PC72dlsw: 2D large double-quantum F1 spectral width POST_C7 pulse program

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Large double-quantum F1 spectral width 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.

2*del360 = τ1 + τ4 + τ3

*** Outline ***

Code for Avance III spectrometers with topSpin2.1 operating system

;pc72dlsw  (TopSpin 2.0)

;SQ-DQ experiment using POST_C7 sequence
;for setup use pc71d
;M. Hong ...
;Hohwy, M. Jakobsen, H.J. Eden, M. Levitt, M.H., Nielsen, N.C., 
;J. Chem. Phys. 108, 2686-2694 (1998)
;revised 11/19/03 JOS

;Avance II+ version
;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
;p1  : detection pulse at pl1

;cnst31 : spinning speed
;l0 : number of composite C7 cycles for DQ excitation 
;l1 : number of composite C7 cycles for DQ reconversion 
;l2 : number of 2/7 rotor revolutions for DQ evolution
;l3 : number of 2/7 rotor revolution increments for DQ evolution
;l20: # of pulses in saturation pulse train, 0 if undesired

;inf1: =l3*(2s/cnst31)/7, t1 increment
;FnMode : undefined
;ns  : 16*n
;WDW : F1 QSINE 3,  F2 QSINE 2 or EM

;$COMMENT=SQ-DQ experiment with post-C7 sequence, optimised for large sweep width
;$TYPE=direct excitation
;$SUBTYPE=homonuclear correlation

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

define delay del360


;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt

#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

3 tau1:f1 pl7: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 l0             ;l0 must be a multiple of 7

                               ;double-quantum evolution period
4 del360 ipp13 ipp14           ;increment reconversion pulse phase ph13 and ph14 pointers
  del360                       ;to the next phase in the lists
  lo to 4 times l2             ;del360 = (1s/cnst31)/7

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             ;l1 must be a multiple of 7

  (p1 pl1 ph5):f1              ;detection pulse

  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

7 1m iu2                       ;increment counter l2 in 2*Tr/7
  lo to 7 times l3

  ;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

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)  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 

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

Example: 31P in VPI-5 zeolite with AV500

31P 2D spectrum of VPI5 obtained with PC7lsw DQ pulse program

31P POST C7 DQ-SQ spectrum with large F1 spectral width of VPI-5 zeolite; rotor spinning speed: 10 kHz.

Pulseprogram parameters for pc72dlsw.ppm:

PULPROG pc72dlsw.ppm
TD 2048
NS 16
DS 0
SWH [Hz] 12500.00
AQ [s] 0.0820100
RG 4
DW [µs] 40.000
DE [µs] 6.50
CNST11 0.0000000
CNST31 10000.0000000
D1 [s] 10.00000000
D20 [s] 0.10000000
d31 [s] 0.00010000
in0 [s] 0.00002857
inf1 [s] 0.00002857
L1 59
l2 0
L3 1
L20 20
ZGOPTNS -Dpresat
count 200
del360 [s] 0.00001429
Channel f1  
NUC1 31P
P1 [µs] 3.00
PL1 [dB] 8.00
PL7 [dB] 7.80
SFO1 [MHz] 202.4830777
tau1 [µs] 3.57
tau2 [µs] 10.71
tau3 [µs] 14.29

Acquisition parameters:

  F2 F1
PULPROG pc72dlsw.ppm  
AQ_mod DQD  
FnMODE   undefined
TD 2048 400
NS 16  
DS 0  
TD0 1  
SW [ppm] 61.7336 172.8626
SWH [Hz] 12500.000 35001.750
IN_F [µs]   28.57
AQ [s] 0.0820100 0.0057140
NUC1 31P 31P
O1 [Hz] -1593.30 -1593.30
O1P [ppm] -7.869 -7.869
SFO1 [MHz] 202.4830777 202.4830777
BF1 [MHz] 202.4846710 202.4846710


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    PC7 pulse sequence

    Definition of PC7 excitation pulse.

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Solid-state NMR bibliography for:

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