Proton-detected heteronuclear edited and correlated nuclear magnetic resonance and nuclear Overhauser effect in solution

The proton has been the nucleus of choice for NMR studies of macromolecules because it is ubiquitous; it provides the highest sensitivity; its resonances can be identified with types of amino and nucleic acids by means of experiments utilizing proton spin-spin interaction and chemical shift; and, most important, proton NMR yields distance information via the nuclear Overhauser effect (NOE). Many of these advantages are lost for larger biopolymers (molecular weight more than 15 kDa) for which the line width is considerably greater than the proton-proton spin-spin interaction. The spin-spin interaction is then useless or difficult to use for assignment; and furthermore the proton line width and the number of proton resonances both increase in proportion to the molecular weight, thereby increasing the problem of resonance overlap to an intolerable degree.

[1]  J. Markley,et al.  Nuclear magnetic resonance studies of two-iron-two-sulfur ferredoxins. 3. Heteronuclear (carbon-13, proton) two-dimensional NMR spectra, 13C peak assignments, and 13C relaxation measurements , 1983 .

[2]  S. Opella,et al.  One- and two- dimensional 15N/1H NMR of filamentous phage coat proteins in solution. , 1985, Biochemical and biophysical research communications.

[3]  F. Eckstein,et al.  Assignment of resonances in the 31P NMR spectrum of d(GGAATTCC) by regiospecific labeling with oxygen-17. , 1984, Biochemistry.

[4]  F. Richards,et al.  1H-15N heteronuclear NMR studies of Escherichia coli thioredoxin in samples isotopically labeled by residue type. , 1985, Biochemistry.

[5]  D. Doddrell,et al.  Pulse sequences utilizing the correlated motion of coupled heteronuclei in the transverse plane of the doubly rotating frame , 1983 .

[6]  H. Vorbrüggen,et al.  Nucleoside syntheses, XXV1) A new simplified nucleoside synthesis , 1981 .

[7]  A. Redfield Stimulated echo NMR spectra and their use for heteronuclear two-dimensional shift correlation , 1983 .

[8]  A. Bax,et al.  Proton and carbon-13 assignments from sensitivity-enhanced detection of heteronuclear multiple-bond connectivity by 2D multiple quantum NMR , 1986 .

[9]  R. Griffey,et al.  Assignment of proton amide resonances of T4 lysozyme by 13C and 15N multiple isotopic labeling , 1986 .

[10]  H. Yamada,et al.  Tyrosine phenol lyase. I. Purification, crystallization, and properties. , 1970, The Journal of biological chemistry.

[11]  D. Cowburn,et al.  Two-dimensional 1H-113Cd chemical-shift correlation maps by 1H-detected multiple-quantum NMR in metal complexes and metalloproteins , 2002 .

[12]  V. Kollman,et al.  13C nuclear magnetic resonance studies of the biosynthesis by Microbacterium ammoniaphilum of L-glutamate selectively enriched with carbon-13. , 1982, The Journal of biological chemistry.

[13]  D. Doddrell,et al.  A vector description of multiple-quantum coherence in AXn spin systems , 1983 .

[14]  G. Wider,et al.  X-relayed 1H-1H correlated spectroscopy , 1984 .

[15]  G. Wagner,et al.  Simplification of two-dimensional proton NMR spectra using an X-filter , 1986 .

[16]  E. Hahn,et al.  Pulsed Nuclear Resonance Spectroscopy , 1960 .

[17]  J. Gerlt,et al.  A General Procedure for Assigning the 31P Spectra of Nucleic Acids , 2002 .

[18]  R. Griffey,et al.  15N-labeled Escherichia coli tRNAfMet, tRNAGlu, tRNATyr, and tRNAPhe. Double resonance and two-dimensional NMR of N1-labeled pseudouridine. , 1985, The Journal of biological chemistry.

[19]  C. S. Irving,et al.  Dynamic structure of whole cells probed by nuclear Overhauser enhanced nitrogen-15 nuclear magnetic resonance spectroscopy. , 1977, Proceedings of the National Academy of Sciences of the United States of America.

