Arg side chain NC correlation experiment

; (Yuichi Yoshimura and Frans Mulder 31/Aug/2016)
; compatibility topspin3.5pl5
;
; 13C-detected Ne-Cz and Nh-Cz correlations for
; probing Arg residues (f1:13C, f2:1H, f3:15N)
;
; f2(He/Hh) -> f3(Ne/Nh,t1) -> f1(Cz,t2)
;
; Magnetization transfer from 1H to 15N (DIPSI-2):
; mixing time (d27) = p45*28.778*L5
;
; Magnetization transfer from 15N to 13C (DIPSI-3):
; mixing time (d28) = p46*54.325*L1
;
; (if L7 = 0) 1H-coupled 15N encoding (without 1H decoupling)
; (else) 1H decoupling during 15N chemical shift evolution
;
; (if L3 = 0) 15N decoupling during acquisition
; (else) 1H and 15N decoupling during acquisition

;$CLASS=HighRes
;$DIM=2D
;$TYPE=
;$SUBTYPE=
;$COMMENT=

prosol relations=<triple_c>

#include <Avance.incl>
#include <Delay.incl>
#include <Grad.incl>

“d11=30m”
“d12=20u”
“p16=1m”
“p19=300u”
“d16=200u”

; 1H/15N-CP (p45 = 62.5 u, RF field of 4.0 kHz)
“if ( l5 %4 == 0 ) { l6=l5/4; }”
“if ( l5 %4 == 1 ) { l6=(l5-1)/4; }”
“if ( l5 %4 == 2 ) { l6=(l5-2)/4; }”
“if ( l5 %4 == 3 ) { l6=(l5-3)/4; }”
“d27=p45*28.778*l5”; DIPSI-2 mixing time
“plw25=plw2*(pow((p3/p45),2))”
“plw23=plw3*(pow((p21/p45),2))”

; 15N/13C-CP (p46 = 140 u, RF field of 1.8 kHz)
“if ( l1 %4 == 0 ) { l2=l1/4; }”
“if ( l1 %4 == 1 ) { l2=(l1-1)/4; }”
“if ( l1 %4 == 2 ) { l2=(l1-2)/4; }”
“if ( l1 %4 == 3 ) { l2=(l1-3)/4; }”
“d28=p46*54.325*l1”; DIPSI-3 mixing time
“plw24=plw1*(pow((p1/p46),2))”
“plw22=plw3*(pow((p21/p46),2))”

“d0=3u”
“in0=inf1/2”

“p22=p21*2”

“plw0=0”

“DELTA=d0*2+p8”

“cnst11=o2/bf2”
“cnst21=o1/bf1”
“spoff13=bf1*(cnst21+cnst22)/2000000-o1”
“spoff24=0”

1 ze
d11 pl12:f2
d27 ; 1H -> 15N (DIPSI-2) mixing time
d28 ; 15N -> 13C (DIPSI-3) mixing time
2 d11 do:f2 do:f3
d11 pl1:f1 pl2:f2 pl3:f3

d1
50u UNBLKGRAD
(p1 ph0):f1 (p21 ph0):f3
4u
p16:gp0
d16

(p3 ph1):f2
4u pl25:f2 pl23:f3

8 (p45*3.556 ph21):f2 (p45*3.556 ph21):f3
(p45*4.556 ph22):f2 (p45*4.556 ph22):f3
(p45*3.222 ph21):f2 (p45*3.222 ph21):f3
(p45*3.167 ph22):f2 (p45*3.167 ph22):f3
(p45*0.333 ph21):f2 (p45*0.333 ph21):f3
(p45*2.722 ph22):f2 (p45*2.722 ph22):f3
(p45*4.167 ph21):f2 (p45*4.167 ph21):f3
(p45*2.944 ph22):f2 (p45*2.944 ph22):f3
(p45*4.111 ph21):f2 (p45*4.111 ph21):f3

(p45*3.556 ph22):f2 (p45*3.556 ph22):f3
(p45*4.556 ph21):f2 (p45*4.556 ph21):f3
(p45*3.222 ph22):f2 (p45*3.222 ph22):f3
(p45*3.167 ph21):f2 (p45*3.167 ph21):f3
(p45*0.333 ph22):f2 (p45*0.333 ph22):f3
(p45*2.722 ph21):f2 (p45*2.722 ph21):f3
(p45*4.167 ph22):f2 (p45*4.167 ph22):f3
(p45*2.944 ph21):f2 (p45*2.944 ph21):f3
(p45*4.111 ph22):f2 (p45*4.111 ph22):f3

