Analytical Methods in Supramolecular Chemistry E-Book
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- Herausgeber: Wiley-VCH
- Kategorie: Wissenschaft und neue Technologien
- Sprache: Englisch
The second edition of "Analytical Methods in Supramolecular Chemistry" comes in two volumes and covers a broad range of modern methods and techniques now used for investigating supramolecular systems, e. g. NMR spectroscopy, mass spectrometry, extraction methods, crystallography, single molecule spectroscopy, electrochemisty, and many more. In this second edition, tutorial inserts have been introduced, making the book also suitable as supplementary reading for courses on supramolecular chemistry. All chapters have been revised and updated and four new chapters have been added. A must-have handbook for Organic and Analytical Chemists, Spectroscopists, Materials Scientists, and Ph.D. Students in Chemistry. From reviews of the first edition: "This timely book should have its place in laboratories dealing with supramolecular objects. It will be a source of reference for graduate students and more experienced researchers and could induce new ideas on the use of techniques other than those usually used in the laboratory." Journal of the American Chemical Society (2008) VOL. 130, NO. 1 doi: 10.1021/ja0769649 "The book as a whole or single chapters will stimulate the reader to widen his horizon in chemistry and will help him to have new ideas in his research." Anal Bioanal Chem (2007) 389:2039-2040 DOI: 10.1007/s00216-007-1677-1
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Seitenzahl: 1471
Veröffentlichungsjahr: 2012
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Table of Contents
Related Titles
Title Page
Copyright
Preface
List of Contributors
Volume I
Chapter 1: Introduction
1.1 Some Historical Remarks on Supramolecular Chemistry
1.2 The Noncovalent Bond: a Brief Overview
1.3 Basic Concepts in Supramolecular Chemistry
1.4 Conclusions: Diverse Methods for a Diverse Research Area
References
Chapter 2: Quantitative Analysis of Binding Properties
2.1 Theoretical Principles
2.2 A Practical Course of Binding Constant Determination by UV/Vis Spectroscopy
2.3 Practical Course of Action for NMR Spectroscopic Binding Constant Determination
2.4 Other Important Examples with Practical Actions of Data Treatment
2.5 Conclusion
References
Chapter 3: Isothermal Titration Calorimetry in Supramolecular Chemistry
3.1 Introduction
3.2 The Thermodynamic Platform
3.3 Acquiring Experimental Calorimetric Data
3.4 Extending the Measurement Range
3.5 Perspectives
Acknowledgment
References
Chapter 4: Extraction Methods
4.1 Introduction
4.2 The Extraction Technique
4.3 The Technical Process
4.4 The Extraction Equilibrium
4.5 Principles of Supramolecular Extraction
4.6 Examples of Supramolecular Extraction
4.7 Conclusions and Future Perspectives
Acknowledgments
References
Chapter 5: Mass Spectrometry and Gas Phase Chemistryof Supramolecules
5.1 Introduction
5.2 Instrumentation
5.3 Particularities and Limitations of Mass Spectrometry
5.4 Beyond Analytical Characterization: Tandem MS Experiments for the Examinationof the Gas-Phase Chemistry of Supramolecules
