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Nuclear Magnetic Resonance of Biological Macromolecules PDF

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METHODS IN ENZYMOLOGY EDITORS-IN-CHIEF John N. Abelson Melvin I. Simon DIVISIONOFBIOLOGY CALIFORNIAINSTITUTEOFTECHNOLOGY PASADENA,CALIFORNIA FOUNDINGEDITORS Sidney P. Colowick and Nathan O. Kaplan Contributors to Volume 394 Articlenumbersareinparenthesesandfollowingthenamesofcontributors. Affiliationslistedarecurrent. Thomas B. Acton (8), Center for Ad- Paul B. Card (1), Departments of Bio- vanced Biotechnology and Medicine, chemistryandPharmacology,University Department of Molecular Biology and of Texas Southwestern Medical Center, Biochemistry, Rutgers University, Pis- Dallas,Texas75390 cataway,NewJersey08854 Yi-WenChiang (8), Centerfor Advanced James Aramini (8), Center for Advanced Biotechnology and Medicine, Depart- Biotechnology and Medicine, Depart- ment of Molecular Biology and Bioche- ment of Molecular Biology and Bio- mistry, Rutgers University, Piscataway, chemistry, Rutgers University, NewJersey08854 Piscataway,NewJersey08854 TeresaCliment(8),CenterforAdvanced Cheryl Arrowsmith (5), Ontario Cancer Biotechnology and Medicine, Depart- Institute and Department of Medical ment of Molecular Biology and Bioche- Biophysics, University of Toronto, mistry, Rutgers University, Piscataway, Toronto,Ontario,M5G2M9Canada NewJersey08854 HanudattaS.Atreya(4),Departmentof Bonnie Cooper (8), Center for Advanced Chemistry, University at Buffalo, The Biotechnology and Medicine, Depart- State University of New York, Buffalo, ment of Molecular Biology and Bioche- NewYork14260 mistry, Rutgers University, Piscataway, NewJersey08854 Michael C. Baran (5, 8), Center for Ad- vanced Biotechnology and Medicine, LorenzoCorsini(2),InstituteforBiophy- Department of Molecular Biology and sicalChemistry,UniversityofFrankfurt, Biochemistry, Rutgers University, 60439Frankfurt,Germany Piscataway,NewJersey08854 L. David Finger (22), Department of AdBax(3),NationalInstituteofDiabetes Chemistry and Biochemistry, University and Digestive and Kidney Diseases, of California, Los Angeles, California National Institutes of Health, Bethesda, 90095 Maryland20892 A. A. De Angelis (14), Department of G. C. Benison (7), Department of Bio- ChemistryandBiochemistry,University chemistry and Molecular Biology, Uni- of California, San Diego, La Jolla, versity of Georgia, Athens, Georgia California92093 30602 FrankDelaglio(3),NationalInstituteof P. Bernado´ (17), Institut de Biologie DiabetesandDigestiveandKidneyDis- Structurale, Jean Pierre Ebel, 38027 eases, National Institutes of Health, Grenoble,France Bethesda,Maryland20892 ix x contributors to volume 394 NataliaG.Denissova(8),CenterforAd- Kevin H. Gardner (1), Departments of vanced Biotechnology and Medicine, Biochemistry and Pharmacology, Uni- Department of Molecular Biology and versity of Texas Southwestern Medical Biochemistry, Rutgers University, Pis- Center,Dallas,Texas75390 cataway,NewJersey08854 MarkGerstein(8),DepartmentofMole- Shawn M. Douglas (8), Department of cular Biophysics and Biochemistry Molecular Biophysics and Biochemistry and Department of Computer Science, and Department of Computer Science, Yale University, New Haven, Connecti- YaleUniversity,NewHaven,Connecticut cut06520 06520 C.V.Grant(14),DepartmentofChemis- Volker Do¨tsch (2), Institute for Biophy- try and Biochemistry, University of Ca- sicalChemistry,UniversityofFrankfurt, lifornia,SanDiego,LaJolla,California 60439Frankfurt,Germany 92093 FlorianDurst(2),InstituteforBiophysi- MichaelJ.Grey(18),DepartmentofBio- cal Chemistry, University of Frankfurt, chemistry and Molecular Biophysics, 60439Frankfurt,Germany Columbia University, New York, H. Jane Dyson (11), Department of NewYork10032 Molecular Biology and Skaggs Institute AlexanderGrishaev(10),NationalInsti- forChemicalBiology,ScrippsResearch tuteofDiabetesandDigestiveandKid- Institute, La Jolla, California 92037 ney Diseases, National Institutes of Christian Eichmu¨ller (6), Institute of Health,Bethesda,Maryland20892 Organic Chemistry, University of In- Kristin C. Gunsalus (8), Department of nsbruck,A-6020Innsbruck,Austria Biology, Center for Comparative Func- ElanZ.Eisenmesser(21),Departmentof tional Genomics, New York Univeristy, NewYork,NewYork10003 Biochemistry, Brandeis University, Waltham,Massachusetts02454 Philip J. Hajduk (23), Abbott Labora- Charles D. Ellis (12), Department of tories,AbbottPark,Illinois60064 Biochemistry, Vanderbilt University Kathleen B. Hall (19), Department School of Medicine, Nashville, Tennes- of Biochemistry and Molecular see37232 Biophysics, Washington University JohnK.Everett(8),CenterforAdvanced School of Medicine, St. Louis, Biotechnology and Medicine, Depart- Missouri 63110 ment of Molecular Biology and Bioche- Chi Kent Ho (8), Center for Advanced mistry, Rutgers University, Piscataway, Biotechnology and Medicine, Depart- NewJersey08854 ment of Molecular Biology and Bioche- JuliFeigon(22),DepartmentofChemistry mistry, Rutgers University, Piscataway, and Biochemistry, University of Califor- NewJersey08854 nia,LosAngeles,California90095 BerndHoffmann(6),InstituteofTheoreti- J.Garcı´adelaTorre(17),Departamento cal Chemistry and Molecular Structural deQu´ımicaF´ısica,UniversidaddeMur- Biology, University of Vienna, A-1030 cia,30071Murcia,Spain Vienna,Austria contributors to volume394 xi Yuanpeng Janet Huang (5), Center for Robert Konrat (6), Institute of Theoreti- AdvancedBiotechnologyandMedicine, cal Chemistry and Molecular Structural Department of Molecular Biology Biology, University of Vienna, A-1030 and Biochemistry, Rutgers University, Vienna,Austria Piscataway,NewJersey08854 Georg Kontaxis (3), Department of John F. Hunt (8), Department of Biolo- Theoretical Chemistry and Molecular gical Sciences, Columbia University, Structural Biology, University of New York, New York 10027 Vienna,A-1030Vienna,Austria Jeffrey R. Huth (23), Abbott Labora- Miguel Llina´s (10), Department of tories,AbbottPark,Illinois60064 Chemistry, Carnegie Mellon University, Pittsburgh,Pennsylvania15213 Peter M. Hwang (13), Departments of Medical Genetics, Biochemistry, PeterJ.Lukavsky(16),MRCLaboratory and Chemistry, University of of Molecular Biology, Cambridge, CB2 Toronto, Toronto, Ontario, M5S 1A1 2QH,England Canada Li Chung Ma (8), Center for Advanced MasayoriInouye(8),DepartmentofBio- Biotechnology and Medicine, Depart- chemistry,RobertWoodJohnsonMedi- mentofMolecularBiologyandBiochem- cal School, University of Medicine and istry, Rutgers University, Piscataway, Dentistry of New Jersey, Piscataway, NewJersey08854 NewJersey08854 Daphne Macapagal (8), Center for Ad- Jaison Jacob (12), Department of vanced Biotechnology and Medicine, Department of Molecular Biology and Biochemistry, Vanderbilt University Biochemistry, Rutgers University, Pis- School of Medicine, Nashville, Tennes- cataway,NewJersey08854 see37232 Thomas L. James (24), Department of K.L.Mayer(7),DepartmentofBiochem- istry and Molecular Biology, University PharmaceuticalChemistry,Universityof ofGeorgia,Athens,Georgia30602 California, San Francisco, California 94143 Moriz Mayer (24), Biovertis AG, 1080 Vienna,Austria