(p45*3.556 ph22):f2 (p45*3.556 ph22):f3
(p45*4.556 ph21):f2 (p45*4.556 ph21):f3
(p45*3.222 ph22):f2 (p45*3.222 ph22):f3
(p45*3.167 ph21):f2 (p45*3.167 ph21):f3
(p45*0.333 ph22):f2 (p45*0.333 ph22):f3
(p45*2.722 ph21):f2 (p45*2.722 ph21):f3
(p45*4.167 ph22):f2 (p45*4.167 ph22):f3
(p45*2.944 ph21):f2 (p45*2.944 ph21):f3
(p45*4.111 ph22):f2 (p45*4.111 ph22):f3

(p45*3.556 ph21):f2 (p45*3.556 ph21):f3
(p45*4.556 ph22):f2 (p45*4.556 ph22):f3
(p45*3.222 ph21):f2 (p45*3.222 ph21):f3
(p45*3.167 ph22):f2 (p45*3.167 ph22):f3
(p45*0.333 ph21):f2 (p45*0.333 ph21):f3
(p45*2.722 ph22):f2 (p45*2.722 ph22):f3
(p45*4.167 ph21):f2 (p45*4.167 ph21):f3
(p45*2.944 ph22):f2 (p45*2.944 ph22):f3
(p45*4.111 ph21):f2 (p45*4.111 ph21):f3

lo to 8 times l6

if “l5 %4 == 0”
{
}
else
{
(p45*3.556 ph21):f2 (p45*3.556 ph21):f3
(p45*4.556 ph22):f2 (p45*4.556 ph22):f3
(p45*3.222 ph21):f2 (p45*3.222 ph21):f3
(p45*3.167 ph22):f2 (p45*3.167 ph22):f3
(p45*0.333 ph21):f2 (p45*0.333 ph21):f3
(p45*2.722 ph22):f2 (p45*2.722 ph22):f3
(p45*4.167 ph21):f2 (p45*4.167 ph21):f3
(p45*2.944 ph22):f2 (p45*2.944 ph22):f3
(p45*4.111 ph21):f2 (p45*4.111 ph21):f3

if “l5 %4 == 1”
{
}
else
{
(p45*3.556 ph22):f2 (p45*3.556 ph22):f3
(p45*4.556 ph21):f2 (p45*4.556 ph21):f3
(p45*3.222 ph22):f2 (p45*3.222 ph22):f3
(p45*3.167 ph21):f2 (p45*3.167 ph21):f3
(p45*0.333 ph22):f2 (p45*0.333 ph22):f3
(p45*2.722 ph21):f2 (p45*2.722 ph21):f3
(p45*4.167 ph22):f2 (p45*4.167 ph22):f3
(p45*2.944 ph21):f2 (p45*2.944 ph21):f3
(p45*4.111 ph22):f2 (p45*4.111 ph22):f3

if “l5 %4 == 2”
{
}
else
{
(p45*3.556 ph22):f2 (p45*3.556 ph22):f3
(p45*4.556 ph21):f2 (p45*4.556 ph21):f3
(p45*3.222 ph22):f2 (p45*3.222 ph22):f3
(p45*3.167 ph21):f2 (p45*3.167 ph21):f3
(p45*0.333 ph22):f2 (p45*0.333 ph22):f3
(p45*2.722 ph21):f2 (p45*2.722 ph21):f3
(p45*4.167 ph22):f2 (p45*4.167 ph22):f3
(p45*2.944 ph21):f2 (p45*2.944 ph21):f3
(p45*4.111 ph22):f2 (p45*4.111 ph22):f3
}
}
}

4u pl3:f3
(p21 ph1):f3
4u

p16:gp1
d16 pl0:f1 pl12:f2

if “l7 == 0”
{
}
else
{
d12 cpd2:f2 ph0
}

(p21 ph4):f3
d0
(p8:sp13 ph0):f1
d0
(p22 ph0):f3
DELTA
(p21 ph6):f3

if “l7 == 0”
{
d12
}
else
{
d12 do:f2
}
p16:gp2
d16 pl2:f2
(p3 ph0):f2
d12
p16:gp2
d16