[20]  P. Agris,et al.  Transfer RNA contains sites of localized positive charge: carbon NMR studies of [13C]methyl-enriched Escherichia coli and yeast tRNAPhe. , 1986, Biochemistry.

[21]  R. Lipnick,et al.  Synthesis of nitrogen‐15 labelled uracil and its 1‐deuteromethyl 3‐deuteromethyl, and 1,3‐dideuteromethyl derivatives (1) , 1980 .

[22]  NMR OF PROTONS COUPLED TO CARBON-13 NUCLEI ONLY , 1981 .

[23]  R. Griffey,et al.  Proton NMR measurements of bacteriophage T4 lysozyme aided by 15N isotopic labeling: structural and dynamic studies of larger proteins. , 1987, Proceedings of the National Academy of Sciences of the United States of America.

[24]  P. Wright,et al.  Site-selective observation of nuclear Overhauser effects in proteins via isotopic labeling , 1987 .

[25]  C. Hilbers,et al.  Structure and Dynamics of RNA , 1986, NATO ASI Series.

[26]  A. Bax,et al.  Sensitivity-enhanced two-dimensional heteronuclear shift correlation NMR spectroscopy , 1986 .

[27]  R. Griffey,et al.  Isotope-detected 1H NMR studies of proteins: a general strategy for editing interproton nuclear Overhauser effects by heteronuclear decoupling, with application to phage lambda repressor. , 1986, Proceedings of the National Academy of Sciences of the United States of America.

[28]  A. Bax,et al.  Two-Dimensional Heteronuclear Chemical-Shift Correlation in Proteins at Natural Abundance 15N and 13C Levels , 1987 .

[29]  A. Bax,et al.  Sensitivity-enhanced two-dimensional heteronuclear relayed coherence transfer NMR spectroscopy , 1986 .

[30]  R. Griffey,et al.  Nuclear magnetic resonance observation and dynamics of specific amide protons in T4 lysozyme. , 1985, Biochemistry.

[31]  R. Griffey,et al.  Efficient syntheses of [3-15N]uracil and [3-15N]thymine. , 1983, Nucleic acids research.

[32]  G. Wagner,et al.  Toward the complete assignment of the carbon nuclear magnetic resonance spectrum of the basic pancreatic trypsin inhibitor. , 1986, Biochemistry.

[33]  M. Llinás,et al.  Nitrogen-15 nuclear magnetic resonance spectrum of alumichrome. Detection by a double resonance Fourier transform technique. , 1976, Journal of the American Chemical Society.

[34]  A. Bax,et al.  Selective observation of phosphate ester protons by 1H <{;31P<}; spin-echo difference spectroscopy , 1984 .

[35]  A. Bax,et al.  Complete proton and carbon-13 assignments of coenzyme B12 through the use of new two-dimensional NMR experiments , 1986 .

[36]  A. Redfield,et al.  Nitrogen-15-labeled yeast tRNAPhe: double and two-dimensional heteronuclear NMR of guanosine and uracil ring NH groups. , 1984, Biochemistry.

[37]  A. Bax,et al.  Complete 1H and 13C Assignments of Coenzyme B12 Through the Use of New Two‐Dimensional NMR Experiments. , 1986 .

[38]  C. Poulter,et al.  2′,3′,5′-Tri-O-benzoyl[4-13C]uridine. An efficient, regiospecific synthesis of the pyrimidine ring , 1978 .

[39]  K. Wüthrich,et al.  Sequence-specific 1H-NMR assignments in rabbit-liver metallothionein-2. , 1986, European journal of biochemistry.

[40]  I. Campbell,et al.  1H NMR measurements of enzyme-catalyzed 15N-label exchange , 1984 .

[41]  R. R. Ernst,et al.  Polypeptide - Metal Cluster Connectivities in Metallothionein 2 by Novel1H -113Cd Heteronuclear Two-Dimensional NMR Experiments , 1986 .

[42]  R. Griffey,et al.  Multiple quantum two-dimensional 1H--15N nuclear magnetic resonance spectroscopy: chemical shift correlation maps for exchangeable imino protons of Escherichia coli tRNAMetf in water. , 1983, Proceedings of the National Academy of Sciences of the United States of America.

