CPMAS pulse program for topSpin2.1 operating system

;cp (TopSpin 2.0)

;basic cp experiment
;written by HF 1.3.2001
;changed by JOS 05/06/03
;comments added by STE 4.4.2006

;Avance II+ version
;parameters: 
;p3 : proton 90 at power level pl12
;p15 : contact time at pl1 (f1) and sp0 (f2)
;pl1 : X power level during contact
;sp0 : proton power level during contact
;pl2 : =120dB, not used
;pl12 : decoupling power level (if not pl13)
;pl13 : special decoupliong power level
;d1 : recycle delay
;cnst21 : on resonance, usually = 0
;pcpd2 : pulse length in decoupling sequence
;cpdprg2 : cw, tppm (at pl12), or lgs, cwlg, cwlgs (LG-decoupling) 
;here pl13 is used instead of pl12)
;spnam0 : use e.g. ramp.100 for variable amplitude CP
;zgoptns : -Dfslg, -Dlacq, or blank

;$COMMENT=basic cp experiment, arbitrary contact and decoupling schemes
;$CLASS=Solids
;$DIM=1D
;$TYPE=cross polarisation
;$SUBTYPE=simple 1D
;$OWNER=Bruker
prosol relations=<solids_cp>

#include <Avancesolids.incl>

#ifdef fslg
#include <lgcalc.incl>
;cnst20 : RF field achieved at pl13
;cnst21 : on resonance, usually = 0
;cnst22 : positive LG offset
;cnst23 : negative LG offset
;cnst24 : additional LG-offset
#endif /* fslg */
;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt
"acqt0=1u*cnst11"

1 ze        ;accumulate into an empty memory

2 d1 do:f2  ;recycle delay, decoupler off in go-loop
#include <p15_prot.incl>
            ;make sure p15 does not exceed 10 msec
            ;let supervisor change this pulseprogram if 
            ;more is needed
#ifndef lacq
            ;disable protection file for long acquisition change decoupling power !!!
            ;or you risk probe damage
            ;if you set the label lacq (ZGOPTNS -Dlacq), the protection is disabled

#include <aq_prot.incl>
            ;allows max. 50 msec acquisition time, supervisor
            ;may change  to max. 1s at less than 5 % duty cycle
            ;and reduced decoupling field
#endif

  1u fq=cnst21:f2
  (p3  ph1):f2 (1u pl12):f2            ;proton 90° pulse
  (p15 pl1 ph2):f1 (p15:sp0 ph10):f2   ;contact pulse with square or ramp shape ramp.100 on F2
  go=2 ph31 cpds2:f2                   ;select appropriate decoupling sequence 
                                       ;pl12 is used here with cw, tppm, spinal, pl13 with cwlg, cwlgs,
                                       ;pmlg-36 (x, -x, -x, x with PMLG-9), pmlg-2 (2 * pmlg-36), pmlg-4 (4 * pmlg-36), dumbo_1+0
  1m do:f2                             ;decoupler off
  wr #0                                ;save data to disk
HaltAcqu, 1m                           ;jump address for protection files
exit                                   ;quit

ph0=  0
ph1=  1 3
ph10= 0
ph2=  0 0 2 2 1 1 3 3
ph31= 0 2 2 0 1 3 3 1
  

Example1: FSLG ¹H -> ¹³C in adamantane with AV500

Frequency Switched Lee Goldberg heteronuclear decoupling

CP MAS pulse sequence with fslg decoupling

¹³C CP MAS spectrum of adamantane with fslg decoupling

Pulseprogram parameters for fslg:

1. Cristina Coelho, João Rocha, P. K. Madhu, and Luís Mafra
   Practical aspects of Lee-Goldburg based CRAMPS techniques for high-resolution ¹H NMR spectroscopy in solids: Implementation and applications,
   J. Magn. Reson. 194, 264-282 (2008).
   Abstract
2. Matthias Ernst, Aswin Verhoeven, and Beat H. Meier
   High-speed magic-angle spinning ¹³C MAS NMR spectra of adamantane: Self-decoupling of the heteronuclear scalar interaction and proton spin diffusion,
   J. Magn. Reson. 130, 176-185 (1998).
   Abstract
3. P. Tekely, P. Palmas, and D. Canet
   Effect of proton spin exchange on the residual ¹³C MAS NMR linewidths. Phase-modulated irradiation for efficient heteronuclear decoupling in rapidly rotating solids,
   J. Magn. Reson. A 107, 129-133 (1994).
   Abstract
4. T. Terao, H. Miura, and A. Saika
   Measurements of the ¹³C-¹H coupling constants in solid adamantane: Resolution enhancement by multiple-pulse decouplings,
   J. Magn. Reson. 49, 365-367 (1982).
   Abstract

