title: HSQC-ADEQUATE: an investigation of data requirements.
abstract: Utilizing (13)C-(13)C connectivity networks for the assembly of carbon skeletons from HSQC-ADEQUATE spectra was recently reported. HSQC-ADEQUATE data retain the resonance multiplicity information of the multiplicity-edited GHSQC spectrum and afford a significant improvement in the signal-to-noise (s/n) ratio relative to the 1,1-ADEQUATE data used in the calculation of the HSQC-ADEQUATE spectrum by unsymmetrical indirect covariance (UIC) processing methods. The initial investigation into the computation of HSQC-ADEQUATE correlation plots utilized overnight acquisition of the 1,1-ADEQUATE data used for the calculation. In this communication, we report the results of an investigation of the reduction in acquisition time for the 1,1-ADEQUATE data to take advantage of the s/n gain during the UIC processing to afford the final HSQC-ADEQUATE correlation plot. Data acquisition times for the 1,1-ADEQUATE spectrum can be reduced to as little as a few hours, while retaining excellent s/n ratios and all responses contained in spectra computed from overnight data acquisitions. Concatenation of multiplicity-edited GHSQC and 1,1-ADEQUATE data also allows the interrogation of submilligram samples with 1,1-ADEQUATE data when using spectrometers equipped with 1.7-mm Micro CryoProbes ™.
authors: Merck Research Laboratories, Discovery and Preclinical Sciences-Global Chemistry, Structure Elucidation Group, Summit, NJ 07901, USA. gary.martin2@merck.com
authors: Gary E
authors: GE
authors: Martin
authors: Bruce D
authors: BD
authors: Hilton
authors: M Robert
authors: MR
authors: Willcott
authors: Kirill A
authors: KA
authors: Blinov
mesh_terms: D002247:Carbon Isotopes; D016208:Databases, Factual; D009682:Magnetic Resonance Spectroscopy / Q000379:methods* / Q000592:standards; D015394:Molecular Structure; D012015:Reference Standards; D013331:Strychnine / Q000737:chemistry*
chemical_list: D002247:Carbon Isotopes; D013331:Strychnine