5.5 Selected Examples
5.6 Conclusions
References
Chapter 6: Diffusion NMR in Supramolecular Chemistry and Complexed Systems
6.1 Introduction
6.2 Concepts of Molecular Diffusion
6.3 Measuring Diffusion with NMR
6.4 Applications of Diffusion NMR in Supramolecular Chemistry: Selected Examples
6.5 Advantages and Limitations of High Resolution Diffusion NMR
6.6 Diffusion NMR and Chemical Exchange
6.7 Diffusion Modes and Signal Decay in Diffusion MR Experiments
6.8 Applications of Diffusion NMR in Complex Systems
6.9 Summary and Outlook
References
Chapter 7: Photophysics and Photochemistry of Supramolecular Systems
7.1 Introduction
7.2 Spectrophotometry and Spectrofluorometry
7.3 Time-Resolved Fluorescence Techniques
7.4 Fluorescence Anisotropy
7.5 Transient Absorption Spectroscopy
7.6 Concluding Remarks
References
Chapter 8: Circular Dichroism Spectroscopy
8.1 Basic Considerations
8.2 Measurement Techniques (Methodology of CD Measurement)
8.3 Processing of Circular Dichroism Spectra
8.4 Theory
8.5 Examples of Vibrational Circular Dichroism Applications
8.6 Concluding Remarks
References
Volume II
Chapter 9: Electrochemical Methods
9.1 Introduction
9.2 Basic Principles of Electrochemistry
9.3 Overview of Electrochemical Techniques
9.4 Electrochemical Analysis of Supramolecular Systems
9.5 Selected Examples
9.6 Concluding Remarks
Acknowledgments
References
Chapter 10: Crystallography and Crystal Engineering
10.1 Introduction
10.2 Crystallography
10.3 Crystal Engineering
10.4 Methyl-Resorcinarene as a Crystal Engineering Target
10.5 Concluding Remarks
Acknowledgments
References
Chapter 11: Scanning Probe Microscopy
11.1 Introduction: What Is the Strength of Scanning Probe Techniques?
11.2 How Do Scanning Probe Microscopes Work?
11.3 Which Molecules Can Be Studied?
11.4 What Results Have Been Obtained in the Field of Supramolecular Chemistry?
Acknowledgments
References
Chapter 12: Single-Molecule Force Spectroscopy of Supramolecular Complexes
12.1 Introduction and Motivation
12.2 Functionally Immobilizing Supramolecules
12.3 Supramolecular Interactions Investigated by AFM-SMFS
12.4 Summary and Outlook
Acknowledgments
References
Chapter 13: Confocal Laser Scanning Microscopy: a Versatile Spectroscopic Tool for the Investigation of Molecular Gels
13.1 Introduction: Molecular Gels
13.2 Methods Classically Used for the Characterization of Molecular Gels
13.3 Confocal Laser Scanning Microscopy (CLSM)
13.4 Applications of CLSM to the Study of Molecular Gels
13.5 Conclusion
References
Chapter 14: Transmission Electron Microscopy (TEM) of Radiation Sensitive Supramolecular Architectures – Strategies for a Comprehensive Structure Characterization
14.1 Introduction
14.2 Instrumentation
14.3 Contrast in TEM
14.4 Sample Preparation
14.5 Strategies and Examples to Characterize Supramolecular Structures by Complementary TEM Methods
Acknowledgment
References
Chapter 15: The Characterization of Synthetic Ion Channels and Pores
15.1 Introduction
15.2 Methods
15.3 Characteristics
15.4 Structural Studies
15.5 Concluding Remarks
Acknowledgment
References
Chapter 16: Theoretical Methods for Supramolecular Chemistry
16.1 Introduction
16.2 A Survey of Theoretical Methods
16.3 Standard Classification of Intermolecular Interactions
16.4 Qualitative Understanding and Decomposition Schemes
16.5 General Mechanism for a Static, Step-Wise View on Host–Guest Recognition
16.6 Conclusions and Perspective
Acknowledgments
References
Index
Related Titles
Samori, P. / Cacialli, F. (eds.)
Functional Supramolecular Architectures
for Organic Electronics and Nanotechnology
2010
ISBN: 978-3-527-32611-2
Sliwa, W. / Kozlowski, C.
Calixarenes and Resorcinarenes
Synthesis, Properties and Applications
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Ceroni, P., Credi, A., Venturi, M. (eds.)
Electrochemistry of Functional Supramolecular Systems
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Andrews, D. L. (ed.)
Encyclopedia of Applied Spectroscopy
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Vögtle, F. / Richardt, G. / Werner, N.
Dendrimer Chemistry
Concepts, Syntheses, Properties, Applications
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ISBN: 978-3-527-32066-0
van Leeuwen, P. W. N. M. (ed.)
Supramolecular Catalysis
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Diederich, F., Stang, P. J., Tykwinski, R. R. (eds.)
Modern Supramolecular Chemistry
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The Editors
Prof. Dr. Christoph Schalley
Freie Universität Berlin
Institut für Chemie und Biochemie
Takustr. 3
14195 Berlin
Germany
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© 2012 Wiley-VCH Verlag & Co. KGaA, Boschstr. 12, 69469 Weinheim, Germany
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Preface
Editing the second edition of “Analytical Methods in Supramolecular Chemistry” was a great pleasure – in particular, since all contributors to the first edition immediately agreed to update their first edition chapters with the progress made since the book first appeared in print. In addition, several new chapters have been added so that the second edition is now a two-volume set and contains an even broader overview of the methods that are applied to investigate and characterize supramolecules and large non-covalent aggregates.
The contributions dealing with methods to analyze the thermochemistry of molecular recognition through NMR and UV/VIS titrations by Keiji Hirose, through isothermal titration calorimetry by Franz Schmidtchen and through extraction methods by Holger Stephan, Maja Kubeil and Kerstin and Karsten Gloe include many new examples which add more detailed insight into the methods described.
While the first edition was certainly somewhat biased towards discrete supramolecules, the new chapters contribute information on methods devoted to the study of extended structures. Besides the chapter on membrane pores by Stefan Matile and Naomi Sakai, which was already part of the first edition, Christoph Böttcher introduces the reader to (cryo-)transmission electron microscopy. A prominent example in this chapter is the structural characterization of gels based on amphiphilic hexonamides. Anthony D'Aléo, André Del Guerzo and Frédéric Fages describe the spectroscopic characterization of gels by confocal laser scanning microscopy. Furthermore, Yoram Cohen and his coworkers added to their chapter on DOSY-NMR methods work on extended systems such as supramolecular polymers, zeolites, micelles, cells and tissues and Kari Rissanen included a substantial addition on crystal engineering in the crystallography chapter.
However, the second edition also extends the length scales at the other end: Bianca Hermann's and Regine Hofmann's contribution on scanning probe microscopic methods is followed by a chapter on single-molecule force spectroscopy provided by Tobias Schroeder, Jochen Mattay and Dario Anselmetti.
