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C13_CHD2_METmethylCPMG.cw
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C13_CHD2_METmethylCPMG.cw
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;C13_CHD2_METmethylCPMG.gcm
;Version for BOTH topSpin v2 & v3
;Change calculation of l6 below to:
; "l6=d5/d8+0.01" ;for TopSpin v2
; "l6=d5/d8-0.49" ;for TopSpin v3
;
;Pulse sequence to measure 13C-methyl R2-exchange contribution to relaxation
;for isolated 13CHD2 of Methionine.
;Including optional 2H refocusing by hard 180 during long CPMG delays.
;Optional 2H decoupling during t1.
;See instructions at the end of pulse sequence
;
; 1) use vclist for different cpmg fields
; 2) interleaved acquisition ns - cpmg - hypercomplex - t1
; 3) cpmgloop = 0,2,4,6,8,...,40
;
;Based on uw_C13_CPMG_Rex_NH_fm_500_my_v5.c, which in turn is
;based on N15_CPMG_Rex_NH_fm_500.c
;
;Coded by Göran Carlström 2014-11-18
;Edited 2014-11-28 to BLKGRAD during CPMG-periods
;Copyright 2014 Göran Carlström, Lund University, Sweden
;
;Disclaimer
;The pulse program has been tested and used on a Bruker AVANCE III HD 500 MHz
;spectrometer at Lund University, Sweden, and on a Bruker AVANCE 600 MHz
;spectrometer enquipped with a 1H,13C,15N TCI cryoprobe at AstraZeneca R&D
;Mölndal, Sweden. The sequence is made available without any expressed
;warranty. We are not liable for any potential damage that might be caused in
;connection with the pulse program. We are not responsible for any damage on
;your hardware or software caused by the use of this pulse program.
;
; channel 1 - 1H
; channel 2 - 13C
; channel 4 - 2H
;$CLASS=HighRes
;$OWNER=Goran
;$DIM=pseudo_3D
prosol relations=<triple>
#include <Avance.incl>
#include <Grad.incl>
#include <Delay.incl>
define list<loopcounter> cpmglist = <$VCLIST>
aqseq 312
"in10=inf2/2"
;***** PULSES *****
"p2=2*p1"
"p4=2*p3"
"p6=2*p5"
"p17=0.5*p16"
"p18=0.9*p16"
"p19=0.3*p16"
"p26=2.0*p25"
;***** LOOPS *****
"l1=(td1)"
"l2=(td2/2)"
"l3=0"
"l6=0"
"l7=0"
"l9=1"
;***** DELAYS *****
"d4=1.0/(4.0*cnst3)" ;taub
"d7=1.0/(4.0*cnst3)" ;taua
"d5=d3/4.0" ;tau_CPMG
"d17=d16/2.0"
"d10=3u"
"d11=30m"
"d12=20u"
"d13=3u"
"d21=0"
"d22=0"
"d23=d5-p5"
"d30=p1*2.385+2.5*d19-p3"
"DELTA1=d7-p17-d16-d13"
"DELTA3=d4-p17-d16-d13"
;"DELTA4=d4-p18-d16-d13"
"DELTA4=d4-p18-d16-d13-d30-p3-0.6366*p1" ; CW
;"DELTA5=DELTA4-d12"
"DELTA5=d4-p18-d16-d13-d12-d30-p3"
;"DELTA6=DELTA3-p5"
"DELTA6=d4-p17-d16-6u-larger(p2,p3)-0.6366*p1" ; CW
"DELTA7=d4+p2"
"cnst31=4.0*atan(1.0)" ;PI
"acqt0=0"
1 ze
d11 pl12:f2
;#if defined(H2REF) || defined(H2DEC)
d11 LOCKDEC_ON
50u LOCKH_ON
d11 H2_PULSE
;#endif /* H2REF, H2DEC */
2 d11 do:f2
d11
3 d11
4 d11
5 d12 pl1:f1 ;set transmitter power
d12 pl2:f2 ;set decoupler power
;#if defined(H2REF) || defined(H2DEC)
d12 pl4:f4 ;set power for 4th channel
d13 BLKGRAD
d11 H2_LOCK
6m LOCKH_OFF
;#endif /* H2REF, H2DEC */
d12 fq=0:f1 ;set transmitter offset
"l3=cpmglist"
if "l3==0" goto 6
"d5=d3/(4.0*l3)"
"d23=d5-p5"
;#ifdef H2REF
if "d5<d8" goto 9
"l6=d5/d8-0.49" ;for TopSpin v3
; "l6=d5/d8+0.01" ;for TopSpin v2
"l7=l6-1"
if "d5/(2.0*l6)<p25" goto 9
"d21=d5/(2.0*l6)-p25"
if "d21<p5" goto 9
"d22=d21-p5"
"l9=0"
goto 6
9 d13
"l9=1"
d13
;#endif /* H2REF */
6 d13
; d12 pl9:f1 ;set transmitter power for presat
; d12 fq=cnst1:f1 ;set transmitter offset for presat
; (p9 ph10):f1 ;presat
; d13
; d12 pl1:f1 ;set transmitter power
; d12 fq=0:f1 ;set transmitter offset
d1
;#if defined(H2REF) || defined(H2DEC)
50u LOCKH_ON
