PC72d: 2D double quantum excitation POST_C7 pulse program for TopSpin2.1

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.

;pc72d (TopSpin 2.0)

;SQ-DQ experiment using POST_C7 sequence
;for setup of the 2D INADEQUATE type experiments
;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

;Avance II+ version
;parameters:
;d1  : recycle delay
;d0  : incremented delay (2D) [3 usec]
;d20 : delay between saturation pulses

;pl1 : f1 power level for presaturation pulses and detection pulse
;pl7 : for POST C7 recoupling sequence, B1=7*cnst31 in Hz
;pl2 : =120 dB, not used here
;p1  : detection pulse at pl1

;cnst31 : spinning speed, make sure cnst31>1000
;l1  : number of composite C7 cycles for DQ excitation 
;l3  : number of rotor revolution for DQ evolution
;l20 : # of pulses in saturation pulse train, 0 if undesired

;in0 : =l3*(1s/cnst31), t1 increment
;FnMode : undefined
;mc2    : STATES-TPPI
;nd0 : 1
;ns  : n*16
;WDW : F1 QSINE 3,  F2 QSINE 2 or EM
;zgoptns :-Dpresat or blank

;$COMMENT=SQ-DQ experiment with post-C7 sequence
;$CLASS=Solids
;$DIM=2D
;$TYPE=direct excitation
;$SUBTYPE=homonuclear correlation
;$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=1s/cnst31"
  "d0=3u"
  "in0=l3*d31"

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

#include <rot_prot.incl>
#include <Avancesolids.incl>

  ze                           ;acquire into a cleared memory
1 d31

#ifdef presat                  ;set with -Dpresat
pres, d20                      ;delay between saturation pulses
  (p1 pl1 ph1):f1              ;saturation loop if required
  lo to pres times l20
#endif /* presat */

2 d1
  1m rpp11                     ;reset the phase program ph11 pointer to the first element
  1m rpp12                     ;reset the phase program ph12 pointer to the first element
  1m rpp13                     ;reset the phase program ph13 pointer to the first element
  1m rpp14                     ;reset the phase program ph14 pointer to the first element
  1u pl7:f1

3 tau1:f1 ph11 ipp13 ipp14     ;c7 excitation, 1 loop = 2*Tr/7, 
                               ;increment reconversion pulse phase ph13 and ph14 pointers
                               ;to the next phase in the lists
  tau4:f1 ph12 ipp12           ;increment phase ph12 pointer
  tau3:f1 ph11 ipp11           ;increment phase ph11 pointer
                               ;to the next phase in the lists
  lo to 3 times l1

  d0                           ;DQ evolution period

6 tau1:f1 ph13                 ;c7 reconversion, 1 loop = 2*Tr/7,
  tau4:f1 ph14 ipp14           ;increment phase ph14 pointer
  tau3:f1 ph13 ipp13           ;increment phase ph13 pointer
                               ;to the next phase in the lists
  lo to 6 times l1

  (p1 pl1 ph5):f1              ;detection pulse
  2u
  gosc ph31                    ;gosc does not loop to 1
                               ;start ADC with ph31 signal routing

                               ;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 2 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= 0                         ;for saturation pulse

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)   0.00  51.43 102.86 154.29 205.71 257.14 308.57 
ph14 = (float,90.0) 180.00 231.43 282.86 334.29 385.71 437.14 488.57 

;ph11=(65536)     0  9362 18725 28087 37449 46811 56174 
;ph12=(65536) 32768 42130 51493 60855  4681 14043 23406
;ph13=(65536)     0  9362 18725 28087 37449 46811 56174 
;ph14=(65536) 32768 42130 51493 60855  4681 14043 23406 

ph5=   0 0 0 0 2 2 2 2 1 1 1 1 3 3 3 3
ph31 = 0 2 0 2 2 0 2 0 1 3 1 3 3 1 3 1    ;ph31 = ph5 + 2*ph13
  

Example: ³¹P in VPI-5 zeolite with AV500

Intensity of ³¹P POST C7 spectrum of zeolite VPI-5 versus the number of composite C7 cycles for DQ excitation; rotor spinning speed: 10 kHz.

Pulseprogram parameters for pc71d.ppm:

³¹P POST C7 DQ-SQ spectrum of VPI-5 zeolite; rotor spinning speed: 10 kHz.

Pulseprogram parameters for pc72d.ppm:

Acquisition parameters:

1. Javier Enrique de Oñate Martinez
   Structural investigations on the large-pore aluminophosphate molecular sieve VPI-5,
   Zürich, 1997.
   Dissertation

References

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    Definition of PC7 excitation pulse.

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    Chem. Phys. Lett. 242, 304-309 (1995).
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    Definition of C7 excitation pulse.

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    ¹³C---¹H dipolar recoupling dynamics in ¹³C multiple-pulse solid-state NMR,
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Solid-state NMR bibliography for: