C14_4^5bsw-2d: 2D big F1 spectral width double quantum / single quantum correlation C14₄⁵ pulse program (TopSpin2.1)

*** Outline ***

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

Code for Avance III spectrometers with topSpin2.1 operating system

;c14-4-52dbsw (TopSpin 2.1)

;2D SQ-DQ correlation experiment with C14_4^5 sequence
;by GALT, Nov. 2, 2001
;DQ correlation - inadequate type sequence
;C14_4^5 sequence for lower RF requirements (as compared e.g. to C7)
;for setup use c14-4-51d
;requires high spin rates to cover large frequency range (e.g. 20 kHz at 600 MHz)

;Avance III version
;parameters:
;d0 : =0.1u, t1 evolution
;d1 : recycle delay

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

;pl11 : Power level for C14_4^5 recoupling sequence B1=3.5*cnst31 in Hz

;cnst10 : =-180*cnst31*d0, recalculated during acquisition
;cnst31 : spinning frequency
;l0 : number of composite C14_4^5 cycles (usually a multiple of 7)
;ndo : 1
;FnMode : undefined
;mc2 : STATES-TPPI
;WDW : f1 QSINE 3, f2 QSINE 2 or EM
;use "xau xfshear rotate" to shift spectrum suitably along f1
;ns  : = 16*n
;zgoptns :-Dpresat or blank

;$COMMENT=SQ-DQ experiment with C14_4^5 sequence
;$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 tau2
  "tau2=((1s/cnst31)/7)"       ;180° pulse

  "d31=1s/cnst31"              ;one rotor period

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

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

  ze
  "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

  "cnst10=-180*cnst31*d0"      ;phase correction for C14_4^5 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 C14_4^5 RF condition

                               ;C14_4^5 excitation
3 (tau2 ph11 ipp11 ipp13 ipp14):f1  ;first 180° C14_4^5 excitation pulse at pl11
                               ;increment phase ph11 pointer
                               ;increment reconversion pulse phase ph13 and ph14 pointers
  (tau2 ph12 ipp12):f1              ;second 180° C14_4^5 excitation pulse, 
                               ;increment phase ph12 pointer
  lo to 3 times l0             ;l0 = multiple of 14

  d0                           ;DQ evolution period

                               ;C14_4^5 reconversion
4 (tau2 ph13+cnst10 ipp13):f1       ;first 180° C14_4^5 reconversion pulse, 
                               ;increase ph13 by cnst10 due to evolution period, 
                               ;increment phase ph13 pointer
  (tau2 ph14+cnst10 ipp14):f1       ;second 180° C14_4^5 reconversion pulse, 
                               ;increase ph14 by cnst10 due to evolution period, 
                               ;increment phase ph14 pointer
  lo to 4 times l0             ;l0 = multiple of 14

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

                               ;DQ filtering (four phase cycling):
  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          ;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 pulses

ph11=(65536)    0 23406 46811  4681 28087 51493  9362     ;C14_4^5(0..6)
            32768 56174 14043 37449 60855 18725 42130     ;C14_4^5(7..13)
ph12=(65536)    0 23406 46811  4681 28087 51493  9362
            32768 56174 14043 37449 60855 18725 42130

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

                               ;;C14_4^5 excitation and reconversion pulse phases
                               ;are identical

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