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Transition-Metal Complexes of Beta-Furfuraldoxime." (1972)

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Transition-Metal Complexes of Beta-Furfuraldoxime. Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1972 Transition-Metal Complexes of Beta- Furfuraldoxime. Max Earl Pickerill Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Pickerill, Max Earl, "Transition-Metal Complexes of Beta-Furfuraldoxime." (1972). LSU Historical Dissertations and Theses. 2355. https://digitalcommons.lsu.edu/gradschool_disstheses/2355 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Historical Dissertations and Theses by an authorized administrator of LSU Digital Commons. For more information, please contact [email protected]. INFORMATION TO USERS This dissertation was produced from a microfilm copy of the original document. While the most advanced technological means to photograph and reproduce this document have been used, the quality is heavily dependent upon the quality of the original submitted. The following explanation of techniques is provided to help you understand markings or patterns which may appear on this reproduction. 1. The sign or “target'' for pages apparently lacking from the document photographed is "Missing Page(s)". If it was possible to obtain the missing page(s) or section, they are spliced into the film along with adjacent pages. This may have necessitated cutting thru an image and duplicating adjacent pages to insure you complete continuity. 2. When an image on the film is obliterated with a large round black mark, it is an indication that the photographer suspected that the copy may have moved during exposure and thus cause a blurred image. You will find a good image of the page in the adjacent frame. 3. 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University Microfilms 300 North Zeeb Road Ann Arbor, Michigan 48106 A Xerox Education Company 73-13,679 PICKERILL, Max Earl, 1925- TRANSITION METAL COMPLEXES OF/0 -FURFURALDOXIME. The Louisiana State University and Agricultural and Mechanical College, Ph.D., 1972 Chemistry, inorganic University Microfilms, A XEROX Company , Ann Arbor, Michigan THIS DISSERTATION HAS BEEN MICROFILMED EXACTLY AS RECEIVED TRANSITION METAL COMPLEXES OF 0“FURFURALDOXIME A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Chemistry by Max Earl Pickerill B.S., Kansas State College at Pittsburg, I95I M.S., Fort Hays Kansas State College, 1953 December, 1972 PLEASE NOTE: Some pages may have i nd i st inet print. Filmed as received. University Microfilms, A Xerox Education Company To Eddie, Natalie, David, Beverly, Cindy and Jon ii ACKNOWLEDGMENT The writer wishes to express his deepest appreciation to Dr. Buddhadev Sen, under whose direction this work was performed, for his helpful guidance throughout the course of this investigation, and for his patience, understanding, motivation and friendship. The author would like also to express his thanks to Dr. George Newkome, Dr. Frank Cartledge, Dr. William Baddley, and Mr. Joseph Pagano for valuable discussions and suggestions. As an NSF participant, the author further acknowledges Dr. Robert Nauman, the director of the NSF program, for his counseling and stimulating harassment. Final acknowledgment goes to the author's wife, Maxine, for "holding the fort" during his absence. The author gratefully acknowledges financial support received from a Science Faculty Fellowship awarded by the National Science Foundation for part of this investigation. The writer also wishes to thank the Charles E. Coates Memorial Fund of the LSU Foundation donated by George H. Coates for expenses pertinent to the publication of the doctoral dissertation. iii TABLE OF CONTENTS Page ACKNOWLEDGMENT............................................... iii LIST OF S Y M B O L S ............................................. vi LIST OF TABLES.................................................viii LIST OF F I G U R E S ............................................ ix ABSTRACT........................ x INTRODUCTION ................................................. xii CHAPTER I - THEORY A. Inorganic Complex Compounds ............ 1 B. O x i m e s ............................................ k C. Oxime Preparations ................................ 