D.H.Jones(14),DepartmentofChemis- try and Biochemistry, University of Ca- M.F.Mesleh(14), DepartmentofChem- lifornia,SanDiego,LaJolla,California istryandBiochemistry,UniversityofCa- 92093 lifornia,SanDiego,LaJolla,California 92093 Murthy D. Karra (12), Department of Biochemistry, Vanderbilt University GaetanoT.Montelione(5,8),Centerfor School of Medicine, Nashville, Tennes- AdvancedBiotechnologyandMedicine, see37232 Department of Molecular Biology and Biochemistry, Rutgers University and LewisE.Kay(13),DepartmentsofMedi- Robert Wood Johnson Medical School, calGenetics,Biochemistry,andChemis- Piscataway,NewJersey08854 try, University of Toronto, Toronto, Ontario,M5S1A1Canada Hunter N. B. Moseley (5), Center for AdvancedBiotechnologyandMedicine, Dorothee Kern (21), Department of Department of Molecular Biology Biochemistry, Brandeis University, and Biochemistry, Rutgers University, Waltham,Massachusetts02454 Piscataway,NewJersey08854 xii contributors to volume 394 S.J.Opella(14),DepartmentofChemis- Daryl R. Sauer (23), Abbott Labora- try and Biochemistry, University of Ca- tories,AbbottPark,Illinois60064 lifornia,SanDiego,LaJolla,California Zach Serber (2), Department of Molecu- 92093 lar Pharmacology, Stanford University KirillOxenoid(12),DepartmentofBio- SchoolofMedicine,Stanford,California chemistry, Vanderbilt University School 94305 ofMedicine,Nashville,Tennessee37232 Ritu Shastry (8), Center for Advanced Arthur G. Palmer, III (18), Department Biotechnology and Medicine, Depart- ofBiochemistryandMolecularBiophy- ment of Molecular Biology and Bioche- sics, Columbia University, New York, mistry, Rutgers University, Piscataway, NewYork10032 NewJersey08854 S.H.Park(14),DepartmentofChemistry Liang-yu Shih (8), Center for Advanced andBiochemistry,UniversityofCalifor- Biotechnology and Medicine, Depart- nia, San Diego, La Jolla, California ment of Molecular Biology and Bioche- 92093 mistry, Rutgers University, Piscataway, M.Pons(17),DepartmentdeQu´ımicaOr- NewJersey08854 ga`nica, Universitat de Barcelona, 08028 Ichio Shimada (20), Division of Physical Barcelona, Spain, and Laboratori de Chemistry, Graduate School of Phar- RMN de Biomole`cules, Parc Cientific maceutical Sciences, The University deBarcelona,08028Barcelona,Spain of Tokyo, Hongo, Tokyo 113-0033, RobertPowers(5),DepartmentofChem- Japan istry, University of Nebraska—Lincoln, Scott A. Showalter (19), Department Lincoln,Nebraska68588 of Biochemistry and Molecular J. H. Prestegard (7), Complex Carbohy- Biophysics, Washington University School of Medicine, St. Louis, Mis- drate Research Center, University of souri 63110 Georgia,Athens,Georgia30602 Joseph D. Puglisi (16), Department of FrankSo¨nnichsen(12),ClevelandCenter Structural Biology, Stanford University for Structural Biology and Department SchoolofMedicine,Stanford,California of Physiology and Biophysics, Case 94305 Western Reserve University, Cleveland, Ohio44106 Paranji K. Rajan (8), Center for Ad- vanced Biotechnology and Medicine, Othmar Steinhauser (6), Institute of Department of Molecular Biology and Theoretical Chemistry and Molecular Biochemistry, Rutgers University, Pis- StructuralBiology,UniversityofVienna, cataway,NewJersey08854 A-1030Vienna,Austria Carol A. Rohl (9), Department of Bio- ChaohongSun(23),AbbottLaboratories, molecular Engineering, University of AbbottPark,Illinois60064 California,SantaCruz,California95064 G.V.T. Swapna (8), Center for Advanced CharlesR.Sanders(12),Departmentof Biotechnology and Medicine, Depart- Biochemistry and Center for Structural ment of Molecular Biology and Bioche- Biology,VanderbiltUniversitySchoolof