*0.5 gron1
5u groff
d0*0.5 gron0
5u groff
# ifdef LABEL_CN
(center (p1*2 ph0):f1 (p4*2 ph0 3u 3u pl2 p4*2:sp4 ph0):f2)
# else
(p1*2 ph0):f1
# endif
d0
;goto 999
;--------Rance-Kay transfer back ----------------------------
98 (center (p1 ph0):f1 (p7 ph8):f3)
DELTA2 gron2
10u groff
(center(p1*2 ph0):f1 (p7*2 ph0):f3)
DELTA2 gron2
10u groff
; ---second INEPT ----------------------------------------
(center (p1 ph1):f1 (p7 ph1):f3) ;DOUBLE 90
DELTA3 gron3
10u groff
(center(p1*2 ph0):f1 (p7*2 ph0):f3)
DELTA3 gron3
10u groff
(d26*0.5 p19 ph0:r):f1
998 245u
DELTA4
(p1*2 ph0):f1
5u
p24:gp4
200u
999 5u ; jump point for water optimisation
#ifdef LABEL_CN
5u pl30:f2 ; 13C DECOUPLING POWER
#else
5u
#endif
10u pl31:f3
20u BLKGRAMP
; acquisition
#ifdef LABEL_CN
go=2 ph31 cpds3:f3 cpd2:f2
500u do:f3
500u do:f2
#else
go=2 ph31 cpds3:f3
1m do:f3
#endif
1m LOCKH_OFF
d11 wr #0 if #0 zd
; loop over relaxation times
2m iu2
lo to 3 times 2
; loop over 15N evolution
1m ip8*2
1m igrad EA
1m ru2
lo to 4 times 2
1m id0
lo to 5 times l3
1m do:f3
1m BLKGRAD
exit
ph0=0
ph1=1 ;check right phase for Boltzmann !!!!!
ph2=2
ph7= 1 3 3 1
ph8= 0
ph31=1 3 3 1
;-------------NOTES----------------------
;o1p = 4.7 ppm
;o2p=176 ppm (CO)
;o3p=119 ppm
;NS=4*n
;in0=inf/2
;SW=1/(2*in0)
;echo-antiecho in N15 (process as Complex in NmrDraw before splitting the spectra)
; 1H pulses
;p1: 90 deg hard 1H pulse @pl1
;p19 last 90 deg hard 1H pulse @pl1, can be adjusted for improving water-supression
;pl1: 1H 90 deg
;pl0: 120 dB
; 13C pulses
;p4: 13CO selective 180 deg (23.7*2us @ 600 MHz) @pl4
;pl4: 13C 90 deg
;sp4: 13CA selective 180 deg (23.7*2us @ 600 MHz)
;15N pulses
;p7 : 90 deg hard 15N pulse @pl7
;pl7 :15N 90 deg
;CPDPRG3: garp (aq 15N decoupling)
;pcpd3: 15N decoupling (200u @pl31)
;pl31: 15N decoupling power
; gradients
;p20: 1000u
;p21: 200u
;p24: 201u Echo/Anti-echo decoding gradient
;p25: 1000u Echo/Anti-echo half-encoding gradient
;for z-only gradients
;gpz0: 1.5%
;gpz1: -1.5%
;gpz2: -3%
;gpz3: 0.5%
;gpz4: 40%
;gpz5: 40%
;gpz10: 1%
;gpz11: 2%
;gpz20: 28%
;gpz21: 50%
;gpnam4 SINE.10
;gpnam5 SINE.10
;gpnam20 SINE.50
;gpnam21 SINE.10