4 D. Stereoisomerism.................................... 7 E. Transitional Metal Complexes with O x i m e s .......... 15 F. Furfuraldoxime as a Chelate Group ......... 20 G. Hydrogen Bonding .................................. 23 CHAPTER II - EXPERIMENTAL A. Materials.......................................... 23 B. Preparation of the C o m p o u n d s ...................... 25 C. Spectrophotometric Measurements.................... 28 D. Magnetic Susceptibility Measurement................ 29 E. Conductivity Measurements.......................... 30 F. Elemental A n a l y s i s ............................ 3° iv Page G. Melting Point ....................................... 31 H. Molecular Weights................................... 31 CHAPTER III - RESULTS AND DISCUSSIONS A. Physicochemical D a t a ............................... 32 B. Infrared Spectra ................................... 35 C. Conductivity....................................... 3$ D. Magnetic Susceptibilities........................... 61 E. Bonding........................ .................. 61 F. Electronic Spectra ................................. 6k CONCLUSIONS................................................ 68 LIST OF REFERENCES.......................................... TO VITA ........................................................ lk v LIST OF SYMBOLS py pyridine giy glycine acac acetylacetonate en ethylened iamine Ph phenyl tren tris-(aminoethyl)amine phenan phenanthroline HPPK syn-phenyl-2 -pyridlyketoxime PPK ketoximate anion DMSO dimethylsulfoxide EMF d imethy 1 f ormamid e m. p . melting point in degrees centigrade n.m.r. nuclear magnetic resonance p.p.m. parts per million ASIS aromatic solvent induced shift Hz hertz IMS tetramethylsilane V> dipole moment INDO incomplete neglect differential overlap D Debye B.M. Bohr Magneton FDH 2 -furfuraldoxime FD furfuraldoximate anion vi dh2 DMG or dimethylglyoxime DH dimethylglyoxime less the oximino proton V frequency X magnetic susceptibility T Mulliken triply degenerate symmetry term A Mulliken singly degenerate symmetry term (1 ) symmetry state symmetric to rotation (2 ) symmetry state antisymmetric to rotation i.r. infrared M metal (II) oxidation state of two (III) oxidation state of three DMG dimethylglyoxime E-Z Entgegen-Zusammen e.u. entropy unit vii LIST OF TABLES Table Page I. Elemental Analysis of the Compounds................... 33 II. Properties of the Compounds........................... 3^ III. I. R. Spectra in cm 1 ................................. 5° IV. Molar Conductance of the M(ll) and M(lll)Complexes in E t h a n o l ........................................ 59 V. Theoretical and Observed Magnetic Moments for the M(ll) and M(lll) Complexes in the Solid State.... 60 VI. Absorption-Band Positions of Electronic Spectra for the M(II) and the M(lll) C o m p l e x e s ................ 66 VII. Spectral Assignments for Metal Complexes of j3-Furfuraldoxime.................................. 67 viii LIST OF FIGURES Figure Page 1. Infrared Hydroxyl Stretching Bands of Hydrogen Bound Groups in (a) Mn(FDH)2 Cl2 (b) Zn(FDH)2Cl2 (<0 Ni(FDH)2Cl2 (d) Pd(FDH)2Cl2 (e) Cu (FDH)2C12 (f) Fe(FDH)2 C12 (g) Co(FDH)2 C12 .................. 51 2. Infrared Low Energy Bands (2000-600 cm *) (a) 0-FDH mull in C4 C16 (b) 0.2 M j8“FDH in CC14 ............................ 52 3 . Infrared High Energy Bands (if000-2000 cm x) (a) jfJ-FDH mull in C4 C16 (b) 0.2 M 0-FDH in CHC13 (c) 0.1 M 0-FDH in CHC13 (d) 0.2 M 0-FDH in CC14 ............................ 53 k. Infrared Low Energy Bands of Cu(FDH)2C12 .......... 5^ 5. Infrared Hydroxyl Stretching Band of Hydrogen Bound Groups in the Tris Complexes (a) Cr(FDH)3Cl3 (b) Fe(FDH)3Cl3 (c) Infrared High Energy Bands of Pd(FD)2 .......... 55 6 . Framework Model of the Tris FDH C o m p l e x e s .......... 56 7 . Framework Model of the Bis FDH Complexes............ 57 ix ABSTRACT The ligand, 2-furfuraldoxime, forms air stable crystalline complexes with the bi- and trivalent transitional metal chlorides from chromium to zinc. These compounds have not previously been characterized. They have the general formula M(FDH)XC1X in which x is 2 or 3 depending upon the charge on the central metal cation. Analytical and spectral data indicate that the metal is six coordinate
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