Example2: PMLG ¹H -> ¹³C in adamantane with AV500

Phase Modulated Lee Goldberg heteronuclear decoupling

CP MAS pulse sequence with pmlg decoupling

¹³C CP MAS spectrum of adamantane with pmlg decoupling

Pulseprogram parameters for pmlg:

Example3: DUMBO-1 ¹H -> ¹³C in adamantane with AV500

Decoupling Under Mind Boggling Optimisation-1 heteronuclear decoupling

CP MAS pulse sequence with DUMBP-1 decoupling

¹³C CP MAS spectrum of adamantane with DUMBO-1 decoupling

Pulseprogram parameters for dumbo:

References

1. Ségolène Laage, Joseph R. Sachleben, Stefan Steuernagel, Roberta Pierattelli, Guido Pintacuda, and Lyndon Emsley
   Fast acquisition of multi-dimensional spectra in solid-state NMR enabled by ultra-fast MAS,
   J. Magn. Reson. 196, 133-141 (2009).
   Abstract
2. Erin E. Wilson, Ayorinde Awonusi, Michael D. Morris, David H. Kohn, Mary M. J. Tecklenburg, and Larry W. Beck
   Three structural roles for water in bone observed by solid-state NMR,
   Biophys. J. 90, 3722-3731 (2006).
   Abstract
3. Pellegrino Conte, Riccardo Spaccini, and Alessandro Piccolo
   State of the art of CPMAS ¹³C-NMR spectroscopy applied to natural organic matter,
   Prog. Nucl. Magn. Reson. Spectrosc. 44, 215-223 (2004).
   Abstract
4. Riqiang Fu, Jun Hu, and Timothy A. Cross
   Towards quantitative measurements in solid-state CPMAS NMR: A Lee-Goldburg frequency modulated cross-polarization scheme,
   J. Magn. Reson. 168, 8-17 (2004).
   Abstract
5. S. Reinhard and J. Blümel
   ³¹P CP/MAS NMR of polycrystalline and immobilized phosphines and catalysts with fast sample spinning,
   Magn. Reson. Chem. 41, 406-416 (2003).
   Abstract
6. Mei Hong, Xiaolan Yao, Karen Jakes, and Daniel Huster
   Investigation of molecular motions by Lee-Goldburg cross-polarization NMR spectroscopy,
   J. Phys. Chem. B 106, 7355-7364 (2002).
   Abstract
7. Vladimir Ladizhansky and Shimon Vega
   Polarization transfer dynamics in Lee-Goldburg cross polarization nuclear magnetic resonance experiments on rotating solids,
   J. Chem. Phys. 112, 7158-7168 (2000).
   Abstract
8. 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
9. P. Tekely, V. Gérardy, P. Palmas, D. Canet, and A. Retournard
   Measurement of Hartmann-Hahn cross-polarization dynamics with quenching of proton T1ρ relaxation dependence,
   Solid State Nucl. Magn. Reson. 4, 362-367 (1995).
   Abstract
10. S. Hediger, B. H. Meier, and R. R. Ernst
    Rotor-synchronized amplitude-modulated nuclear magnetic resonance spin-lock sequences for improved cross polarization under fast magic angle sample spinning,
    J. Chem. Phys. 102, 4000-4011 (1995).
    Abstract
11. G. Metz, X. Wu, and S. O. Smith
    Ramped-amplitude cross polarization in magic-angle-spinning NMR,
    J. Magn. Reson. A 110, 219-227 (1994).
    Abstract
12. P. Tekely, P. Palmas, and D. Canet
    Effect of proton spin exchange on the residual ¹³C MAS NMR linewidths. Phase-modulated irradiation for efficient heteronuclear decoupling in rapidly rotating solids,
    J. Magn. Reson. A 107, 129-133 (1994).
    Abstract

Solid-state NMR bibliography for: