wpmlg2d: homonuclear dipole-dipole pmlg decoupling pulse program for TopSpin2.1




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Code for Avance III spectrometers with topSpin2.1 operating system

;wpmlg2d (TOPSPIN 2.1)
;windowed PMLG homonuclear decoupling, digital mode, proton-proton spin diffusion 2D experiment
;purified version according to Leskes, Madhu and Vega, Chem. Phys. Lett., in press
;using shapes for wpmlg
;HF 26.09.07
;spin 10-15 kHz according to RF field
;set: 
;p9 2.4-4.5 usec, depending on probe deadtime, usually:
;for 200 and 300 MHz, CRAMPS probe required or use 4.5 usec
;use digital mode, swh=10-20 kHz
;before ft, set s sw=sw/0.58

;set:
;d1 : recycle delay

;p1 : proton 90 degree pulse at pl12
;set o1p around 10 ppm or -4 ppm, usually better on left side of spectrum

;pl12 : power level for initial pulses
;pl13 : power level for pmlg, set cnst20 to RF field at pl13, for simplicity, use pl13=pl12
;       sensible proton RF-field: 80 000 Hz for 300-400 MHz proton frequency, 100000 for 500-600 MHz
;       120000 for 600 MHz and higher (due to probe bandwidth differences)
;ns=n*4
;spnam1=m5m or m3m, m5p or m3p 
;shape consists of 10 (6) slices of length 2*p5/10 (/6), 
;set cnst20 for approximate RF field, adjust power for best result, 
;shape duration recalculated so slice is a multiple of 100 ns
;set l11=number of oversampled datapoints to be sampled, 8-32 depending on
;    available window, check acqu in ased for sensible value.
;select Fn_Mode STATES-TPPI to be able to correct for peak folding
;set l3 and swh such that scaledsw and scaledsw1 are calculated as close as possible

;$COMMENT=homonuclear decoupling with w-pmlg
;$CLASS=Solids
;$DIM=2D
;$TYPE=homonuclear decoupling
;$SUBTYPE=explicit acquisition

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

dwellmode auto

#include <Avancesolids.incl>
#include <Delayssolids.incl>
#include <lgcalc.incl>  /*;set cnst20 to RF field at pl13, wpmlg pulse calculated as multiple of 100 ns */

  "sp1=pl13"
  "d3=p9"                     ;p9 sets the window to make sure it is in micorseconds
  "d9=0.1u*(l11)"             ;set the sampling window in Avancesolids.incl
  "inf1=(l3*(d3+p5))*4"       ;t1 increment
  "l0=0"                      ;reset F1 dwell counter
  "blktr2 = 0.7u"             ;this opens the transmitter gate 0.7 usec before the
                              ;pulse, so the transmitter noise is not sampled

define delay dead
  "dead=1.2u"
define delay acqu             ;small window, defined by d3, 2.5-4.5 usec depending
  "acqu=2*p9-1.2u-d9-.1u"     ;on probe deadtime large window-sampling period
                              ;make sure shape slice durations are a multiple of 0.1 usec
define loopcounter smooth
  "smooth=10*p5"
define pulse polish
  "polish=1u*smooth/10"
define pulse wpmlg
  "wpmlg=2*polish"
define delay cycle
  "cycle=4*p9+2*wpmlg+.2u"
define loopcounter count
  "count=aq/cycle"            ;make sure td datapoints are sampled
define delay rest             ;make sure sampling proceeds throughout the sequence
  "rest=aq-(count*cycle)"

define loopcounter scaledsw1
  "scaledsw1=(1/l3*cycle)/0.47"
define loopcounter scaledsw
  "scaledsw=1e6/(2*dw*0.47)" 
define loopcounter setswh
  "setswh=scaledsw1*0.47"
define delay realdwell1
  "realdwell1=2/scaledsw1"    ;effective dwell is cycle time *scaling factor
define delay realdwell
  "realdwell=2/scaledsw"
define delay setdwell
  "setdwell=2/setswh"

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

1 ze                          ;acquire into a cleared memory
  realdwell1                  ;show calculated dwell and swh in F1 
  realdwell
  setdwell
2 d1 pl12:f1                  ;recycle delay
  10u reset1:f1               ;synchronise pulse and detection RF
  p1:f1 ph0                   ;first 90 at pl12

3 d3 pl13:f1
  d3
  (wpmlg:sp1  ph11^):f1
  d3
  d3
  (wpmlg:sp1  ph11^):f1
  lo to 3 times l0
  p1:f1 ph5

  d8                          ;mixing
  STARTADC                    ;prepare adc for sampling, set reference frequency, defined in Avancedru.incl
  RESETPHASE                  ;reset reference phase

  (p1 pl12 ph1):f1
  .1u DWL_CLK_ON
4 dead  pl13:f1
  acqu
  d9 RG_ON
  .1u RG_OFF                  ;take l11 complex data points
  (wpmlg:sp1  ph10^):f1
  dead
  acqu
  d9 RG_ON
  .1u RG_OFF
  (wpmlg:sp1  ph10^):f1
  lo to 4 times count         ;make sure td points are sampled
  rest
  1u  DWL_CLK_OFF
  rcyc=2                      ;next scan
5 100m wr #0 if #0 zd         ;save data

  1m ip0                      ;90° phase increment
  lo to 2 times 2             ;t1 quadrature detection

6 1m iu0*l3
  1m
  lo to 2 times nrows         ;nrows=td1/2
  exit                        ;finished



ph0= 0
ph1= 1 2 3 0
ph2= 0 
ph4= 0
ph5= 2
ph10=0 2
ph11=0 2
ph30=0
ph31=1 2 3 0
  

References

  1. Subhradip Paul, Rajendra Singh Thakur, Mithun Goswami, Andrea C. Sauerwein, Salvatore Mamone, Maria Concistrč, Hans Förster, Malcolm H. Levitt, and P. K. Madhu
    Supercycled homonuclear dipolar decoupling sequences in solid-state NMR,
    J. Magn. Reson. 197, 14-19 (2009).
    Abstract
     
  2. Michal Leskes, P. K. Madhu, and Shimon Vega
    Proton line narrowing in solid-state nuclear magnetic resonance: New insights from windowed phase-modulated Lee-Goldburg sequence,
    J. Chem. Phys. 125, 124506/1-124506/18 (2006).
    Abstract
     

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