title: Simultaneous determination of 1H-1H and 1H-13C residual dipolar couplings in a chiral liquid crystal solvent using a natural abundance HSQC experiment.
abstract: A high-resolution, phase-sensitive, natural abundance F2-coupled 1H-13C HSQC (F2HSQC) NMR experiment was developed to measure simultaneously both (n)D(HH) and 1D(CH) residual dipolar couplings (RDCs) of small molecules present in a chiral polypeptide liquid crystal solvent system composed of poly-gamma-benzyl-L-glutamate (PBLG) in CDCl3. Because this is an indirect-detection NMR experiment, the relatively small amount of sample (7.5 mg in this study) and short acquisition times (5 h) that are required make this HSQC experiment well suited for samples that are either limited in solubility or in quantity or require short analysis times. The F2HSQC experiment can be performed without any specialized equipment or sample modification and can enhance our ability to measure RDCs accurately and rapidly in polypeptide liquid crystal solvents.
authors.affiliation: Wyeth Research, Discovery Analytical Chemistry, CN 8000, Princeton, New Jersey 08543-8000, USA. marathv@wyeth.com
authors.forename: Vasilios M
authors.initials: VM
authors.lastname: Marathias
authors.forename: Igor
authors.initials: I
authors.lastname: Goljer
authors.forename: Alvin C
authors.initials: AC
authors.lastname: Bach
mesh_terms: D002247:Carbon Isotopes; D003461:Crystallography / Q000379:methods*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008832:Microchemistry / Q000379:methods*; D010455:Peptides / Q000032:analysis / Q000737:chemistry*; D011522:Protons; D012997:Solvents / Q000032:analysis / Q000737:chemistry*; D013237:Stereoisomerism
chemical_list: D002247:Carbon Isotopes; D010455:Peptides; D011522:Protons; D012997:Solvents