- Title Information
- Title
- Synergistic Effect of X-ray Crystallography and Solution NMR
on Structural Characterization of Organolithium Complexes
- Name:
Personal
- Name Part
- Guang, Jie
- Role
- Role Term:
Text
- creator
- Origin Information
- Copyright Date
- 2015
- Physical Description
- Extent
- xvi, 135 p.
- digitalOrigin
- born digital
- Note
- Thesis (Ph.D. -- Brown University (2015)
- Name:
Personal
- Name Part
- Williard, Paul
- Role
- Role Term:
Text
- Director
- Name:
Personal
- Name Part
- Basu, Amit
- Role
- Role Term:
Text
- Reader
- Name:
Personal
- Name Part
- Seto, Christopher
- Role
- Role Term:
Text
- Reader
- Name:
Corporate
- Name Part
- Brown University. Chemistry
- Role
- Role Term:
Text
- sponsor
- Genre (aat)
- theses
- Abstract
- Structural characterization of organolithium compounds in solution is an important but challenging task. Solution nuclear magnetic resonance (NMR) and X-ray crystallography are two of the most powerful and widely used methods to overcome this challenge. However the correct and reliable interpretation for the NMR spectra of organolithium complexes is difficult, because a) NMR samples contain impurities because organolithium compounds are air-sensitive; b) even pure samples can be mixture as organolithium reagents form various oligomers and mixed aggregates; c) peak assignments in NMR spectra can be ambiguous as different oligomers and aggregates may have very similar structures and present duplicate absorbance. On the other hand, the limitation of X-ray crystallography is also obvious: as a solid-state method, X-ray diffraction (XRD) does not offer structural information for the liquid state. However the combination of NMR and XRD presents a synergistic effect, because NMR helps optimize the preparation conditions of various crystals and X-ray analysis offers trustworthy structural information and unambiguous assignment to partial NMR spectra. This combination becomes the crucial foundation for the interpretation of the NMR data. A variety of systems has been studied by this NMR/XRD integrated protocal including lithium enolates, lithium amide bases and perfluoro Grignard reagents. This thesis incorporates examples that illustrate the application of X-ray crystallography and a variety of multi nuclei (1H, 2H, 6Li, 13C, 19F) NMR techniques including referenced diffusion-ordered NMR spectroscopy (DOSY) to structural analysis.
- Subject
- Topic
- organolithium
- Subject
- Topic
- solution NMR
- Subject (FAST)
(authorityURI="http://id.worldcat.org/fast", valueURI="http://id.worldcat.org/fast/1047962")
- Topic
- Organolithium compounds
- Subject (FAST)
(authorityURI="http://id.worldcat.org/fast", valueURI="http://id.worldcat.org/fast/1181820")
- Topic
- X-ray crystallography
- Record Information
- Record Content Source (marcorg)
- RPB
- Record Creation Date
(encoding="iso8601")
- 20150601
- Language
- Language Term:
Code (ISO639-2B)
- eng
- Language Term:
Text
- English
- Identifier:
DOI
- 10.7301/Z0NC5ZKV
- Access Condition:
rights statement
(href="http://rightsstatements.org/vocab/InC/1.0/")
- In Copyright
- Access Condition:
restriction on access
- Collection is open for research.
- Type of Resource (primo)
- dissertations