Home and Applets
> Pulse Program
> 2Q/1Q Correlation
> 2D Big DQ F1 Spectral Width POST_C7 Pulse Program

Since non-phase cycling is applied to the PC7 excitation pulse, four-phase cycling is applied to the detection pulse P1 for selecting the 0Q -> -1Q coherence order jump, and four-phase cycling is applied to the PC7 reconversion pulse for filtering DQ coherences.


Andreas Brinkmann, Mattias Edén, and Malcolm H. Levitt, Synchronous helical pulse sequences in magic-angle spinning nuclear magnetic resonance: Double quantum recoupling of multiple-spin systems, J. Chem. Phys. 112, 8539-8554 (2000).
Code for Avance III spectrometers with topSpin2.1 operating system
;pc72dbigsw (TopSpin 2.0) ;SQ-DQ experiment using POST_C7 sequence ;for setup of the 2D INADEQUATE type experiments ;Hohwy, M. Jakobsen, H.J. Eden, M. Levitt, M.H., Nielsen, N.C., ;J. Chem. Phys. 108, 2686-2694 (1998) ;revised 09/09/03 JOS ;Avance II+ version ;parameters: ;d1 :recycle delay ;d0 : incremented delay (2D) [1 usec] ;d20 :delay between saturation pulses ;pl1 : f1 power level for presaturation pulses and detection pulse ;pl7 : for C7 recoupling sequence, B1=7*cnst31 in Hz ;pl2 : =120 dB, not used here ;p1 : detection pulse at pl1 ;p9 : used as t1 increment (= inf1) for d0 ;cnst31 : spinning speed, make sure cnst31>1000 ;l1 : number of composite C7 cycles for DQ excitation ;l20 : # of pulses in saturation pulse train, 0 if undesired ;FnMode : undefined because the pulse program contains no mc statement ;mc2 : STATES-TPPI ;nd0 : 1 ;ns : n*16 ;WDW : F1 QSINE 3, F2 QSINE 2 or EM ;zgoptns :-Dpresat or blank ;$COMMENT=SQ-DQ experiment with post-C7 sequence ;$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 tau1 "tau1=((0.25s/cnst31)/7)" ; 90° pulse define pulse tau4 "tau4=((1s/cnst31)/7)" ;360° pulse define pulse tau3 "tau3=((0.75s/cnst31)/7)" ;270° pulse "d31=1s/cnst31" ;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt "acqt0=1u*cnst11" #include <rot_prot.incl> 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 lo to pres times l20 #endif /* presat */ 2 d1 ;recycle delay "cnst1=180*cnst31*d0" ;phase correction for PC7 reconversion pulse ;due to t1 DQ evolution period, ;defined by the phase-time relationships 1m rpp11 ;reset the phase program ph11 pointer to the first element 1m rpp12 ;reset the phase program ph12 pointer to the first element 1m rpp13 ;reset the phase program ph13 pointer to the first element 1m rpp14 ;reset the phase program ph14 pointer to the first element 1u pl7:f1 ;switch to PC7 RF condition 3 tau1:f1 ph11 ipp13 ipp14 ;pc7 excitation, 1 loop = 2*Tr/7, ;increment reconversion pulse phase ph13 and ph14 ;pointers to the next phase in the lists tau4:f1 ph12 ipp12 ;increment phase ph12 pointer tau3:f1 ph11 ipp11 ;and phase ph11 pointer ;to the next phase in the lists lo to 3 times l1 d0 ;double-quantum evolution period 6 tau1:f1 ph13+cnst1 ;pc7 reconversion, 1 loop = 2*Tr/7, ;increase ph13 by cnst1 due to evolution period tau4:f1 ph14+cnst1 ipp14 ;increase ph14 by cnst1 due to evolution period, ;increment phase ph14 pointer to the next phase in the list tau3:f1 ph13+cnst1 ipp13 ;increase ph13 by cnst1 due to evolution period, ;increment phase ph13 pointer to the next phase in the list lo to 6 times l1 (p1 pl1 ph5):f1 ;detection pulse 2u gosc ph31 ;gosc does not loop to 1 ;start ADC with ph31 signal routing ;DQ filtering (four phase cycling): ;1m ip13 ;increments