(p21 ph5):f3
4u pl24:f1 pl12:f2 pl22:f3

9 (p46*2.722 ph11):f1 (p46*2.722 ph11):f3
(p46*4.389 ph12):f1 (p46*4.389 ph12):f3
(p46*2.778 ph11):f1 (p46*2.778 ph11):f3
(p46*3.056 ph12):f1 (p46*3.056 ph12):f3
(p46*0.333 ph11):f1 (p46*0.333 ph11):f3
(p46*2.556 ph12):f1 (p46*2.556 ph12):f3
(p46*4.000 ph11):f1 (p46*4.000 ph11):f3
(p46*2.722 ph12):f1 (p46*2.722 ph12):f3
(p46*4.111 ph11):f1 (p46*4.111 ph11):f3
(p46*3.778 ph12):f1 (p46*3.778 ph12):f3
(p46*3.889 ph11):f1 (p46*3.889 ph11):f3
(p46*2.889 ph12):f1 (p46*2.889 ph12):f3
(p46*3.000 ph11):f1 (p46*3.000 ph11):f3
(p46*0.333 ph12):f1 (p46*0.333 ph12):f3
(p46*2.500 ph11):f1 (p46*2.500 ph11):f3
(p46*4.050 ph12):f1 (p46*4.050 ph12):f3
(p46*2.830 ph11):f1 (p46*2.830 ph11):f3
(p46*4.389 ph12):f1 (p46*4.389 ph12):f3

(p46*2.722 ph12):f1 (p46*2.722 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3
(p46*2.778 ph12):f1 (p46*2.778 ph12):f3
(p46*3.056 ph11):f1 (p46*3.056 ph11):f3
(p46*0.333 ph12):f1 (p46*0.333 ph12):f3
(p46*2.556 ph11):f1 (p46*2.556 ph11):f3
(p46*4.000 ph12):f1 (p46*4.000 ph12):f3
(p46*2.722 ph11):f1 (p46*2.722 ph11):f3
(p46*4.111 ph12):f1 (p46*4.111 ph12):f3
(p46*3.778 ph11):f1 (p46*3.778 ph11):f3
(p46*3.889 ph12):f1 (p46*3.889 ph12):f3
(p46*2.889 ph11):f1 (p46*2.889 ph11):f3
(p46*3.000 ph12):f1 (p46*3.000 ph12):f3
(p46*0.333 ph11):f1 (p46*0.333 ph11):f3
(p46*2.500 ph12):f1 (p46*2.500 ph12):f3
(p46*4.050 ph11):f1 (p46*4.050 ph11):f3
(p46*2.830 ph12):f1 (p46*2.830 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3

(p46*2.722 ph12):f1 (p46*2.722 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3
(p46*2.778 ph12):f1 (p46*2.778 ph12):f3
(p46*3.056 ph11):f1 (p46*3.056 ph11):f3
(p46*0.333 ph12):f1 (p46*0.333 ph12):f3
(p46*2.556 ph11):f1 (p46*2.556 ph11):f3
(p46*4.000 ph12):f1 (p46*4.000 ph12):f3
(p46*2.722 ph11):f1 (p46*2.722 ph11):f3
(p46*4.111 ph12):f1 (p46*4.111 ph12):f3
(p46*3.778 ph11):f1 (p46*3.778 ph11):f3
(p46*3.889 ph12):f1 (p46*3.889 ph12):f3
(p46*2.889 ph11):f1 (p46*2.889 ph11):f3
(p46*3.000 ph12):f1 (p46*3.000 ph12):f3
(p46*0.333 ph11):f1 (p46*0.333 ph11):f3
(p46*2.500 ph12):f1 (p46*2.500 ph12):f3
(p46*4.050 ph11):f1 (p46*4.050 ph11):f3
(p46*2.830 ph12):f1 (p46*2.830 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3

(p46*2.722 ph11):f1 (p46*2.722 ph11):f3
(p46*4.389 ph12):f1 (p46*4.389 ph12):f3
(p46*2.778 ph11):f1 (p46*2.778 ph11):f3
(p46*3.056 ph12):f1 (p46*3.056 ph12):f3
(p46*0.333 ph11):f1 (p46*0.333 ph11):f3
(p46*2.556 ph12):f1 (p46*2.556 ph12):f3
(p46*4.000 ph11):f1 (p46*4.000 ph11):f3
(p46*2.722 ph12):f1 (p46*2.722 ph12):f3
(p46*4.111 ph11):f1 (p46*4.111 ph11):f3
(p46*3.778 ph12):f1 (p46*3.778 ph12):f3
(p46*3.889 ph11):f1 (p46*3.889 ph11):f3
(p46*2.889 ph12):f1 (p46*2.889 ph12):f3
(p46*3.000 ph11):f1 (p46*3.000 ph11):f3
(p46*0.333 ph12):f1 (p46*0.333 ph12):f3
(p46*2.500 ph11):f1 (p46*2.500 ph11):f3
(p46*4.050 ph12):f1 (p46*4.050 ph12):f3
(p46*2.830 ph11):f1 (p46*2.830 ph11):f3
(p46*4.389 ph12):f1 (p46*4.389 ph12):f3

lo to 9 times l2

if “l1 %4 == 0”
{
}
else
{
(p46*2.722 ph11):f1 (p46*2.722 ph11):f3
(p46*4.389 ph12):f1 (p46*4.389 ph12):f3
(p46*2.778 ph11):f1 (p46*2.778 ph11):f3
(p46*3.056 ph12):f1 (p46*3.056 ph12):f3
(p46*0.333 ph11):f1 (p46*0.333 ph11):f3
(p46*2.556 ph12):f1 (p46*2.556 ph12):f3
(p46*4.000 ph11):f1 (p46*4.000 ph11):f3
(p46*2.722 ph12):f1 (p46*2.722 ph12):f3
(p46*4.111 ph11):f1 (p46*4.111 ph11):f3
(p46*3.778 ph12):f1 (p46*3.778 ph12):f3
(p46*3.889 ph11):f1 (p46*3.889 ph11):f3
(p46*2.889 ph12):f1 (p46*2.889 ph12):f3
(p46*3.000 ph11):f1 (p46*3.000 ph11):f3
(p46*0.333 ph12):f1 (p46*0.333 ph12):f3
(p46*2.500 ph11):f1 (p46*2.500 ph11):f3
(p46*4.050 ph12):f1 (p46*4.050 ph12):f3
(p46*2.830 ph11):f1 (p46*2.830 ph11):f3
(p46*4.389 ph12):f1 (p46*4.389 ph12):f3

if “l1 %4 == 1”
{
}
else
{
(p46*2.722 ph12):f1 (p46*2.722 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3
(p46*2.778 ph12):f1 (p46*2.778 ph12):f3
(p46*3.056 ph11):f1 (p46*3.056 ph11):f3
(p46*0.333 ph12):f1 (p46*0.333 ph12):f3
(p46*2.556 ph11):f1 (p46*2.556 ph11):f3
(p46*4.000 ph12):f1 (p46*4.000 ph12):f3
(p46*2.722 ph11):f1 (p46*2.722 ph11):f3
(p46*4.111 ph12):f1 (p46*4.111 ph12):f3
(p46*3.778 ph11):f1 (p46*3.778 ph11):f3
(p46*3.889 ph12):f1 (p46*3.889 ph12):f3
(p46*2.889 ph11):f1 (p46*2.889 ph11):f3
(p46*3.000 ph12):f1 (p46*3.000 ph12):f3
(p46*0.333 ph11):f1 (p46*0.333 ph11):f3
(p46*2.500 ph12):f1 (p46*2.500 ph12):f3
(p46*4.050 ph11):f1 (p46*4.050 ph11):f3
(p46*2.830 ph12):f1 (p46*2.830 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3

if “l1 %4 == 2”
{
}
else
{
(p46*2.722 ph12):f1 (p46*2.722 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3
(p46*2.778 ph12):f1 (p46*2.778 ph12):f3
(p46*3.056 ph11):f1 (p46*3.056 ph11):f3
(p46*0.333 ph12):f1 (p46*0.333 ph12):f3
(p46*2.556 ph11):f1 (p46*2.556 ph11):f3
(p46*4.000 ph12):f1 (p46*4.000 ph12):f3
(p46*2.722 ph11):f1 (p46*2.722 ph11):f3
(p46*4.111 ph12):f1 (p46*4.111 ph12):f3
(p46*3.778 ph11):f1 (p46*3.778 ph11):f3
(p46*3.889 ph12):f1 (p46*3.889 ph12):f3
(p46*2.889 ph11):f1 (p46*2.889 ph11):f3
(p46*3.000 ph12):f1 (p46*3.000 ph12):f3
(p46*0.333 ph11):f1 (p46*0.333 ph11):f3
(p46*2.500 ph12):f1 (p46*2.500 ph12):f3
(p46*4.050 ph11):f1 (p46*4.050 ph11):f3
(p46*2.830 ph12):f1 (p46*2.830 ph12):f3
(p46*4.389 ph11):f1 (p46*4.389 ph11):f3
}
}
}

