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Myersalexander.Pdf (3.037Mb) SYNTHESIS AND REACTIVITY OF LOW-VALENT URANIUM AND NEPTUNIUM COMPLEXES _______________________________________ A Dissertation presented to the Faculty of the Graduate School at the University of Missouri-Columbia _______________________________________________________ In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy _____________________________________________________ By ALEXANDER J. MYERS Dr. Justin R. Walensky, Dissertation Supervisor DECEMBER 2019 The undersigned, appointed by the dean of the Graduate School, have examined the dissertation entitled SYNTHESIS AND REACTIVITY OF LOW-VALENT URANIUM AND NEPTUNIUM COMPLEXES presented by Alexander J. Myers, a candidate for the degree of Doctor of Philosophy of Chemistry, and hereby certify that, in their opinion, it is worthy of acceptance. Professor Justin R. Walensky Professor Silvia S. Jurisson Professor Wesley H. Bernskoetter Professor Bret D. Ulery Acknowledgements I would like to thank my wife, Heather Saxon, who encouraged me to go to graduate school in the first place. None of this would have happened if it wasn’t for you. My advisor, Justin Walensky, for all of his help, advice and the opportunities he has given me. I don’t know how you put up with me all these years but I’m glad you did. Wayne Lukens for all of his help; teaching me about preparing and running my SQUID and EPR samples. Charles Barnes, Steven Kelley, and Wei Wycoff, for their help with X-ray Crystallography and NMR spectroscopy Everyone in the Walensky group: Andrew Behrle, Pokpong Rungthanaphatsophon, Michael Tarlton, Robert Ward, Sean Vilanova, Alexander Gremillion, Andrew Lane, Andrew Breshears, Kira Behm, Matthew Vollmer, Steven Renfroe, and Jonathan Fajen. ii TABLE OF CONTENTS Acknowledgements ........................................................................................................ ii List of Figures ................................................................................................................ vi List of Tables................................................................................................................... x List of Abbreviations .....................................................................................................xii Abstract ........................................................................................................................ xiv Introduction ..................................................................................................................... 1 t Chapter 1: Structure and Properties of [(4,6- Bu2C6H2O)2Se]2An(THF)2, An = U, Np, and Their Reaction with p-Benzoquinone .................................................................... 6 Introduction ..................................................................................................................... 6 Experimental ................................................................................................................... 7 General Considerations .................................................................................................... 7 General considerations for 237Np ..................................................................................... 8 Crystallographic Data Collection and Structure Determination ...................................... 10 Magnetic Measurements ................................................................................................ 12 EPR Experimental ......................................................................................................... 17 Results and Discussion .................................................................................................. 18 Conclusion .................................................................................................................... 30 Chapter 2: U(III) and Th(IV) Alkyl Complexes as Potential Starting Materials...... 31 Introduction ................................................................................................................... 31 Experimental ................................................................................................................. 32 General Considerations .................................................................................................. 32 Crystallographic Data Collection and Structure Determination ...................................... 36 iii Magnetism Measurements ............................................................................................. 38 Results and Discussion .................................................................................................. 40 Conclusion .................................................................................................................... 48 Chapter 3: Synthesis and Utility of a Neptunium(III) Hydrocarbyl Complex .......... 49 Introduction ................................................................................................................... 49 Experimental ................................................................................................................. 51 General considerations ................................................................................................... 51 General considerations for 237Np .................................................................................... 52 Crystallographic Data Collection and Structure Determination ...................................... 53 Magnetic Measurements ................................................................................................ 55 Results and Discussion .................................................................................................. 57 Conclusion .................................................................................................................... 65 Chapter 4: Formation of Np(IV)-Chalcogenido Bonds from E-E Bond Cleavage with a Np(III) Aryloxide Complex ...................................................................................... 66 Introduction ................................................................................................................... 66 Experimental ................................................................................................................. 67 General Considerations for 237Np ................................................................................... 67 Crystallographic Data Collection and Structure Determination ...................................... 69 Results ........................................................................................................................... 71 Appendix A: Influence of Substituents on the Electronic Structure of Mono- and Bis(Phosphido) Thorium(IV) Complexes ................................................................... 74 Introduction ................................................................................................................... 74 Experimental ................................................................................................................ 76 iv General Considerations .................................................................................................. 76 Computational Details ................................................................................................... 81 Crystal Structure Determination and Refinement ........................................................... 82 Results and Discussion .................................................................................................. 84 Spectroscopy and TD-DFT Calculations ........................................................................ 90 Conclusion .................................................................................................................... 99 Appendix B: Coordination Chemistry and QTAIM Analysis of Homoleptic i Dithiocarbamate Complexes, M(S2CN Pr2)4, M = Ti, Zr, Hf, Th, U, Np ................. 101 Introduction ................................................................................................................. 101 Experimental ............................................................................................................... 103 General Considerations ................................................................................................ 103 General Considerations for 237Np ................................................................................. 103 Crystallographic Data Collection and Structure Determination .................................... 108 Computational Details ................................................................................................. 110 Results ......................................................................................................................... 111 Topological Properties of the Electron Density ............................................................ 116 Integrated Properties of the Electron Density ............................................................... 117 Discussion ................................................................................................................... 119 Conclusion .................................................................................................................. 120 References ................................................................................................................... 121 Vita ............................................................................................................................
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