Literature-based outline for “Theory and Implementation of Techniques for Oriented Systems I”
Stanley J. Opella
University of California, San Diego
Introduction
Solid-state NMR spectroscopy
Pines A, Gibby MG, Waugh JS (1972) Proton-enhanced nuclear induction spectroscopy. A method for high
resolution NMR of dilute spins in solids. J Chem Phys 56, 1776-1777.
Urbina J, Waugh JS (1974) Proton-enhanced NMR of lipids and biomembranes. Proc Natl Acad Sci 71, 50625067.
Nuclear spin interactions are anisotropic
Pake GE (1948) Nuclear resonance absorption in hydrated crystals: Fine structure of the proton line. J Chem
Phys 16, 427-336.
Lauterbur PC (1958) Anisotropy of the C13 chemical shift in calcite. Phys Rev Lett 1, 343-344.
Attenuation of dipole-dipole couplings
Lee M Goldlburg WI (1965) NMR line narrowing by a rotating rf field. Phys Rev 140, 1261-1271.
Waugh JS, Huber, LM, Waugh JS (1968) Approach to high-resolution NMR in solids. Phys Rev Lett 20, 180182.
High resolution solid-state NMR spectra of crystals and powders
Pines A, Gibby MG, Waugh JS (1973) Proton-enhanccd NMR of dilute spins in solids. J Chem Phys 59, 569590.
Opella SJ, Frey MH, Cross TA (1979) Detection of individual carbon resonances in solid proteins. 101, 58565857.
Cross TA, DiVerdi JA, Opella SJ (1982) Strategy for nitrogen NMR of biopolymers. J Am Chem Soc 104, 17591761.
Measurement of dipole-dipole couplings
Muller L, Kumar A, Baumann T, Ernst RR (1974) Transient oscillations in NMR cross-polarization experiments
in solids. Phys Rev Lett 32, 1403-1406/
Hester RK, Ackerman JL, Cross VR, Waugh JS (1975) Resolved dipolar coupling spectra of dilute nuclear
spins in solids. Phys Rev Lett 34, 993-995.
Hester RK, Ackerman JL, Neff BL, Waugh JS (1976) Separated local field spectra in NMR: determination of
structure of solids. Phys Rev Lett 36, 1081-1083.
High resolution solid-state NMR spectra of aligned samples
Opella SJ, Waugh JS (1977) Two-dimensional 13C NMR of highly oriented polyethylene. J Chem Phys 66,
4919-4924.
Cross TA, Opella SJ (1983) Protein structure by solid-state NMR. J Am Chem Soc 105, 306-308.
Cross TA, Opella SJ (1985) Protein structure by solid state NMR: Residues 40 to 45 of bacteriophage fd coat
protein. J Mol Biol 182. 367-381.
Wu CH, Ramamoorthy A, Opella SJ (1994) High-resolution heteronuclear dipolar solid-state NMR
spectroscopy. J Magn Reson A109, 270-272.
Ramamoorthy A, Wu CH, and Opella SJ (1995) Three-dimensional solid-state NMR experiment that correlates
the chemical shift and dipolar coupling frequencies of two heteronuclei. J Magn Reson B107, 88-90.
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Nevzorov A, Opella SJ (2003) A “magic sandwich” pulse sequence with reduced offset dependence for highresolution separated local field spectroscopy. J Magn Reson
Marassi FM, Ramamoorthy A, Opella SJ (1997) Complete resolution of the solid-state NMR spectrum of a
uniformly 15N-labeled membrane protein in phospholipid bilayers. Proc Natl Acad Sci 94, 8551-8556.
Mapping of structure onto spectra.
Marassi GM Opella SJ (2000) A solid-state NMR index of helical membrane protein structure and topology. J
Magn Reson 144, 150-155.
Wang J, Denny J, Tian C, Kim S, Mo Y, Kovacs F, Song Z, Nishimura K, Gan Z, Fu R, Quine JR, Cross TA
(2000) Imaging membrane protein helical wheels. J Magn Reson 144, 162-167.
Kovacs FA, Denny JK, Song Z, Quine JR, Cross TA (2000) Helix tilt of the M2 transmembrane peptide from
influenza A virus: An intrinsic property. J Mol Biol 295, 11-125.
Mesleh MF, Veglia G, DeSilva TM, Marassi FM, Opella SJ (2002) Dipolar waves as NMR maps of protein
structure. J Am Chem Soc 124, 4206-4207.
