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Xerox University Microfilms 300 North Zeeb Road Ann Arbor, Michigan 48106 76- 17,990 INFORMATION TO USERS This material 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. When a map, drawing or chart, etc., was part of the material being photographed the photographer followed a definite method in "sectioning" the material. It is customary to begin photoing at the upper left hand corner of a large sheet and to continue photoing from left to right in equal sections with a small overlap. If necessary, sectioning is continued again — beginning below the first row and continuing on until complete. 4. The majority of users indicate that the textual content is of greatest value, however, a somewhat higher quality reproduction could be made from "photographs" if essential to the understanding of the dissertation. Silver prints of "photographs" may be ordered at additional charge by writing the Order Department, giving the catalog number, title, author and specific pages you wish reproduced. 5. PLEASE NOTE: Some pages may have indistinct print. Filmed as received. Xerox University Microfilms 300 North Zeeb Road Ann Arbor, Michigan 48106 76- 17,990 HUNG, Yann, 1948- STUDIES ON TRANSITION METAL ION COMPLEXES OF MULTIDENTATE LIGANDS. I . KINETICS OF AQUATION OF DICHLORO-TETRAAMINE COMPLEXES OF COBALT(III) INVOLVING MACROCYCLIC COMPLEXES. I I . STEREORESTRICTIVE CHELATION—METAL COMPLEXES OF SPARTEINE AND BISPIDINE. The Ohio State U niversity, Ph.D., 1976 Chemistry, inorganic Xerox University Microfilms,Ann Arbor, Michigan 48106 0 1976 YANN HUNG ALL RIGHTS RESERVED STUDIES ON TRANSITION METAL ION COMPLEXES OF MULTIDENTATE LIGANDS. I. Kinetics of Aquation of Dichloro-tetraamine Complexes of Cobalt(IU) Involving Macrocyclic Complexes. II. Stereorestrictive Chelation—Metal Complexes of Sparteine and Bispidine. DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Yann Hung, B. S. •M-l-l-H-H-H- The Ohio State University 1976 Reading Committee: Approved By Dr. D. K. Busch Dr. Eugene P. Schram Dr. Gary G. Christoph J § . f (■ i A dviser ACKNOWLEDGEMENT I would like to express my sincere appreciation to those individuals who helped me to learn, especially my parents and Professor Daryle H. Busch. CURRICULUM VITAE November 18 1948 B orn—Taipei, Taiwan 1970 B. S ., National Taiwan University, Taipei* Taiwan 1970-1973 Teaching Assistant, Department of Chemistry, The Ohio State University, Columbus, Ohio 1973-1974 Stauffer Chemical Company Fellowship 1974-1976 Research Assistant, The Ohio State Univer­ sity, Columbus, Ohio 1976 Ph.D ., The Ohio State University, Columbus Ohio FIELD OF STUDY Major Field: Inorganic Chemistry Studies in Coordination Chemistry, Professor Daryle H. Busch TABLE OF CONTENTS Page No.. Acknowledgement .................................................................................................. ii Curriculum Vitae...................................................................... iii List of Tables ............... viii List of Figures ........................................................................ x Kinetics of Aquation of Dichloro-tetraamine Complexes of Cobalt(IIl) Involving Macrocyclic Ligands. I. Introduction ....................... .......................................................... .1 Aquation of Cobalt Complexes ................. 6 Aquation of trans-Complexes .................................................. 7 Aquation of cis-C omplexe s ...................................................... .4 5 Hg2+ Induced Aquation ...........................................................................................17 Base Hydrolysis of Cobalt(H3) Complexes ..................... 18 Anation of Cobalt(H3). .................................... ........22 Statement of the Problem .............................................................................................24 n. Experimental... ....................................................................... 25 Physical Measurements ...............................................................................................25 Syntheses ............................................. 26 K inetics .............................. 31 HI. Results and Discussion ................................................................................ 