mistry, Rutgers University, Piscataway, Medicine,Nashville,Tennessee37232 NewJersey08854 contributors to volume394 xiii Thomas Szyperski (4, 5), Department of MichaelWilson(8),DepartmentofMo- Chemistry, University at Buffalo, The lecularBiophysicsandBiochemistryand State University of New York, Buffalo, Department of Computer Science, Yale NewYork14260 University, New Haven, Connecticut 06520 RobertoTejero(5),CenterforAdvanced Peter E. Wright (11), Department Biotechnology and Medicine, Depart- of Molecular Biology and Skaggs Insti- ment of Molecular Biology and tute for Chemical Biology, Scripps Re- Biochemistry, Rutgers University, Pis- search Institute, La Jolla, California cataway,NewJersey08854 92037 Changlin Tian (12), Department of Magnus Wolf-Watz (21), Department Biochemistry, Vanderbilt University of Biochemistry, Brandeis University, School of Medicine, Nashville, Tennes- Waltham,Massachusetts02454 see37232 Haihong Wu (22), Department of H. Valafar (7), Department of ChemistryandBiochemistry,University Computer Science, University of South of California, Los Angeles, California Carolina, Columbia, South Carolina 90095 29208 Margaret Wu (8), Center for Advanced Biotechnology and Medicine, De- Chunyu Wang (18), Department of Bio- partment of Molecular Biology and chemistry and Molecular Biophysics, Biochemistry, Rutgers University, Columbia University, New York, New Piscataway,NewJersey08854 York10032 Rong Xiao (8), Center for Advanced Gerhard Wider (15), Institute for Biotechnology and Medicine, Depart- Molecular Biology and Biophysics, ment of Molecular Biology and ETH Zurich, CH-8093 Zurich, Biochemistry, Rutgers University, Switzerland Piscataway, New Jersey 08854 METHODS IN ENZYMOLOGY VolumeI.PreparationandAssayofEnzymes EditedbySidneyP.ColowickandNathanO.Kaplan VolumeII.PreparationandAssayofEnzymes EditedbySidneyP.ColowickandNathanO.Kaplan VolumeIII.PreparationandAssayofSubstrates EditedbySidneyP.ColowickandNathanO.Kaplan VolumeIV.SpecialTechniquesfortheEnzymologist EditedbySidneyP.ColowickandNathanO.Kaplan VolumeV.PreparationandAssayofEnzymes EditedbySidneyP.ColowickandNathanO.Kaplan VolumeVI.PreparationandAssayofEnzymes(Continued) PreparationandAssayofSubstrates SpecialTechniques EditedbySidneyP.ColowickandNathanO.Kaplan VolumeVII.CumulativeSubjectIndex EditedbySidneyP.ColowickandNathanO.Kaplan VolumeVIII.ComplexCarbohydrates EditedbyElizabethF.NeufeldandVictorGinsburg VolumeIX.CarbohydrateMetabolism EditedbyWillisA.Wood VolumeX.OxidationandPhosphorylation EditedbyRonaldW.EstabrookandMaynardE.Pullman VolumeXI.EnzymeStructure EditedbyC.H.W.Hirs VolumeXII.NucleicAcids(PartsAandB) EditedbyLawrenceGrossmanandKivieMoldave VolumeXIII.CitricAcidCycle EditedbyJ.M.Lowenstein VolumeXIV.Lipids EditedbyJ.M.Lowenstein VolumeXV.SteroidsandTerpenoids EditedbyRaymondB.Clayton xv xvi methods in enzymology VolumeXVI.FastReactions EditedbyKennethKustin VolumeXVII.MetabolismofAminoAcidsandAmines(PartsAandB) EditedbyHerbertTaborandCeliaWhiteTabor VolumeXVIII.VitaminsandCoenzymes(PartsA,B,andC) EditedbyDonaldB.McCormickandLemuelD.Wright VolumeXIX.ProteolyticEnzymes EditedbyGertrudeE.PerlmannandLaszloLorand VolumeXX.NucleicAcidsandProteinSynthesis(PartC) EditedbyKivieMoldaveandLawrenceGrossman VolumeXXI.NucleicAcids(PartD) EditedbyLawrenceGrossmanandKivieMoldave VolumeXXII.EnzymePurificationandRelatedTechniques EditedbyWilliamB.Jakoby VolumeXXIII.Photosynthesis(PartA) EditedbyAnthonySanPietro VolumeXXIV.PhotosynthesisandNitrogenFixation(PartB) EditedbyAnthonySanPietro VolumeXXV.EnzymeStructure(PartB) EditedbyC.H.W.HirsandSergeN.Timasheff