all phases of ph13 by 90° ;1m ip14 ;increments all phases of ph14 by 90° 1m ip13*16384 ;increments all phases of ph13 by 90° 1m ip14*16384 ;increments all phases of ph14 by 90° lo to 2 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 ;increments all phases of ph11 by 45°, ;90° phase for DQ coherence ;1m ip12 ;increments all phases of ph12 by 45°, ;90° phase for DQ coherence 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=inf1=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 = (float,45.0) 0.00 51.43 102.86 154.29 205.71 257.14 308.57 ;ph12 = (float,45.0) 180.00 231.43 282.86 334.29 385.71 437.14 488.57 ;ph13 = (float,90.0) 0.00 51.43 102.86 154.29 205.71 257.14 308.57 ;ph14 = (float,90.0) 180.00 231.43 282.86 334.29 385.71 437.14 488.57 ph11=(65536) 0 9362 18725 28087 37449 46811 56174 ph12=(65536) 32768 42130 51493 60855 4681 14043 23406 ph13=(65536) 0 9362 18725 28087 37449 46811 56174 ph14=(65536) 32768 42130 51493 60855 4681 14043 23406 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
References
-
N. Chandrakumar
1D double quantum filter NMR studies,
in Annual Reports on NMR Spectroscopy, Graham A. Webb (Ed.), Elsevier, Amsterdam, vol. 67, pages 265-329 (2009).
Abstract
-
Giuseppe Pileio, Maria Concistrč, Neville McLean, Axel Gansmüller, Richard C. D. Brown, and Malcolm H. Levitt
Analytical theory of γ-encoded double-quantum recoupling sequences in solid-state nuclear magnetic resonance,
J. Magn. Reson. 186, 65-74 (2007).
Abstract
-
M. J. Potrzebowski, J. Gajda, W. Ciesielski, and I. M. Montesinos
Distance measurements in disodium ATP hydrates by means of 31P double quantum two-dimensional solid-state NMR spectroscopy, (PC7, asymmetric peaks)
J. Magn. Reson. 179, 173-181 (2006).
Abstract
-
Sebastian Olejniczak, Pawel Napora, Jaroslaw Gajda, Wlodzimierz Ciesielski, Marek J. Potrzebowski
31P double-quantum solid-state NMR study of phosphoroorganic compounds with (O)P-O-P-(O), (S)P-O-P(S) and (S)P-S-P(O) unit, (PC7)
Solid State Nucl. Magn. Reson. 30, 141-149 (2006).
Abstract
-
Colan E. Hughes and Marc Baldus
Magic-angle-spinning solid-state NMR applied to polypeptides and proteins,
in Annual Reports on NMR Spectroscopy, Graham A. Webb (Ed.), Elsevier, Amsterdam, vol. 55, pages 121-158 (2005).
Abstract
-
Ingo Schnell
Dipolar recoupling in fast-MAS solid-state NMR spectroscopy,
Prog. Nucl. Magn. Reson. Spectrosc. 45, 145-207 (2004).
Abstract
-
Yoh Matsuki, Hideo Akutsu, and Toshimichi Fujiwara
Precision 1H-1H distance measurement via 13C NMR signals: utilization of 1H-1H double-quantum dipolar interactions recoupled under magic angle spinning conditions,
Magn. Reson. Chem. 42, 291-300 (2004).
Abstract
-
T. Karlsson, J. M. Popham, J. R. Long, N. Oyler, and G. P. Drobny
A study of homonuclear dipolar recoupling pulse sequences in solid-state nuclear magnetic resonance, (DRAWS, PC7, SPC5, R1426, R2246; phase cycling)
J. Am. Chem. Soc. 125, 7394-7407 (2003).
Abstract
-
M. Bjerring, T. Vosegaard, A. Malimendal, and N.C. Nielsen
Methodological development of solid-state NMR for characterization of membrane proteins, (PC7, C7)
Concepts Magn. Reson. A 18, 111-129 (2003).
Abstract
-
G. P. Drobny, J. R. Long, T. Karlsson, W. Shaw, J. Popham, N. Oyler, P. Bower, J. Stringer,
D. Gregory, M. Mehta, and P. S. Stayton
Structural studies of biomateriaux using double-quantum solid-state NMR spectroscopy,
Annu. Rev. Phys. Chem. 54, 531-571 (2003).
