PC7CP2d: 2D cross-polarization/2Q excitation POST_C7 pulse program for TopSpin2.1




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2D CP/2Q excitation with PC7 pulse sequence

Since non-phase cycling is applied to the PC7 excitation pulse, four-phase cycling is applied to the detection pulse P1 for selecting the 0Q -> -1Q coherence order jump, and four-phase cycling is applied to the PC7 reconversion pulse for filtering DQ coherences.

Avoid cross-polarization during POST C7 excitation and reconversion.


*** Outline ***


Code for Avance III spectrometers with topSpin2.1 operating system

;pc7cp2d (TopSpin 2.1)

;2D SQ-DQ correlation experiment with POST_C7 sequence and cross polarization
;Hohwy, M. Jakobsen, H.J. Eden, M. Levitt, M.H., Nielsen, N.C., 
;J. Chem. Phys. 108, 2686-2694 (1998)
;revised 09/09/03 JOS  modified by HF 14.5.07

;Avance III version
;parameters:
;d1 : recycle delay
;d0 : incremented delay (2D) [1 usec]

;p1  : detection pulse at pl1
;p3  : 1H excitation pulse @ PL12
;p5  : FSLG 2pi pulse set by lgcalc.incl
;p15 : HH contact pulse

;pl1  : f1 power level
;pl2  : =120dB, not used
;pl7  : for POST C7 recoupling sequence, B1=7*cnst31 in Hz
;pl12 : for 1H excitation and decoupling
;pl13 : for LG decoupling cpdprg1 = cwlg or cw13 or tppm13
;pcpd2  : decoupling pulse f2 @ PL12, pcpd = 2*P3-0.2us used by TPPM and SPINAL
;sp0    : proton power level during contact
;spnam0 : for CP on 1H e.g. ramp.64 
;cpdprg1: decoupling f2 during C7, e.g. cw (or cwlg) or tppm
;cpdprg2: decoupling f2, e.g. tppm15, SPINAL64

;cnst20: LG-RF field as adjusted, in Hz used to calculate cnst22 
;        and cnst23 +and - LG frequency
;cnst21: =0 frequency reset on resonance (set by lgclac.incl)
;cnst22: +LG frequency offset calc. by lgcalc.incl
;cnst23: -LG frequency offset calc. by lgcalc.incl
;cnst24: offset for 1H evol. during FSLG
;cnst31: spinning speed

;l0    : number of composite C7 cycles for DQ excitation 
;        and DQ reconversion (multiple of 7)
;l3    : number of rotorperiods for t1 increment
;in0   : =l3*(1s/cnst31), t1 increment
;FnMode: undefined
;mc2   : STATES-TPPI
;ns    : 32*n
;WDW : F1 QSINE 3,  F2 QSINE 2 or EM
;use "xau xfshear rotate" to shift spectrum suitably along f1

;$COMMENT=SQ-DQ experiment with post-C7 sequence, cp for excitation
;$CLASS=Solids
;$DIM=2D
;$TYPE=cross polarisation
;$SUBTYPE=homonuclear correlation
;$OWNER=Bruker

define loopcounter count       ;for STATES-TPPI procedure
  "count=td1/2"                ;and STATES cos/sin procedure

define pulse tau1
  "tau1=((0.25s/cnst31)/7)"    ; 90° pulse
define pulse tau4
  "tau4=((1s/cnst31)/7)"       ;360° pulse
define pulse tau3
  "tau3=((0.75s/cnst31)/7)"    ;270° pulse

  "d31=1/cnst31"
  "in0=l3*d31"
  "inf1=l3*d31"

;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt
"acqt0=1u*cnst11"

#include <lgcalc.incl>
                               ;calculates cnst22 from cnst20, RF field at pl13
#include <rot_prot.incl>

  "d0=1u"

  ze
1 d31
2 d1 do:f2                     ;recycle delay, decoupler off

#include <p15_prot.incl>
            ;make sure p15 does not exceed 10 msec
            ;let supervisor change this pulseprogram if 
            ;more is needed
#ifndef lacq
            ;disable protection file for long acquisition change decoupling power !!!
            ;or you risk probe damage
            ;if you set the label lacq (ZGOPTNS -Dlacq), the protection is disabled

#include <aq_prot.incl>
                               ;allows max. 50 msec acquisition time, supervisor
                               ;may change  to max. 1s at less than 5 % duty cycle
                               ;and reduced decoupling field

  1m rpp11                     ;reset the phase ph11 pointer to the first element
  1m rpp12                     ;reset the phase ph12 pointer to the first element
  1m rpp13                     ;reset the phase ph13 pointer to the first element
  1m rpp14                     ;reset the phase ph14 pointer to the first element

  1u fq=cnst22:f2              ;show LG frequencies
  1u fq=cnst23:f2
  1u fq=cnst21:f2

  (p3 pl12 ph1):f2             ;proton 90° pulse
  (p15 pl1 ph2):f1 (p15:sp0 ph10):f2            ;contact pulse with square or 
                                                ;ramp shape ramp.100 on F2

  (p1 pl1 ph4):f1              ;90° pulse putting magnetization back to z-axis 
                               ;for PC7 double-quantum excitation

3 (tau1 pl7 ph11 ipp13 ipp14):f1 (1u cpds1):f2  ;c7 excitation, 1 loop = 2*Tr/7, 
                               ;increment reconversion pulse phase ph13 and ph14 pointers
                                                ;pl13=120 for masr > 15 kHz
                                                ;F2 decoupling cw (or cwlg) or tppm
  (tau4 ph12 ipp12):f1         ;increment phase ph12 pointer
  (tau3 ph11 ipp11):f1         ;increment phase ph11 pointer
                               ;to the next phase in the lists
  lo to 3 times l0             ;l0 DQ excitation block = DQ reconversion block

4 d0 cpds2:f2                                   ;double-quantum evolution time, 
                                                ;F2 decoupling tppm15, SPINAL64

5 (tau1 ph13):f1 (1u cpds1):f2                  ;c7 reconversion, 1 loop = 2*Tr/7,
                                                ;F2 decoupling cw (or cwlg) or tppm
  (tau4 ph14 ipp14):f1         ;increment phase ph14 pointer
  (tau3 ph13 ipp13):f1         ;increment phase ph13 pointer
                               ;to the next phase in the lists
  lo to 5 times l0

  (p1 pl1 ph5):f1 (1u cpds2):f2                 ;F2 decoupling cpdprg2 spinal64, 
                                                ;@ pl12, cnst21=on resonance, 
                                                ;pcpd=2*p3-0.2us
                                                ;detection pulse
  gosc ph31                    ;gosc does not loop to 1
                               ;start ADC with ph31 signal routing
  1m do:f2                     ;decoupling off
                               ;DQ filtering (four phase cycling):
  ;1m ip13                      ;increments all phases of ph13 by 90°
  ;1m ip14                      ;increments all phases of ph14 by 90°
  1m ip13*16384                ;increments all phases of ph13 by 90°
  1m ip14*16384                ;increments all phases of ph14 by 90°

  lo to 1 times ns             ;next scan

  100m wr #0 if #0 zd          ;save data

  ;1m  ip11                     ;increments all phases of ph11 by 45°, 
                                ;90° phase for DQ coherence
  ;1m  ip12                     ;increments all phases of ph12 by 45°,
                                ;90° phase for DQ coherence
  1m ip11*8192                 ;increments all phases of ph11 by 45°, 
                               ;90° phase for DQ coherence
  1m ip12*8192                 ;increments all phases of ph12 by 45°,
                               ;90° phase for DQ coherence
  lo to 1 times 2              ;t1 quadrature detection

  1m id0

  ;1m rp11                     ;reset all phases of ph11, ph12, ph13, and ph14 
  ;1m rp12                     ;to their original values, i.e. to the values they 
  ;1m rp13                     ;had before the first ip11, ip12, ip13, and ip14
  ;1m rp14                     ;in case of STATES remove semicolon at beginning of the 4 lines

  lo to 1 times count          ;count = td1/2

HaltAcqu, 1m
exit

ph1= 1 1 1 1 3 3 3 3
ph2= 0
ph4= 3 3 3 3 1 1 1 1
ph5= 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 1 1 1 1 1 1 1 1 3 3 3 3 3 3 3 3
ph10=0

;ph11 = (float,45.0)   0.00  51.43 102.86 154.29 205.71 257.14 308.57 
;ph12 = (float,45.0) 180.00 231.43 282.86 334.29 385.71 437.14 488.57 
;ph13 = (float,90.0)  90.00 141.43 192.86 244.29 295.71 347.14 398.57 
;ph14 = (float,90.0) 270.00 321.43 372.86 424.29 475.71 527.14 578.57 

ph11=(65536)     0  9362 18725 28087 37449 46811 56174 
ph12=(65536) 32768 42130 51493 60855  4681 14043 23406 
ph13=(65536) 16384 25746 35109 44471 53833 63195  7022 
ph14=(65536) 49152 58514  2341 11703 21065 30427 39790 

ph31= 0 2 0 2 0 2 0 2 2 0 2 0 2 0 2 0 1 3 1 3 1 3 1 3 3 1 3 1 3 1 3 1
  

References

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    1D double quantum filter NMR studies,
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  2. Giuseppe Pileio, Maria Concistrč, Neville McLean, Axel Gansmüller, Richard C. D. Brown, and Malcolm H. Levitt
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  3. M. J. Potrzebowski, J. Gajda, W. Ciesielski, and I. M. Montesinos
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  5. Colan E. Hughes and Marc Baldus
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  14. Mattias Edén, Andreas Brinkmann, Henrik Luthman, Lars Eriksson, and Malcolm H. Levitt
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    J. Chem. Phys. 108, 2686-2694 (1998).
    Abstract
    PC7 pulse sequence

    Definition of PC7 excitation pulse.

     
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    C7 pulse sequence

    Definition of C7 excitation pulse.

     
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