SPC52dbigsw: 2D big double-quantum F1 spectral width SPC5 pulse program for TopSpin2.1

*** Outline ***

• Code for Avance III spectrometers with topSpin2.1 operating system
• Example: ³¹P in VPI-5 zeolite with AV700
• References

Code for Avance III spectrometers with topSpin2.1 operating system

;spc52dbigsw  (TopSpin 2.1)
;modified for AVIII by HF, May 14, 07

;2D SQ-DQ correlation experiment with SPC5 sequence
;for the original C7 sequence see: Lee et al. Chem Phys Lett 242, 304-309, 1995
;see Hohwy, Rienstra, Jaroniec and Griffin, JCP 110, 7983, 1999

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

;p1 : f1 presaturation pulses and detection pulse at pl1
;p9 : used as t1 increment for d0

;pl2  : =120dB, not used
;pl11 : for SPC5 recoupling sequence B1=5*cnst31 in Hz

;cnst31 : spinning speed
;l0  : number of composite SPC5 cycles multiple of 5 in DQ excitation
;l2  : number of composite SPC5 cycles multiple of 5 in DQ reconversion
;l20 : # of pulses in saturation pulse train
;ns : 16*n
;FnMode : undefined
;mc2 : STATES-TPPI
;nd0 : 1
;WDW : F1 QSINE 3,  F2 QSINE 2 or EM
;use "xau xfshear rotate" to shift spectrum suitably along f1
;zgoptns :-Dpresat or blank

;$COMMENT=SQ-DQ experiment with SPC5 sequence
;$CLASS=Solids
;$DIM=2D
;$TYPE=direct excitation
;$SUBTYPE=homonuclear correlation
;$OWNER=Bruker

define pulse pul360
  "pul360=(1s/cnst31)/5"    ;360° pulse
define pulse pul90
  "pul90=(0.25s/cnst31)/5"  ; 90° pulse
define pulse pul270
  "pul270=(0.75s/cnst31)/5" ;270° pulse

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

  "d31=(1s/cnst31)"

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

#include <rot_prot.incl>
                            ;protect for too slow rotation

  ze                        ;acquire into a cleared memory

  "d0=0.1u"                 ;make sure a short d0 is used initially

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                        ;recycle delay

  "cnst1=180*cnst31*d0"     ;phase correction for SPC5 reconversion pulse,
                            ;due to t1 DQ evolution period,
                            ;defined by the phase-time relationships

  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 pl11:f1                ;switch to SPC5 RF condition

3 pul90  ph11 ipp13 ipp14   ;SPC5 DQ excitation
                            ;increment reconversion phase ph13 and ph14 pointers
  pul360 ph12 ipp12         ;increment phase ph12 pointer
  pul270 ph11 ipp11         ;increment phase ph11 pointer
  lo to 3 times l0          ;l0 = multiple of 5

4 d0                        ;double-quantum evolution period

5 pul90  ph13+cnst1         ;SPC5 DQ reconversion
                            ;increase ph13 by cnst1 due to evolution period
  pul360 ph14+cnst1 ipp14   ;increase ph14 by cnst1 due to evolution period,
                            ;increment phase ph14 pointer
  pul270 ph13+cnst1 ipp13   ;increase ph13 by cnst1 due to evolution period,
                            ;increment phase ph13 pointer
  lo to 5 times l2          ;l2 = multiple of 5

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

                            ;DQ filtering (four phase cycling):
  40u ip13*16384            ;increments all phases of ph13 by 90°
  40u ip14*16384            ;increments all phases of ph14 by 90°
  lo to 1 times ns          ;next scan

  100m wr #0 if #0 zd       ;delay for disk I/O, store signal,
                            ;increase FID number
                            ;delete memory data
                            ;do not perform dummy scans
                            ;with next acquisition

  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

  "d0=d0+p9"                ;set p9=increment for F1 (to make it usec!)

  ;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= (65536)     0 13107 26214 39322 52429 32768 45875 58982  6554 19661
ph12= (65536) 32768 45875 58982  6554 19661     0 13107 26214 39322 52429
ph13= (65536) 16384 29491 42598 55706  3277 49152 62259  9830 22937 36044
ph14= (65536) 49152 62259  9830 22937 36044 16384 29491 42598 55706  3277

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