Abstract
-
Wyndham Bolling Blanton
High Performance Computations in NMR,
Berkeley, 2002.
Ph.D
-
Juraj Pivarč
Application of the Multiple Quantum NMR Spectroscopy for Investigation of the Dipole-Dipole Couplings in Amorphous Polymers,
Halle, 4 July 2000.
Dissertation
-
Andreas Brinkmann, Mattias Edén, and Malcolm H. Levitt
Synchronous helical pulse sequences in magic-angle spinning nuclear magnetic resonance: Double quantum recoupling of multiple-spin systems, (CNnν: C721, C1445, C144-5, SC1445; phase cycling)
J. Chem. Phys. 112, 8539-8554 (2000).
Abstract
-
Mattias Edén, Andreas Brinkmann, Henrik Luthman, Lars Eriksson, and Malcolm H. Levitt
Determination of molecular geometry by high-order multiple-quantum evolution in solid-state NMR,
J. Magn. Reson. 144, 266-279 (2000).
Abstract
-
T. Karlsson, A. Brinkmann, P. J. E. Verdegem, J. Lugtenburg, and M. H. Levitt
Multiple-quantum relaxation in the magic-angle-spinning NMR of 13C spin pairs, (C7, phase cycling)
Solid State Nucl. Magn. Reson. 14, 43-58 (1999).
Abstract
-
Mei Hong
Solid-state dipolar INADEQUATE NMR spectroscopy with a large double-quantum spectral width,
J. Magn. Reson. 136, 86–91 (1999).
Abstract
-
Chad M. Rienstra, Mary E. Hatcher, Leonard J. Mueller, Boqin Sun,
Stephen W. Fesik, and Robert G. Griffin
Efficient multispin homonuclear double-quantum recoupling for magic-angle spinning NMR: 13C-13C correlation spectroscopy of U-13C-erythromycin A, (combined MLEV refocusing and C7: CMR7; dependence of DQF efficiency on 1H CW decoupling field strength during mixing; sample size)
J. Am. Chem. Soc. 120, 10602-10612 (1998).
Abstract
-
M. Edén and M. H. Levitt
Excitation of carbon-13 triple quantum coherence in magic-angle-spinning NMR,
Chem. Phys. Lett. 293, 173-179 (1998).
Abstract
-
M. Hohwy, H. J. Jakobsen, M. Edén, M. H. Levitt, and N. C. Nielsen
Broadband dipolar recoupling in the nuclear magnetic resonance of rotating solids: A compensated C7 pulse sequence,
J. Chem. Phys. 108, 2686-2694 (1998).
Abstract
Definition of PC7 excitation pulse.
-
Helen Geen, Johannes Gottwald, Robert Graf, Ingo Schnell, Hans W. Spiess, and Jeremy J. Titman
Elucidation of dipolar coupling networks under magic-angle spinning,
J. Magn. Reson. 125, 224-227 (1997).
Abstract
-
W. A. Dollase, M. Feike, H. Förster, T. Schaller, I. Schnell, A. Sebald, and S. Steuernagel
A 2D 31P MAS NMR study of polycrystalline Cd3(PO4)2,
J. Am. Chem. Soc. 119, 3807-3810 (1997).
Abstract
-
Y. K. Lee, N. D. Kurur, M. Helmle, O. G. Johannessen, N. C. Nielsen, and M. H. Levitt
Efficient dipolar recoupling in the NMR of rotating solids. A sevenfold symmetric radiofrequency pulse sequence, (C7, phase cycling)
Chem. Phys. Lett. 242, 304-309 (1995).
Abstract
Definition of C7 excitation pulse.
-
Yoshitaka Ishii, Jun Ashida, and Takehiko Terao
13C---1H dipolar recoupling dynamics in 13C multiple-pulse solid-state NMR,
Chem. Phys. Lett. 246, 439-445 (1995).
Abstract
-
A. Wokaun and R. R. Ernst
Selective detection of multiple quantum transitions in NMR by two-dimensional spectroscopy,
Chem. Phys. Lett. 52, 407-412 (1977).
Abstract
(top)
[Contact me]
- Last updated February 20, 2018
Copyright © 2002-
pascal-man.com. All rights reserved.