[43]  M. Karplus,et al.  Genetic Methods in High-Resolution NMR Studies of Proteins , 1986 .

[44]  R G Shulman,et al.  1H-Observe/13C-decouple spectroscopic measurements of lactate and glutamate in the rat brain in vivo. , 1985, Proceedings of the National Academy of Sciences of the United States of America.

[45]  M. J. Kime Assignment of resonances of exchangeable protons in the NMR spectrum of the complex formed by Escherichia coli ribosomal protein L25 and uniformly nitrogen‐15 enriched 5 S RNA fragment , 1984, FEBS letters.

[46]  A. Redfield Special Problems of NMR in H2O Solution , 1986 .

[47]  G. Bodenhausen,et al.  Natural abundance nitrogen-15 NMR by enhanced heteronuclear spectroscopy , 1980 .

[48]  J. Gerlt,et al.  Site-directed mutants of staphylococcal nuclease. Detection and localization by 1H NMR spectroscopy of conformational changes accompanying substitutions for glutamic acid-43. , 1987, Biochemistry.

[49]  R. Shulman,et al.  High-resolution proton NMR studies of intracellular metabolites in yeast using 13C decoupling☆ , 1981 .

[50]  A. Bax,et al.  Assignment of the 31P and 1H resonances in oligonucleotides by two‐dimensional NMR spectroscopy , 1986, FEBS letters.

[51]  H. Senn,et al.  Protein structure and interactions by combined use of sequential NMR assignments and isotope labeling , 1987 .

[52]  R. R. Ernst,et al.  Polypeptide-metal cluster connectivities in metallothionein 2 by novel proton-cadmium-113 heteronuclear two-dimensional NMR experiments , 1985 .

[53]  Claudio Nicolini,et al.  NMR in the Life Sciences , 1986, NATO ASI Series.

[54]  K. Uğurbil,et al.  Selective observation of 1H resonances from hydrogens directly bonded to 13C atoms , 1985 .

[55]  G. Wagner,et al.  Selective excitation of 1H resonances coupled to 13C. Hetero COSY and RELAY experiments with 1H detection for a protein , 1986 .

[56]  D. G. Davis,et al.  Natural-abundance 15N NMR studies of Turkey ovomucoid third domain. Assignment of peptide 15N resonances to the residues at the reactive site region via proton-detected multiple-quantum coherence , 1986 .

[57]  K. Wüthrich,et al.  Editing of 2D 1H NMR spectra using X half-filters. combined use with residue-selective 15N labeling of proteins , 1986 .

[58]  B. Sjöberg,et al.  Thioredoxin and glutaredoxin systems : structure and function , 1986 .

[59]  R. Griffey,et al.  Proton NMR studies of nitrogen-15-labeled Escherichia coli tRNAfMet. Assignments of imino resonances for uridine-related bases by proton-nitrogen-15 heteronuclear double resonance difference spectroscopy , 1983 .

[60]  Y. Yamada,et al.  Synthesis of guanosine and its derivatives from 5-amino-1-beta-D- ribofuranosyl-e-imidazolecarboxamide. IV. A new route to guanosine via cyanamide derivative , 1976, Nucleic Acids Res..

[61]  M. J. Kime Assignment of resonances in the Escherichia coli 5 S RNA fragment proton NMR spectrum using uniform nitrogen‐15 enrichment , 1984, FEBS letters.

[62]  P. Agris,et al.  Nuclear magnetic resonance signal assignments of purified [13C]methyl-enriched yeast phenylalanine transfer ribonucleic acid. , 1985, Biochemistry.

[63]  R. Griffey,et al.  Proton nuclear magnetic relaxation of nitrogen-15-labeled nucleic acids via dipolar coupling and chemical shift anisotropy , 1983 .

[64]  A. Bax,et al.  Simplification of two-dimensional NOE spectra of proteins by 13C labeling , 1987 .

[65]  R. Griffey,et al.  Correlation of proton and nitrogen-15 chemical shifts by multiple quantum NMR☆ , 1983 .

[66]  D. States,et al.  A two-dimensional nuclear overhauser experiment with pure absorption phase in four quadrants☆ , 1982 .

[67]  A. Bax,et al.  Two-dimensional nuclear magnetic resonance spectroscopy. , 1986, Science.

[68]  J. S. Cohen,et al.  Selective observation of 13C-enriched metabolites by 1H NMR , 1983 .

[69]  R. Griffey,et al.  15N-labeled tRNA. Identification of dihydrouridine in Escherichia coli tRNAfMet, tRNALys, and tRNAPhe by 1H-15N two-dimensional NMR. , 1986, The Journal of biological chemistry.

[70]  W. Bachovchin Confirmation of the assignment of the low-field proton resonance of serine proteases by using specifically nitrogen-15 labeled enzyme. , 1985, Proceedings of the National Academy of Sciences of the United States of America.

[71]  J. Gerlt,et al.  A method for the observation of selected proton NMR resonances of proteins , 1986 .

[72]  D. T. Pegg,et al.  Sensitive‐volume localization for in vivo NMR using heteronuclear spin‐echo pulse sequences , 1985, Magnetic resonance in medicine.

[73]  A. Bax,et al.  1H and13C Assignments from Sensitivity-Enhanced Detection of Heteronuclear Multiple-Bond Connectivity by 2D Multiple Quantum NMR , 1986 .

[74]  D. G. Davis,et al.  Observation of 1000-fold enhancement of 15N NMR via proton-detected multiquantum coherences: studies of large peptides , 1984 .

[75]  P. Bolton Heteronuclear relay transfer spectroscopy with proton detection , 1985 .

[76]  L. Mueller,et al.  Proton-detected natural-abundance 15N NMR spectroscopy utilizing constant-time multiple-quantum excitation , 1986 .

[77]  Multiple-quantum 113Cd1H correlation spectroscopy as a probe of metal coordination environments in metalloproteins , 1985 .

[78]  M. Saneyoshi Synthetic Nucleosides and Nucleotides. VIII. Direct Synthesis of the 5'-Phosphate of 4-Thiouridine, 6-Thioinosine and 6-Thioguanosine from the Corresponding Oxy Nucleotide via Thiation Procedure , 1971 .

[79]  G. Bodenhausen,et al.  Resolution enhancement in heteronuclear two-dimensional spectroscopy by realignment of coherence transfer echoes , 1982 .

[80]  R. Cline,et al.  Synthesis of 5-Substituted Pyrimidines via Formaldehyde Addition1 , 1959 .

[81]  G. Bodenhausen,et al.  Indirect detection of mercury-199 NMR: adducts of ethylmercury phosphate with amino acids and ribonuclease , 1982 .

[82]  M. Kainosho,et al.  Local structural features around the C-terminal segment of Streptomyces subtilisin inhibitor studied by carbonyl carbon nuclear magnetic resonances three phenylalanyl residues. , 1987, Biochemistry.

[83]  L. Mueller Sensitivity enhanced detection of weak nuclei using heteronuclear multiple quantum coherence , 1979 .

[84]  M. Kainosho,et al.  Assignment of the three methionyl carbonyl carbon resonances in Streptomyces subtilisin inhibitor by a carbon-13 and nitrogen-15 double-labeling technique. A new strategy for structural studies of proteins in solution. , 1982, Biochemistry.

[85]  T. Henderson,et al.  Purine ring rearrangements leading to the development of cytokinin activity. Mechanism of the rearrangement of 3-benzyladenine to N6-benzyladenine. , 1975, Journal of the American Chemical Society.

[86]  R. Griffey,et al.  Identification of isotope-labeled resonances in two-dimensional proton-proton correlation and exchange spectroscopy with gated heteronuclear decoupling , 1985 .

[87]  D. LeMaster,et al.  Biosynthetic production of 13C-labeled amino acids with site-specific enrichment. , 1982, The Journal of biological chemistry.

[88]  J. Anglister,et al.  Magnetic resonance of a monoclonal anti-spin-label antibody , 1984 .

[89]  E. Hahn,et al.  Nuclear Double Resonance in the Rotating Frame , 1962 .

[90]  H. Vorbrüggen,et al.  New simplified nucleoside synthesis , 1978 .