d12 H2_PULSE
;#endif /* H2REF, H2DEC */
50u UNBLKGRAD
(p3 ph10):f2 ;pulse on 2nd channel
d13
p16:gp1
d16
d12 pl0:f1 ;set transmitter power
(p14:sp1 ph13):f1 ;shaped pulse on transmitter
4u
d12 pl1:f1 ;set transmitter power
;***** INEPT *****
(p1 ph10):f1 ;pulse on transmitter
d13
p17:gp2
d16
DELTA1 ;delay < 1/4J(XH)
( center (p2 ph10):f1 (p4 ph10):f2 )
DELTA1
d13
p17:gp2
d16
(p1 ph11):f1 ;pulse on transmitter
d13
p16:gp5
d17 ;pl5:f2 ;CW
d17 BLKGRAD
;#if defined(H2REF)
d6 pl6:f4 ;delay(taueq);
;#else
; d6
;#endif /* H2REF */
(p3 ph2):f2 ;pulse on 2nd channel (CW)
3u pl5:f2 ; CW
;***** 1st CPMG period *****
if "l3 == 0" goto 7
;#if defined(H2REF)
if "l9 > 0" goto 14 ; no 2H refocusing
if "l7 < 1" goto 13 ; short form 2H refocusing
;***** Use pulsed 2H refocusing, long form *****
11 d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
lo to 11 times l7
d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d22
(p6 ph11):f2 ;pulse on 2nd channel
d22
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
12 d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
lo to 12 times l7
lo to 11 times l3
goto 7
;***** Use pulsed 2H refocusing, short form *****
13 d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d22
(p6 ph11):f2 ;pulse on 2nd channel
d22
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
lo to 13 times l3
goto 7
;#endif /* H2REF */
;***** No pulsed 2H refocusing *****
14 d23
(p6 ph11):f2 ;pulse on 2nd channel
d23
lo to 14 times l3
;***** change 2CyHz to Cx *****
7 d13 UNBLKGRAD
p17:gp6
d16 pl2:f2 ; CW
DELTA6
;***** composite 1H 90y-180x-90y on top of 13C 180x *****
( center (p1 ph11 p2 ph10 p1 ph11):f1 (p4 ph10):f2 )
DELTA6
d13 pl5:f2
p17:gp6
d17 ; d17=0.5*d16
d17 BLKGRAD
;***** start of the CPMG train for second period time_T2/2 on Cx *****
if "l3 == 0" goto 8
;#if defined(H2REF)
if "l9 > 0" goto 24
if "l7 < 1" goto 23 ; CW error! originally goto 22
;***** Use pulsed 2H refocusing, long form *****
21 d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
lo to 21 times l7
d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d22
(p6 ph10):f2 ;pulse on 2nd channel
d22
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
22 d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
lo to 22 times l7
lo to 21 times l3
goto 8
;***** Use pulsed 2H refocusing, short form *****
23 d21
(p26 ph10):f4 ;pulse on 4th 2H channel
d22
(p6 ph10):f2 ;pulse on 2nd channel
d22
(p26 ph10):f4 ;pulse on 4th 2H channel
d21
lo to 23 times l3
goto 8
;#endif /* H2REF */
;***** No pulsed 2H refocusing *****
24 d23
(p6 ph10):f2 ;pulse on 2nd channel
d23
lo to 24 times l3
8 d13 pl2:f2 ; CW
(p3 ph11):f2 ;pulse on 2nd channel CW
d13 UNBLKGRAD
d6 ;delay(taueq);
p19:gp7
;#if defined(H2DEC)
d17 pl4:f4
d17 BLKGRAD
;#else
; d16
;#endif /* H2DEC */
;#if defined(H2DEC)
;***** 2D decoupling on *****
(p23 ph11):f4 ;pulse on 4th 2H channel
4u cpd4:f4
;#endif /* H2DEC */
(p3 ph3):f2 ;pulse on 2nd channel
d4 ;delay(tau1 + taub);
;***** T1 evolution *****
d10
(p2 ph10):f1 ;pulse on transmitter
d10 ;delay(tau1);
(p4 ph10):f2 ;pulse on 2nd channel
DELTA7 ;delay(taub + 2*pw);
(p3 ph11):f2 ;pulse on 2nd channel
;#if defined(H2DEC)
4u do:f4
(p23 ph13):f4 ;pulse on 4th 2H channel
;***** 2D decoupling off *****
;#endif /* H2DEC */
d13 UNBLKGRAD
p16:gp4
d16
(p1 ph10):f1 ;pulse on transmitter
d13
p18:gp3
d16
DELTA4
(p1*0.231 ph11 d19 p1*0.692 ph11 d19 p1*1.462 ph11 d19):f1 (d30 p4 ph10):f2
(p1*1.462 ph13 d19 p1*0.692 ph13 d19 p1*0.231 ph13):f1