Mesleh MF, Lee S, Veglia G, Thiriot DS, Marassi FM, Opella SJ (2003) Dipolar waves map the structure and
topology of helices in membrane proteins. J Am Chem Soc 125, 8928-8935.
Marassi FM (2001) A simple approach to membrane protein secondary structure and topology based on NMR
spectroscopy. Biophys J 80, 994-1003.
Tang M, Waring AJ, Lehrer RI, Hong M (2006) Orientation of a B-hairpin antimicrobial peptide in lipid bilayers
from two-dimensional dipolar chemical-shift correlation NMR. Biophys J 90, 3616-3624.
Approach to structure determination
DeAngelis AA, Jones DH, Grant CV, Park SH, Mesleh MF, Opella SJ (2005) NMR experiments on aligned
samples of membrane proteins. Meth Enzymol 394, 350-382.
Triba MN, Warschawski DE, Devaux PF (2005) Reinvestigation by phosphorus NMR of lipid distribution in
bicelles. Biophys J 88, 1887-1901.
DeAngelis AA, Nevzorov AA, Park SH, Howell SC, Mrse AA, Opella SJ (2004) High-resolution NMR
spectroscopy of membrane proteins in aligned bicelles. J Am Chem Soc 126, 15340-15341.
Motional averaging in solid-state NMR
Mehring M, Griffin RG, Waugh JS (1971) 19F Shielding tensors from coherently narrowed NMR powder
spectra. J Chem Phys 55, 746-755.
Pines A, Gibby MG, Waugh JS (1973) Proton-enhanccd NMR of dilute spins in solids. J Chem Phys 59, 569590.
Frey MH, DiVerdi JA, Opella SJ (1985) Dynamics of phenylalanine in the solid state by NMR. J Am Chem Soc
107, 7311-7315.
Lewis BA, Harbison GS, Herzfeld J, Griffin RG (1985) Structural analysis of a membrane protein:
bacteriorhodopsin peptide backbone orientation and motion. Biochemistry 24, 4671-4679.
Tilted samples and rotational diffusion
McLaughlin AC, Cullis PR, Hemminga MA, Hoult DI, Radda GK, Ritchie GA, Seeley PJ, Richards RE (1975)
Application of 31P NMR to model and biological membrane systems. FEBS Lett 57, 213-218.
Park SH, Mrse AA, Nevzorov AA, DeAngelis AA, Opella SJ (2006) Rotational diffusion of membrane proteins
in aligned phospholipid bilayers by solid-state NMR spectroscopy. J. Magn. Reson 178, 162-165.
Song Z, Kovacs FA, Wang J, Denny JK, Shekar SC, Quine JR, Cross TA (2000) Transmembrane domain of
M2 protein from Influenza A virus studied by solid-state 15N polarization inversion spin exchange at the magic
angle NMR. Biophys J 79, 767-775.
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Nevzorov AA, DeAngelis AA, Park SH, Opella SJ (2006) Uniaxial motional averaging of the chemical shift
anisotropy of membrane proteins in bilayer environments. In NMR of Biological Solids (Ramamoorthy, ed)
CRC Press, 177-190.
Hong M, Doherty T (2006) Orientation determination of membrane-disruptive proteins using powder samples
and rotational diffusion: a simple solid-state NMR approach. Chem Phys Lett 432, 296-300.
Cady SD, Goodman C, Tatko C, DeGrado WF, Hong M (2007) Determining the orientation of uniaxially rotating
membrane proteins using unoriented samples: A 2H, 13C, and 15N solid-state NMR investigation of the
dynamics and orientation of a transmembrane helical bundle. J Am Chem Soc 129, 5719-5729.
Structure determination
Cross TA, Opella SJ (1985) Protein structure by solid state NMR: Residues 40 to 45 of bacteriophage fd coat
protein. J Mol Biol 182. 367-381.
Opella SJ, Marassi FM, Gesell JJ, Valente AP, Kim Y, Oblatt-Montal M, Montal M (1999) Structures of the M2
channel-lining segments from nicotinic acetylcholine and NMDA receptors by NMR spectroscopy. Nature
Structural Biology 6, 374-379.
Ketchem, RR, Hu, W, Cross TA (1993) High-resolution conformation of gramicidin A in lipid bilayer by solidstate NMR. Science 261, 1457-1460.
DeAngelis AA, Howell SC, Nevzorov AA, Opella SJ (2006) Structure determination of a membrane protein with
two trans-membrane helices in aligned phospholipid bicelles by solid-state NMR spectroscopy. J Am Chem
Soc 128, 12256-12267.
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