Finally, the electrochemical investigation of supramolecules is introduced by Paola Ceroni, Alberto Credi and Margherita Venturi – a chapter which nicely complements the contributions on optical spectroscopy as described in the chapters on photochemistry by Bernard Valeur, Mário Berberan-Santos, Monique Martin and Pascal Plaza and on CD spectroscopy by Marie Urbanova and Petr Malo, as well as that on mass spectrometry.
Although the techniques described in the second edition still represent only a selection from the large variety of methods used for the examination of supramolecular aggregates, the coverage is now significantly broader than in the first edition. To make the book useful for experts as well as beginners in the field, many authors have picked up the idea of Bianca Hermann, who included a number of tutorials in her first-edition chapter. These tutorials are printed separately from the text and may be useful to introduce the beginner to specific points with which the experts in the field are probably familiar.
Well aware of the huge effort required to review the methods critically , I am very grateful to all authors that contributed to this second edition of the “Analytical Methods in Supramolecular Chemistry”. They have done a great job in describing the many different methods in a well-readable, but detailed and not too simplistic way, pointing out the potential and the pitfalls of the different methods. The large variety of supramolecular complexes and the difficulties that arise for their characterization from weak bonds and fast dynamics require often the application of several complementary methods. Therefore, a broad knowledge of the techniques that are available and their scope and limitations is required for successful work in supramolecular chemistry. I sincerely hope that the present second edition contributes to this endeavor.
Berlin, October 2011
Christoph A. Schalley
Freie Universität Berlin
List of Contributors
Volume I
Chapter 1
Introduction
Lena Kaufmann and Christoph A. Schalley
1.1 Some Historical Remarks on Supramolecular Chemistry
The fundaments of Supramolecular Chemistry date back to the late nineteenth century, when some of the most basic concepts for this research area were developed. In particular, the idea of coordination chemistry was formulated by Alfred Werner [1], the lock-and-key concept was introduced by Emil Fischer [2], and Villiers and Hebd discovered cyclodextrins, the first host molecules (1891) [3]. A few years later, Paul Ehrlich devised the concept of receptors in his Studies on Immunity (1906) [4] by stating that any molecule can only have an effect on the human body if it is bound (“Corpora non agunt nisi fixata”). Several of these concepts were refined and modified later. Just to provide one example, Daniel Koshland formulated the induced fit concept (1958) for binding events to biomolecules which undergo conformational changes in the binding event [5]. The induced fit model provides a more dynamic view of the binding event, compared with the rather static lock-and-key principle and is thus more easily able to explain phenomena such as cooperativity. Even the German word for “Supramolecule” appeared in the literature as early as 1937, when Wolf and his coworkers introduced the term “Übermolekül” to describe the intermolecular interaction of coordinatively saturated species such as the dimers of carboxylic acids [6].
The question immediately arising from this brief overview on the beginnings of supramolecular chemistry is: Why wasn't it recognized earlier as a research area in its own right? Why did it take more than 40 years from the introduction of the term “Übermolekül” to Lehn's definition of supramolecular chemistry [7] as the “chemistry of molecular assemblies and of the intermolecular bond?” [8].
There are at least two answers. The first relates to the perception of the scientists involved in this area. As long as chemistry accepts the paradigm that properties of molecules are properties of the molecules themselves, while the interactions with the environment are small and – to a first approximation – negligible, there is no room for supramolecular chemistry as an independent field of research. Although solvent effects were already known quite early, this paradigm formed the basis of the thinking of chemists for a long time. However, with an increasing number of examples of the importance of the environment for the properties of a molecule, a paradigm shift occurred in the late 1960s. Chemists started to appreciate that their experiments almost always provided data about molecules in a particular environment. It became clear that the surroundings almost always have a non-negligible effect. Consequently, the intermolecular interactions became the focus of research and a new area was born. With this in mind, chemists were suddenly able to think about noncovalent forces, molecular recognition, templation, self-assembly, and many other aspects into which supramolecular chemistry meanwhile diversified.
The second answer is no less important, although somewhat more technical in nature. Supramolecules are often weakly bound and highly dynamic. Based on intermolecular interactions, complex architectures can be generated, often with long-range order. All these features need specialized experimental methods, many of which still had to be developed in the early days of supramolecular chemistry. As observed quite often, the progress in a certain research area – here supramolecular chemistry – depends on the development of suitable methods. An emerging new method on the other hand leads to further progress in this research field, since it opens new possibilities for the experimenters. It is this second answer which prompted us to assemble the present book in order to provide information on the current status of the methods used in supramolecular chemistry. It also shows how diverse is the methodological basis on which supramolecular chemists rely.
1.2 The Noncovalent Bond: a Brief Overview
Before going into detail with respect to the analytical methods that are applied in contemporary supramolecular chemistry, this brief introduction to some basic concepts and research topics within supramolecular chemistry is intended to provide the reader with some background. Of course, it is not possible to give a comprehensive overview. It is not even achievable to review the last 40 or so years of supramolecular research in a concise manner. For a more in-depth discussion, the reader is thus referred to some excellent text books on supramolecular chemistry [7].
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