VolumeXXVI.EnzymeStructure(PartC) EditedbyC.H.W.HirsandSergeN.Timasheff VolumeXXVII.EnzymeStructure(PartD) EditedbyC.H.W.HirsandSergeN.Timasheff VolumeXXVIII.ComplexCarbohydrates(PartB) EditedbyVictorGinsburg VolumeXXIX.NucleicAcidsandProteinSynthesis(PartE) EditedbyLawrenceGrossmanandKivieMoldave VolumeXXX.NucleicAcidsandProteinSynthesis(PartF) EditedbyKivieMoldaveandLawrenceGrossman VolumeXXXI.Biomembranes(PartA) EditedbySidneyFleischerandLesterPacker VolumeXXXII.Biomembranes(PartB) EditedbySidneyFleischerandLesterPacker VolumeXXXIII.CumulativeSubjectIndexVolumesI-XXX EditedbyMarthaG.DennisandEdwardA.Dennis VolumeXXXIV.AffinityTechniques(EnzymePurification:PartB) EditedbyWilliamB.JakobyandMeirWilchek methodsin enzymology xvii VolumeXXXV.Lipids(PartB) EditedbyJohnM.Lowenstein VolumeXXXVI.HormoneAction(PartA:SteroidHormones) EditedbyBertW.O’MalleyandJoelG.Hardman VolumeXXXVII.HormoneAction(PartB:PeptideHormones) EditedbyBertW.O’MalleyandJoelG.Hardman VolumeXXXVIII.HormoneAction(PartC:CyclicNucleotides) EditedbyJoelG.HardmanandBertW.O’Malley VolumeXXXIX.HormoneAction(PartD:IsolatedCells,Tissues, andOrganSystems) EditedbyJoelG.HardmanandBertW.O’Malley VolumeXL.HormoneAction(PartE:NuclearStructureandFunction) EditedbyBertW.O’MalleyandJoelG.Hardman VolumeXLI.CarbohydrateMetabolism(PartB) EditedbyW.A.Wood VolumeXLII.CarbohydrateMetabolism(PartC) EditedbyW.A.Wood VolumeXLIII.Antibiotics EditedbyJohnH.Hash VolumeXLIV.ImmobilizedEnzymes EditedbyKlausMosbach VolumeXLV.ProteolyticEnzymes(PartB) EditedbyLaszloLorand VolumeXLVI.AffinityLabeling EditedbyWilliamB.JakobyandMeirWilchek VolumeXLVII.EnzymeStructure(PartE) EditedbyC.H.W.HirsandSergeN.Timasheff VolumeXLVIII.EnzymeStructure(PartF) EditedbyC.H.W.HirsandSergeN.Timasheff VolumeXLIX.EnzymeStructure(PartG) EditedbyC.H.W.HirsandSergeN.Timasheff VolumeL.ComplexCarbohydrates(PartC) EditedbyVictorGinsburg VolumeLI.PurineandPyrimidineNucleotideMetabolism EditedbyPatriciaA.HoffeeandMaryEllenJones VolumeLII.Biomembranes(PartC:BiologicalOxidations) EditedbySidneyFleischerandLesterPacker VolumeLIII.Biomembranes(PartD:BiologicalOxidations) EditedbySidneyFleischerandLesterPacker xviii methods in enzymology VolumeLIV.Biomembranes(PartE:BiologicalOxidations) EditedbySidneyFleischerandLesterPacker VolumeLV.Biomembranes(PartF:Bioenergetics) EditedbySidneyFleischerandLesterPacker VolumeLVI.Biomembranes(PartG:Bioenergetics) EditedbySidneyFleischerandLesterPacker VolumeLVII.BioluminescenceandChemiluminescence EditedbyMarleneA.DeLuca VolumeLVIII.CellCulture EditedbyWilliamB.JakobyandIraPastan VolumeLIX.NucleicAcidsandProteinSynthesis(PartG) EditedbyKivieMoldaveandLawrenceGrossman VolumeLX.NucleicAcidsandProteinSynthesis(PartH) EditedbyKivieMoldaveandLawrenceGrossman Volume61.EnzymeStructure(PartH) EditedbyC.H.W.HirsandSergeN.Timasheff Volume62.VitaminsandCoenzymes(PartD) EditedbyDonaldB.McCormickandLemuelD.Wright Volume63.EnzymeKineticsandMechanism(PartA:InitialRateand InhibitorMethods) EditedbyDanielL.Purich Volume64.EnzymeKineticsandMechanism(PartB:IsotopicProbesand ComplexEnzymeSystems) EditedbyDanielL.Purich Volume65.NucleicAcids(PartI) EditedbyLawrenceGrossmanandKivieMoldave Volume66.VitaminsandCoenzymes(PartE) EditedbyDonaldB.McCormickandLemuelD.Wright Volume67.VitaminsandCoenzymes(PartF) EditedbyDonaldB.McCormickandLemuelD.Wright Volume68.RecombinantDNA EditedbyRayWu Volume69.PhotosynthesisandNitrogenFixation(PartC) EditedbyAnthonySanPietro Volume70.ImmunochemicalTechniques(PartA) EditedbyHelenVanVunakisandJohnJ.Langone Volume71.Lipids(PartC) EditedbyJohnM.Lowenstein

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