Analytical Methods in Supramolecular Chemistry Book

Preface XIII

List of Contributors XV

1 Introduction 1
Lena Kaufmann and Christoph A. Schalley

1.1 Some Historical Remarks on Supramolecular Chemistry 1

1.2 The Noncovalent Bond: a Brief Overview 2

1.3 Basic Concepts in Supramolecular Chemistry 4

1.4 Conclusions: Diverse Methods for a Diverse Research Area 21

References 22

2 Quantitative Analysis of Binding Properties 27
Keiji Hirose

2.1 Theoretical Principles 27

2.2 A Practical Course of Binding Constant Determination by UV/Vis Spectroscopy 29

2.3 Practical Course of Action for NMR Spectroscopic Binding Constant Determination 44

2.4 Other Important Examples with Practical Actions of Data Treatment 53

2.5 Conclusion 59

References 66

3 Isothermal Titration Calorimetry in Supramolecular Chemistry 67
Franz P. Schmidtchen

3.1 Introduction 67

3.2 The Thermodynamic Platform 69

3.3 Acquiring Experimental Calorimetric Data 72

3.4 Extending the Measurement Range 88

3.5 Perspectives 100

Acknowledgment 100

References 101

4 Extraction Methods 105
Holger Stephan, Manja Kubeil, Kerstin Gloe, and Karsten Gloe

4.1 Introduction 105

4.2 The Extraction Technique 106

4.3 The Technical Process 108

4.4 The Extraction Equilibrium 109

4.5 Principles of Supramolecular Extraction 112

4.6 Examples of Supramolecular Extraction 114

4.7 Conclusions and Future Perspectives 124

Acknowledgments 125

References 125

5 Mass Spectrometry and Gas Phase Chemistry of Supramolecules 129
Dominik P. Weimann, Michael Kogej, and Christoph A. Schalley

5.1 Introduction 129

5.2 Instrumentation 130

5.3 Particularities and Limitations of Mass Spectrometry 141

5.4 Beyond Analytical Characterization: Tandem MS Experiments for the Examination of the Gas-Phase Chemistry of Supramolecules 143

5.5 Selected Examples 147

5.6 Conclusions 191

References 192

6 Diffusion NMR in Supramolecular Chemistry and Complexed Systems 197
Yoram Cohen, Liat Avram, Tamar Evan-Salem, Sarit Slovak, Noam Shemesh, and Limor Frish

6.1 Introduction 197

6.2 Concepts of Molecular Diffusion 198

6.3 Measuring Diffusion with NMR 198

6.4 Applications of Diffusion NMR in Supramolecular Chemistry: Selected Examples 209

6.5 Advantages and Limitations of High Resolution Diffusion NMR 259

6.6 Diffusion NMR and Chemical Exchange 260

6.7 Diffusion Modes and Signal Decay in Diffusion MR Experiments 265

6.8 Applications of Diffusion NMR in Complex Systems 269

6.9 Summary and Outlook 276

References 279

7 Photophysics and Photochemistry of Supramolecular Systems 287
Bernard Valeur, Màrio Nuno Berberan-Santos, Monique M. Martin, and Pascal Plaza

7.1 Introduction 287

7.2 Spectrophotometry and Spectrofluorometry 288

7.3 Time-Resolved Fluorescence Techniques 296

7.4 Fluorescence Anisotropy 311

7.5 Transient Absorption Spectroscopy 319

7.6 Concluding Remarks 332

References 334

8 Circular Dichroism Spectroscopy 337
Marie Urbanovà and Petr Maloˇn

8.1 Basic Considerations 337

8.2 Measurement Techniques (Methodology of CD Measurement) 343

8.3 Processing of Circular Dichroism Spectra 350

8.4 Theory 356

8.5 Examples of Vibrational Circular Dichroism Applications 359

8.6 Concluding Remarks 363

Abbreviations 364

References 364

Contents to Volume 2

Preface XIII

List of Contributors XV

9 Electrochemical Methods 371
Paola Ceroni, Alberto Credi, and Margherita Venturi

9.1 Introduction 371

9.2 Basic Principles of Electrochemistry 372

9.3 Overview of Electrochemical Techniques 378

9.4 Electrochemical Analysis of Supramolecular Systems 393

9.5 Selected Examples 396

9.6 Concluding Remarks 448

Acknowledgments 449

References 449

10 Crystallography and Crystal Engineering 459
Kari Rissanen

10.1 Introduction 459

10.2 Crystallography 460

10.3 Crystal Engineering 484

10.4 Methyl-Resorcinarene as a Crystal Engineering Target 487

10.5 Concluding Remarks 495

Acknowledgments 497

References 497

11 Scanning Probe Microscopy 499
Bianca A. Hermann and Regina Hoffmann-Vogel

11.1 Introduction: What Is the Strength of Scanning Probe Techniques? 499

11.2 How Do Scanning Probe Microscopes Work? 501

11.3 Which Molecules Can Be Studied? 533

11.4 What Results Have Been Obtained in the Field of Supramolecular Chemistry? 538

Acknowledgments 549

References 550

12 Single-Molecule Force Spectroscopy of Supramolecular Complexes 559
Tobias Schroeder, Volker Walhorn, Jochen Mattay, and Dario Anselmetti

12.1 Introduction and Motivation 559

12.2 Functionally Immobilizing Supramolecules 561

12.3 Supramolecular Interactions Investigated by AFM-SMFS 565

12.4 Summary and Outlook 603

Acknowledgments 604

References 604

13 Confocal Laser Scanning Microscopy: a Versatile Spectroscopic Tool for the Investigation of Molecular Gels 607
Anthony D’Alèo, Andrè Del Guerzo, and Frèdèric Fages

13.1 Introduction: Molecular Gels 607

13.2 Methods Classically Used for the Characterization of Molecular Gels 608

13.3 Confocal Laser Scanning Microscopy (CLSM) 611

13.4 Applications of CLSM to the Study of Molecular Gels 613

13.5 Conclusion 624

References 624

14 Transmission Electron Microscopy (TEM) of Radiation Sensitive Supramolecular Architectures –Strategies for a Comprehensive Structure Characterization 629
Christoph Böttcher

14.1 Introduction 629

14.2 Instrumentation 631

14.3 Contrast in TEM 640

14.4 Sample Preparation 650

14.5 Strategies and Examples to Characterize Supramolecular Structures by Complementary TEM Methods 660

Acknowledgment 698

References 699

Further Reading 709

15 The Characterization of Synthetic Ion Channels and Pores 711
Stefan Matile and Naomi Sakai

15.1 Introduction 711

15.2 Methods 713

15.3 Characteristics 719

15.4 Structural Studies 734

15.5 Concluding Remarks 738

Acknowledgment 739

References 739

16 Theoretical Methods for Supramolecular Chemistry 743
Barbara Kirchner and Markus Reiher

16.1 Introduction 743

16.2 A Survey of Theoretical Methods 746

16.3 Standard Classification of Intermolecular Interactions 766

16.4 Qualitative Understanding and Decomposition Schemes 772

16.5 General Mechanism for a Static, Step-Wise View on Host–Guest Recognition 777

16.6 Conclusions and Perspective 785

Acknowledgments 786

References 786

Index 795