34 Syntheses and Characterization of Complexes ......................................................35 trans-[Co(MAC)Cl;]+ Complexes ........................................................... 35 Isomers of trans-[Co( [lSjaneN^C^]"*". ................... .51 Isomers of trans-[Co( [lGjaneNJ Cl?]* ..............................................................58 cis-[Co(MAC)X^]+ Complexes ............................................................................ 60 TABLE OF CONTENTS Page No. Kinetic Studies. ............ 67 Aquation of trans-[Co(MAC)Cl?]+ Complexes ............................ .68 Case I. Aquation of trans-[Co([i3]aneN4)Cl2]+. ......... 68 Case II. Isomerization of trans-[Co([l3]aneNa)(HgO)2]3t ........................76 Case HI. Aquation of trans(I)-[Co([l5]aneNJC1?]+ ................................... 76 Case IV. Aquation of trans(ID-[Co([l5]aneNa)Cl2]+. .............79 Case V. Conversion of isomer II to isomer I of trans-[Co([l5]- aneN4)Cl(H20)]2+ in aqueous solution ..................................... .82 Case VI. Aquation of trans-[Co([l6]aneN4)Cl2]C104. ............ 85 Aquation of cis-[Co(MAC)Cl?]+ Complexes. ...............................................85 Case I. Aquation of cis-[Co([12]aneNa)C 12]+ ........................................... 85 Case n. Aquation of cis-[Co( [!3]aneNa) Cl2]+ .........................................90 Case m . Isomerization of cis-[Co([l3]aneN/i)Cl2]Cl to trans- [Co( [13]aneN4)Cl2]Cl in M ethanol. ............................ 92 Discussion of the Kinetic Behavior of trans-[Co(MAC)Cl23+. ............. 92 The Kinetic Behavior of cis-[Co(MAC)Cl2]+ Complexes............1 0 3 IV. Sum m ary....... .............................................................................................. 1 0 7 V. Bibliography^ ................ .109 Stereorestrictive Chelation-Metal Complexes of Sparteine and N,Nt-Dimethyl- bispidine. I. Introduction ...................................................................................................................114 H. Experimental ............................................................................................................118 Materials .................................................................................................118 Physical Measurements ......................... 118 Syntheses ..................................................................... 119 K inetics ..................................................................................................................... 426 v TABLE OF CONTENTS Page No. HI. Results and Discussion. ............................ .............. 127 Strain Energy Calculations ............................................... 128 Syntheses and Characterizations. ........................................... 131 Case I. Co(L)X2 C om plexes................................... 131 Case H. Ni(L)X2 Complexes ........................................... 142 Case HI. Cu(L)X2 Complexes .................................... .155 Case IV. Pd(L)X2 Complexes .......................... 164 Case V. [Co(Me4N[i4]aneN4)Cl]C104. ................................ 171 Comparison of Metal-Chloride and Metal-Nitrogen Stretching M odes. ..................................................................................................................171 Kinetic Studies ............................................................................................................... 173 IV. Summary. ........... J.77 V. Bibliography .............................................................................................. 178 LIST OF TABLES P a rt I Table Page No. 1. Ligand Field Parameters for trans-Diacidotetraamine Complexes of [Co([l3-l6]aneN4)Cl2]+ and [Ni([14-16^6^Cl2]. 3 2 . Ideal Metal-Nitrogen Bond Lengths and Planarity of the Macrocyclic Ligands. 3 3. Minimized Strain Energies for the Free Macrocycles. 4 4. Activation Parameters and Steric Courses of the Aquation of Co(L)ACln+. 8 5. Rate Constants and Steric Courses of Aquation of Dichlorotetraaminecobalt(III) Complexes. 9 6. Rates for Base Hydrolysis of [Co(AA)2LCl]n . 20 7. Wavelengths Where the Aquation Was Followed. 32 8. Selected Infrared Spectral Bands for trans-[Co(MAC)C 12]+X. 37 9. Infrared Spectral Bands for_trans- [Co(MAC)C12].Com plexes in CH2-Rocking and Metal-Nitrogen Stretching Regions.
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