dumbod2: homonuclear dipole-dipole windowed-dumbo decoupling pulse program for TopSpin2.1

;dumbod2 (TOPSPIN 2.1)
;windowed DUMBO homonuclear decoupling, digital mode, 
;Leskes, Madhu and Vega, Chem. Phys. Lett. modification to remove center spike
;HF 26.9.2007

;spin 10-13 kHz according to RF field
;p9 2.4-4.5 usec, depending on probe deadtime, usually:
;for 200 and 300 MHz, CRAMPS probe required or use 4.5 usec,
;acqu or p9 must be as short as possible, avoiding dipolar coupling effects between DUMBO sequences,
;l11 or d9 must be as large as possible to improve S/N ratio, but keeping acqu positive,
;before ft, set s sw=sw/0.50

;set:
;d1 : recycle delay
;p1 : proton 90 degree pulse at pl12
;set o1p close to resonance
;pl12 : power level for initial pulse,
;pl13 : power level for DUMBO
;ns=n*4
;spnam1=dumbo1, generated and set with au program dumbo; chose 1 cycle; uses p10 pulse
;at lower field, p10 is used as set (=32 usec), at higher field (500 MHz and up) 24 usec is better
;at higher power, of course.
;set l11=number of oversampled data points to be averaged into one dwell point, 2-32 depending on
;available window, more oversampled data points improve S/N, check acqu in ased to be finite

;$COMMENT=homonuclear decoupling with dumbo
;$CLASS=Solids
;$DIM=1D
;$TYPE=homonuclear decoupling
;$SUBTYPE=explicit acquisition

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

"sp1=pl13"

dwellmode auto

#include <Avancesolids.incl>
#include <Delayssolids.incl>
  "d9=0.1u*(l11)"               ;set the sampling window, defined in Avancesolids.incl
define delay dead
  "dead=1.2u"
define delay acqu               ;small window defined by p9, 2.5-4.5 usec depending
  "acqu=2*p9-1.2u-d9-.1u"       ;on probe deadtime
                                ;acqu or p9 must be as short as possible, avoiding dipolar coupling effects
                                ;l11 or d9 must be as large as possible but keeping acqu positive
define delay cycle
  "cycle=4*p9+2*p10+.1u"
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 pulse dumbop
  "dumbop=p10"                  ;p10 provided by au program dumbo
  "blktr2 = 0.6u"               ;this opens the transmitter gate 0.6 usec before the
                                ;pulse, so the transmitter noise is not sampled

1 ze                            ;acquire into a cleared memory
2 d1 pl12:f1                    ;recycle delay
  10u reset1:f1                 ;synchronise pulse and detection RF
  STARTADC                      ;prepare adc for sampling, set reference frequency, defined in Avancesolids.incl
  RESETPHASE                    ;reset reference phase
  1u rpp10                      ;reset phase list pointer
  p1:f1 ph1                     ;first 90 at pl12
  .1u DWL_CLK_ON
4 dead
  acqu
  d9 RG_ON
  .1u RG_OFF                    ;take l11  complex data points	
  (dumbop:sp1 ph10^):f1
  dead
  acqu
  d9 RG_ON
  .1u RG_OFF
  (dumbop: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                    ;save data
6 exit                          ;finished


ph0= 0
ph1= 0 1 2 3
ph10=0 2
ph30=0
ph31=0 1 2 3
  

Example-1: ¹H in Glycine with AV500

¹H windowed DUMBO spectrum of glycine in a 4-mm diameter, 12-µL HRMAS rotor spinning at 10 kHz; P10 = 27 µs, H-XY probe; Glycine viewed with Jmol.

Pulseprogram parameters for dumbod2.ppm:

¹H windowed DUMBO spectrum of glycine in a 4-mm diameter, 12-µL HRMAS rotor spinning at 10 kHz; P10 = 24 µs.

Pulseprogram parameters for dumbod2:

¹H windowed DUMBO spectrum of glycine in a 4-mm diameter, 12-µL HRMAS rotor spinning at 10 kHz; P10 = 36 µs.

Pulseprogram parameters for dumbod2:

¹H windowed DUMBO spectra of glycine in a 4-mm diameter, 12-µL HRMAS rotor spinning at 10 kHz; H-XY probe, for 5 DUMBO pulse duration p10 values (23.6, 23.8, 24.0, 24.2, and 24.4 µsec).

¹H windowed DUMBO spectra of glycine in a 4-mm diameter, 12-µL HRMAS rotor spinning at ω_rotor = 10 kHz and an H-XY probe, for 2 DUMBO pulse duration p10 values: 26 µsec (blue spectrum) and 27 µsec (red spectrum); rotor-RF peaks are located at 5808, 5345, 4668, and 4169 Hz relative to the carrier frequency.

The position f of a rotor-RF peak is defined by f = m*ω_rotor + n/p10, where f, ω_rotor, and p10 are expressed in Hz, kHz, and msec units, respectively.

The two rotor-RF peak positions 4169 and 4668 Hz allow us to determine the equation for the low frequency peak:
f_L = 1764 ω_rotor - 350/p10

The other two rotor-RF peak positions 5345 and 5808 Hz allow us to determine the equation for the high frequency peak:
f_H = -642 ω_rotor + 318/p10

Pulseprogram parameters for dumbod2.ppm:

¹H windowed DUMBO spectrum of glycine in a 4-mm diameter, 12-µL HRMAS with several rotor spinning speeds; P10 = 24 µs.

Pulseprogram parameters for dumbod2:

1. Renée Siegel, Luís Mafra, and João Rocha
   Improving the ¹H indirect dimension resolution of 2D CRAMPS NMR spectra: A simulation and experimental investigation,
   Solid State Nucl. Magn. Reson. 39, 81-87 (2011).
   Abstract
2. Lorenzo Stievano, Frederik Tielens, Irne Lopes, Nicolas Folliet, Christel Gervais, Dominique Costa, and Jean-François Lambert
   Density functional theory modeling and calculation of NMR parameters: An ab initio study of the polymorphs of bulk glycine,
   Cryst. Growth Des. 10, 3657-3667 (2010).
   Abstract
3. Jean-Paul Amoureux, Bingwen Hu, Julien Trébosc, Qiang Wang, Olivier Lafon, and Feng Deng
   Homonuclear dipolar decoupling schemes for fast MAS,
   Solid State Nucl. Magn. Reson. 35, 19-24 (2009).
   Abstract
4. Waclaw Kolodziejski and Avelino Corma
   ²H → ¹H cross-polarization in deuterated glycine ,
   Solid State Nucl. Magn. Reson. 7, 67-72 (1996).
   Abstract

Example-2: ¹H in L-tyrosine.HCl with AV500 and AV700

¹H windowed DUMBO spectrum of L-tyrosine-HCl in a 4-mm diameter, 12-µL HRMAS rotor spinning at 10 kHz; P10 = 24 µs; L-tyrosine viewed with Jmol.

Pulseprogram parameters for dumbod2:

¹H windowed DUMBO spectrum of L-tyrosine-HCl in a 4-mm diameter, 12-µL HRMAS rotor spinning at 10 kHz; P10 = 27 µs, H-XY probe.

Pulseprogram parameters for dumbod2.ppm:

¹H one-pulse spectrum of L-tyrosine-HCl in a 2.5-mm diameter rotor spinning at 30 kHz; P1 = 2.3 µs; PL1 = 2.25 dB; AV700SB.

¹H windowed DUMBO spectrum of L-tyrosine-HCl in a 2.5-mm diameter rotor spinning at 15 kHz; P10 = 36 µs, AV700SB.

Pulseprogram parameters for dumbod2:

1. Luis Mafra, Renée Siegel, Christian Fernandez, Denis Schneider, Fabien Aussenac, and João Rocha
   High-resolution ¹H homonuclear dipolar recoupling NMR spectra of biological solids at MAS rates up to 67 kHz,
   J. Magn. Reson. 199, 111-114 (2009).
   Abstract
2. B.-J. van Rossum, C. P. de Groot, V. Ladizhansky, S. Vega, and H. J. M. de Groot
   A method for measuring heteronuclear (¹H-¹³C) distances in high speed MAS NMR,
   J. Am. Chem. Soc. 122, 3465-3472 (2000).
   Abstract
3. B.-J. van Rossum, H. Förster, and H. J. M. de Groot
   High-field and high-speed CP-MAS ¹³C NMR heteronuclear dipolar-correlation spectroscopy of solids with frequency-switched Lee-Goldburg homonuclear decoupling,
   J. Magn. Reson. 124, 516-519 (1997).
   Abstract
4. Anne Lesage, Dimitris Sakellariou, Stefan Steuernagel, and Lyndon Emsley
   Carbon-proton chemical shift correlation in solid-state NMR by through-bond multiple-quantum spectroscopy,
   J. Am. Chem. Soc. 120, 13194-13201 (1998).
   Abstract
5. Elena Vinogradov, P. K. Madhu, and Shimon Vega
   Phase modulated Lee-Goldburg magic angle spinning proton nuclear magnetic resonance experiments in the solid state: A bimodal Floquet theoretical treatment,
   J. Chem. Phys. 115, 8983-9000 (2001).
   Abstract
6. Elena Vinogradov, P. K. Madhu, and Shimon Vega
   A bimodal Floquet analysis of phase modulated Lee-Goldburg high resolution proton magic angle spinning NMR experiments,
   Chem. Phys. Lett. 329, 207-214 (2000).
   Abstract
7. Michal Leskes, Stefan Steuernagel, Denis Schneider, P. K. Madhu, and Shimon Vega
   Homonuclear dipolar decoupling at magic-angle spinning frequencies up to 65 kHz in solid-state nuclear magnetic resonance,
   Chem. Phys. Lett. 466, 95-99 (2008).
   Abstract

Example-3: ¹H in L-lysine with AV500

¹H windowed DUMBO spectrum of L-lysine in a 4-mm diameter, 12-µL HRMAS rotor spinning at 10 kHz; P10 = 24 µs; L-lysine viewed with Jmol.

Pulseprogram parameters for dumbod2:

1. Caltec, Division of Geological and Planetary Sciences, Geoffrey A. Blake:
   Spectroscopic Methods in Biochemistry (PDF file)
2. Régis D. Gougeon, Marc Reinholdt, L. Delmotte, Jocelyne Miehé-Brendlé, and Philippe Jeandet
   Solid-state NMR investigation on the interactions between a synthetic montmorillonite and two homopolypeptides,
   Solid State Nucl. Magn. Reson. 29, 322-329 (2006).
   Abstract

Example-4: ¹H in MgO with AV500

¹H windowed DUMBO spectrum of MgO in a 4-mm diameter rotor spinning at ω_rotor = 10 kHz; P10 = 24 µs; H-XY probe; n = 1 before the scaling of the F2 axis and n = 2 after the scaling of the F2 axis.

Pulseprogram parameters for dumbod2.ppm:

1. Céline Chizallet, Hugo Petitjean, Guylène Costentin, Hélène Lauron-Pernot, Jocelyne Maquet, Christian Bonhomme, and Michel Che
   Identification of the OH groups responsible for kinetic basicity on MgO surfaces by ¹H MAS NMR,
   J. Catal. 268, 175-179 (2009).
   Abstract
2. Céline Chizallet, Guylène Costentin, Hélène Lauron-Pernot, Michel Che, Christian Bonhomme, Jocelyne Maquet, Françoise Delbecq, and Philippe Sautet
   Study of the structure of OH groups on MgO by 1D and 2D ¹H MAS NMR combined with DFT cluster calculations,
   J. Phys. Chem. C 111, 18279-18287 (2007).
   Abstract
3. Céline Chizallet, Guylène Costentin, Hélène Lauron-Pernot, Jocelyne Maquet, and Michel Che
   ¹H MAS NMR study of the coordination of hydroxyl groups generated upon adsorption of H₂O and CD₃OH on clean MgO surfaces,
   Appl. Catal. A 307, 239-244 (2006).
   Abstract

Example-5: ¹H in L-alanine with AV500

¹H windowed DUMBO spectrum of L-alanine in a 4-mm diameter, 80-µL rotor spinning at 10 kHz; P10 = 27 µs, H-XY probe; L-alanine viewed with Jmol.

Pulseprogram parameters for dumbod2.ppm:

1. Wen-Qing Wang, Wei Min, Zhi Liang, Li-Ying Wang, Lei Chen, and Feng Deng
   NMR and parity violation: low-temperature dependence in ¹H CRAMPS and ¹³C CP/MAS ssNMR spectra of alanine enantiomer,
   Biophys. Chem. 103, 289-298 (2003).
   Abstract
2. Anne Lesage, Luminita Duma, Dimitris Sakellariou, and Lyndon Emsley
   Improved resolution in proton NMR spectroscopy of powdered solids,
   J. Am. Chem. Soc. 123, 5747-5752 (2001).
   Abstract
3. Ingo Schnell, Adonis Lupulescu, Siegfried Hafner, Dan E. Demco, and Hans W. Spiess
   Resolution enhancement in multiple-quantum MAS NMR spectroscopy,
   J. Magn. Reson. 133, 61-69 (1998).
   Abstract

References

1. Meghan E. Halse and Lyndon Emsley
   A common theory for phase-modulated homonuclear decoupling in solid-state NMR,
   Phys. Chem. Chem. Phys. 14, 9121-9130 (2012).
   Abstract
2. Paul Hogdkinson
   High-resolution ¹H NMR spectroscopy of solids,
   Annu. Rep. Nucl. Magn. Reson. Spectrosc. 72, 185-223 (2011).
   Abstract, Google book
3. Andreas Brinkmann, Suresh Kumar Vasa, Hans Janssen, and Arno P. M. Kentgens
   Proton micro-magic-angle-spinning NMR spectroscopy of nanoliter samples,
   Chem. Phys. Lett. 485, 275-280 (2010).
   Abstract
4. Olivier Lafon, Qiang Wang, Bingwen Hu, Julien Trébosc, Feng Deng, and Jean-Paul Amoureux
   Proton-proton homonuclear dipolar decoupling in solid-state NMR using rotor-synchronized z-rotation pulse sequences,
   J. Chem. Phys. 130, 014504/1-014504/13 (2009).
   Abstract
5. Elodie Salager, Robin S. Stein, Stefan Steuernagel, Anne Lesage, Bénédicte Elena, and Lyndon Emsley
   Enhanced sensitivity in high-resolution ¹H solid-state NMR spectroscopy with DUMBO dipolar decoupling under ultra-fast MAS,
   Chem. Phys. Lett. 469, 336-341 (2009).
   Abstract
6. Subhradip Paul, Rajendra Singh Thakur, Mithun Goswami, Andrea C. Sauerwein, Salvatore Mamone, Maria Concistrè, 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
7. P. K. Madhu
   High-resolution solid-state NMR spectroscopy of protons with homonuclear dipolar decoupling schemes under magic-angle spinning,
   Solid State Nucl. Magn. Reson. 35, 2-11 (2009).
   Abstract
8. Michal Leskes, Stefan Steuernagel, Denis Schneider, P. K. Madhu, and Shimon Vega
   Homonuclear dipolar decoupling at magic-angle spinning frequencies up to 65 kHz in solid-state nuclear magnetic resonance,
   Chem. Phys. Lett. 466, 95-99 (2008).
   Abstract
9. Michal Leskes, P. K. Madhu, and Shimon Vega
   A broad-banded z-rotation windowed phase-modulated Lee-Goldburg pulse sequence for ¹H spectroscopy in solid-state NMR,
   Chem. Phys. Lett. 447, 370-374 (2007).
   Abstract

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