d13
d12 pl12:f2 ;set decoupler power
DELTA5
p18:gp3
d17
d17 BLKGRAD
go=2 ph31 cpd2:f2
d11 do:f2 wr #0 if #0 zd
d11 cpmglist.inc
lo to 3 times l1
d11 ip3 cpmglist.res
lo to 4 times 2
d11 id10
lo to 5 times l2
;#if defined(H2REF) || defined(H2DEC)
d11 H2_LOCK
d11 LOCKH_OFF
d11 LOCKDEC_OFF
;#endif /* H2REF, H2DEC */
exit
ph2 = 0 2
ph3 = 0 0 2 2
ph4 = 0
ph10 = 0
ph11 = 1
ph12 = 2
ph13 = 3
ph31 = 0 2 2 0
;pl0 : 120dB
;pl1 : f1 channel - power level for 1H pulse (default)
;pl2 : f2 channel - power level for 13C pulse (default)
;pl4 : f4 channel - power level for 2H pulse & dec (default)
;pl5 : f2 channel - power level for 13C cpmg [6.6 kHz => 38us pulse length]
;pl6 : f4 channel - power level for 2H refocus during cpmg []
;pl9 : f1 channel - power level for 1H presat
;pl12: f2 channel - power level for 13C CPD/BB decoupling [2.5 kHz => 100us pulse length]
;sp1: f1 channel - shaped pulse H2O flipdown [default]
;p1 : f1 channel - 90 degree high power pulse
;p2 : f1 channel - 180 degree high power pulse [2*p1]
;p3 : f2 channel - 90 degree high power pulse
;p4 : f2 channel - 180 degree high power pulse [2*p3]
;p5 : f2 channel - 90 degree cpmg power pulse [38 us]
;p6 : f2 channel - 180 degree cpmg power pulse [2*p5]
;p9 : f1 channel - presat pulse [1-1.5s]
;p14: f1 channel - 90 degree shaped pulse [5 ms]
;p16: gradient pulse gp1, gp4 & gp5 [1 ms]
;p17: gradient pulse gp2 & gp6 [0.5 ms]
;p18: gradient pulse gp3 [0.9 ms]
;p19: gradient pulse gp7 [0.3 ms]
;p23: f4 channel - 90 degree @ pl4 [300 us]
;p25: f4 channel - 90 degree refocus @ pl6 [300 us]
;p26: f4 channel - 180 degree refocus @ pl6 [2*p25]
;d10 : incremented delay (2D)
;d1 : relaxation delay; 1-5 * T1
;d3 : total time for CPMG trains [<= 40 ms!]
;d4 : 1/(4*JCH) taub [1.785 ms]
;d5 : tau_cpmg
;d6 : taueq, [400 us]
;d7 : < 1/(4*JCH) taua [1.785 ms]
;d8 : tau_lim limiting delay 2H decoupling [2 ms]
;d11: delay for disk I/O [30 ms]
;d12: delay power switching [20 us]
;d16: delay for gradient recovery [200 us]
;d19: delay 3-9-19 watergate [500 200 u, 600 167u, 800 125u]
;cnst1: f1 offset for presat (Hz from carrier) [0]
;cnst3: J(CH) [135 Hz]
;l3: number of cpmg cycles in each period [<= 40 !]
; total number of cycles = 2*l3
;l6: loop for 2H refocusing
;l7: l6-1, loop for 2H refocusing
;l9: flag for 2H
;spnam1: hard or Eburp2.1000
;spoffset1: 0
;inf1: 1/SW(X) = 2 * DW(X)
;in0: 1/(2 * SW(X)) = DW(X)
;nd0: 2
;NS: 4 * n
;DS: 16
;td1: number of experiments
;FnMODE: States-TPPI, TPPI, States or QSEQ
;cpd2: decoupling according to sequence defined by cpdprg2 [garp]
;cpd4: decoupling according to sequence defined by cpdprg4 [waltz16]
;pcpd2: f2 channel - 90 degree pulse for decoupling sequence [133 us]
;pcpd4: f4 channel - 90 degree pulse for decoupling sequence [300 us]
;for z-only gradients:
;gpz1: 32.28% 10.3 G/cm V: 5000
;gpz2: 25.82% 8.24 G/cm V: 4000
;gpz3: 78.09% 39.1 G/cm V: 19000
;gpz4: 71.01% 22.6 G/cm V: 11000
;gpz5: -38.73% 12.4 G/cm V: -6000
;gpz6: 73.98% 37.1 G/cm V: 18000
;gpz7: 35.51% 11.3 G/cm V: 5500
;use gradient files:
;gpnam1: SINE.100
;gpnam2: SINE.100
;gpnam3: RECT.1
;gpnam4: SINE.100
;gpnam5: SINE.100
;gpnam6: RECT.1
;gpnam7: SINE.100
;preprocessor-flags-start
;H2REF: for 2H refocusing pulses during cpmg. Start experiment with
; option -DH2REF (eda: ZGOPTNS)
;H2DEC: for 2H decoupling during t1. Start experiment with
; option -DH2DEC (eda: ZGOPTNS)
;preprocessor-flags-end
;$Id: C13_CHD2_METmethylCPMG.gcm,v 4.0 2015/01/27 11:54:19 gcm Exp $