d12
p19:gp3
d16 pl0:f1 pl16:f3
(p12:sp24 ph0):f1
d12
p19:gp3
d16 BLKGRAD

if “l3 == 0”
{
go=2 ph31 cpd3:f3
}
else
{
go=2 ph31 cpd2:f2 cpd3:f3
}
d11 do:f2 do:f3 mc #0 to 2
F1PH(calph(ph4, +90), caldel(d0, +in0) & calph(ph6, +180) & calph(ph31, +180))

exit

ph0= 0
ph1= 1
ph2= 2
ph3= 3
ph4= 0 2
ph5= 1 1 1 1 3 3 3 3
ph6= 0 0 2 2
ph11=0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2
ph12=2 2 2 2 2 2 2 2 0 0 0 0 0 0 0 0
ph21=0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2
ph22=2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
ph31=0 2 2 0 2 0 0 2

;pl0 : 0 W
;pl1 : f1 channel – power level for pulse (default)
;pl2 : f2 channel – power level for pulse (default)
;pl3 : f3 channel – power level for pulse (default)
;pl12: f2 channel – power level for CPD/BB decoupling
;pl16: f3 channel – power level for CPD/BB decoupling
;pl22: f3 channel – power level for DIPSI-3 (15N/13C)
;pl23: f3 channel – power level for DIPSI-2 (1H/15N)
;pl24: f1 channel – power level for DIPSI-3 (15N/13C)
;pl25: f2 channel – power level for DIPSI-2 (1H/15N)
;sp13: f1 channel – shaped pulse 180 degree (adiabatic)
;sp24: f1 channel – shaped pulse 180 degree (Cz on resonance)
;p1 : f1 channel –  90 degree high power pulse
;p3 : f2 channel –  90 degree high power pulse
;p8 : f1 channel – 180 degree shaped pulse for inversion (adiabatic)
;p12: f1 channel – 180 degree shaped pulse
;p16: gradient pulse [1 ms]
;p19: gradient pulse [300 us]
;p21: f3 channel –  90 degree high power pulse
;p22: f3 channel – 180 degree high power pulse
;p45: f2/f3 channel – CP (DIPSI-2) [62.5 us]
;p46: f1/f3 channel – CP (DIPSI-3) [140 us]
;d0 : incremented delay (2D)
;d1 : relaxation delay; 1-5 * T1
;d11: delay for disk I/O                           [30 msec]
;d12: short delay                                  [20 usec]
;d16: delay for homospoil/gradient recovery
;d27: mixing time (1H -> 15N)                      [~9 msec]
;d28: mixing time (15N -> 13C)                     [~30 msec]
;cnst21: CZ chemical shift offset [= o1p, 156 ppm]
;cnst22: CD chemical shift offset [40.5 ppm]
;o1p: CZ chemical shift offset [156 ppm]
;o2p: HE/HH chemical shift offset [7 ppm]
;o3p: NE/NH chemical shift offset [78 ppm]
;inf1: 1/SW(X) = 2 * DW(X)
;in0: 1/(2 * SW(X)) = DW(X)
;nd0: 2
;l1: DIPSI-3 mixing time (d28, 15N->13C) = p46*54.325*l1
;l2: floor(L1/4)
;l3: = 0 (15N decouple) or 1 (1H & 15N decouple) during t2
;l5: DIPSI-2 mixing time (d27, 1H->15N) = p45*28.778*l5
;l6: floor(L5/4)
;l7: = 0: 1H-coupled 15N encoding (without 1H decoupling)
;NS: number of scans
;DS: dummy scans
;td1: number of experiments
;FnMODE: States-TPPI
;cpd2: decoupling according to sequence defined by cpdprg2
;pcpd2: f2 channel – 90 degree pulse for decoupling sequence
;cpd3: decoupling according to sequence defined by cpdprg3
;pcpd3: f3 channel – 90 degree pulse for decoupling sequence

;for z-only gradients:
;gpz0: 41 %
;gpz1: 30 %
;gpz2: 19 %
;gpz3: 12 %

;use gradient files:
;gpnam0: SINE.100
;gpnam1: SINE.100
;gpnam2: SINE.100
;gpnam3: SINE.100