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Reactions of Sulfur-Dicyanide and Sulfur-Dichlorides with Transition Metal Complexes." (1974)

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Reactions of Sulfur-Dicyanide and Sulfur-Dichlorides with Transition Metal Complexes. Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1974 Reactions of Sulfur-Dicyanide and Sulfur- Dichlorides With Transition Metal Complexes. Diane Singleton Hamilton Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Hamilton, Diane Singleton, "Reactions of Sulfur-Dicyanide and Sulfur-Dichlorides With Transition Metal Complexes." (1974). LSU Historical Dissertations and Theses. 2730. https://digitalcommons.lsu.edu/gradschool_disstheses/2730 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 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 Zeob Road Ann Arbor, Michigan 4a 105 h'V-\ I i 1 75-14,253 ?, HAMILTON, Diane Singleton, 1947- F REACTIONS OF SULFUR DICYANIDE AND SULFUR : DICHLORIDES WITH TRANSITION METAL COMPLEXES. !. The Louisiana State University and Agricultural and Mechanical College, Ph.D., 1974 Chemistry, Inorganic Xerox University MicrofilmsAnn , Arbor, Michigan 48106 THIS DISSERTATION HAS BEEN MICROFILMED EXACTLY AS RECEIVED. REACTIONS OF SULFUR DICYANIDE AND SULFUR DICHLORIDES WITH TRANSITION METAL COMPLEXES 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 Diane Singleton Hamilton A.A.t Southwest Mississippi Junior College, I967 B.S., Louisiana State University, I97O December, 197^ To Ernie ACKNOWLEDGEMENT The author is deeply grateful to Dr. William H. Baddley for his guidance and encouragement throughout this work. A special thanks is due to my fellow-workers, Mr. William Pitts, Mr. George Tupper, and Mr. pranab Choudhury for their meaningful assistance and suggestions in the laboratory, to Mr. Ralph Seab for his performance of most of the elemental analyses reported herein, to Mr. George Sexton for his maintenance of the instruments used in the re­ search, to Mrs. Lynn DeSille for her efficient typing of the manuscript, and to Dr. Duane Wolcott for his skillful drawing of the figures and structures. The author gratefully acknowledges the Dr. Charles E. Coates Memorial Fund of the Louisiana State University Foundation donated by George H. Coates, for expenses incurred in the preparation of this Dissertation. For financial assistance from the Department of Chemistry, Louisiana State University-Baton Rouge, in the form of Teaching and Research Asslstantshlps I am particularly grateful. Finally, I want to thank my parents, Frank and Marguerite Singleton, and my husband, Ernie, for their encouragement and moral support which were essential to my attaining this goal. iii TABLE OF CONTENTS PAGE ACKNOWLEDGMENT............................................. 111 LIST OF TABLES.............................................. vii LIST OF FIGURES..................................... viii LIST OF ABBREVIATIONS....................................... ABSTRACT.................................................... x I. INTRODUCTION......................................... 1 A. Preliminary Remarks............................... I B. Review of Metal Complexes Containing SR and SR2 Ligands.................................. 3 C. Statement of the Problem......................... 7 D. Chemistry of Sulfur Dicyanide, Sulfur Dichlorlde, and Dlsulfur Dichloride................ 8 II. EXPERIMENTAL - GENERAL................................ 20 A. Materials................ 20 B. Instrumentation......... 21 C. General Preparative and Purification Techniques.... 22 III. EXPERIMENTAL - SULFUR DICYANIDE REACTIONS.... 2k A. Reactions of trans-IrX(CO)Le [L = PPh3 , X * Cl, Br, C(CN)3 , NCS; L - FMePh2, AsPh3 , X “ Cl] with s(CN)2........ 2k 1. Preparation and Characterization of the Linkage Isomers IrCl(CN)(SCN)(C0)(PPh3 )2 and IrCl(CN)(NCs)(C0)(PPh3 )2................ 2k 2. Preparation and Characterization of the Linkage Isomers IrCl(CN)(SCN) (C0)(PMePh2) 2 and IrCl(CN) (NCS) (CO) (PMePh2) 2................ 25 3. Preparation and Characterization of the Linkage Isomers irBr(CN)(SCN) (CO)(PPh3 )2 and IrBr (CN)(NCS)(CO) (PPh3 ) 2.................. 26 4. Preparation and Characterization of Ir[C(CN)3](CN)(sCN)(C0)(PPh3)2................ 27 5. Preparation and Characterization of the Linkage Isomers Ir(NCS)(CN)(SCN)(C0)(PPh3)2 and Ir(NCS)2(CN)(CO)(PPh3)2................... 27 iv PAGE 6. Preparation and Characterization of the Linkage Isomers IrCl(CN)(SCN)(CO)(AsPh3)2 and IrCi(CN)(NCS)(CO)(AsPh3 )2............... 28 B. Reaction of IrH(CO)(PPh3 )3 and s(CN)2 ..... ........ 29 C. Reaction of IrH(CO)2 (PPh3 )2 and s(CN)2 ............. 30 D. Reaction of trans-IrClN2 (PPh3 )2 and s(CN)2 ......... 31 E. Reaction of tran£-RhX(CO)(PPh3)2 (X s Cl, Br) and S(CN)2 .......... ............................... 32 1. Preparation and Characterization of the Linkage Isomers RhCl(CN)(SCN)(CO)(PPh3 )2 and RhCl(CN) (NCS) (CO) (PPh3)2.................. 32 2. Preparation and Characterization of RhBr(CN) (SCN) (CO) (PPh3 )2 ....................... 32 F. Reaction of BhCi(PPh3 )3 and s(CN)2 ................. 33 G. Reaction of Pt(pph3)4 and S(CN)2.................. 34 H. Reaction of Pt(Co)2 (PPh3 )2 and S(CN)2 .............. 34 I. Attempted Reaction of AuCl(pph3) and S(CN)2........ 35 IV. RESULTS OF SULFUR DICYANIDE REACTIONS................. 37 V. DISCUSSION OF SULFUR DICYANIDE REACTIONS.............. 41 A. Iridium Chemistry................................. 41 B. Rhodium Chemistry................................. 70 C. Platinum Chemistry................................ jh D. Gold Chemistry.................................... 82 VI. EXPERIMENTAL - SULFUR DICHLORIDE AND DISULFUR DICHLORIDE REACTIONS.................................. 83 A. Reactions of trans-IrX(CO)(PPh3)2 (X = Cl, Br, NCS) with SC12................................ 83 1. Preparation and Characterization of IrCl2(sCl)(CO)(PPh3 )2 ......... 83 2. Preparation and Characterization of IrBrCl (SCI) (CO) ( PPh3 ) ........................ 84 3 . Preparation and Characterization of Ir(NCS)Cl(SCl)(CO) (PPh3) 2..................... 84 B. Reaction of [lr(diphos)2]Cl and SC12.... ......... 85 C. Reaction of _trans-RhCl(CO) (PPh3 )2 and SC12 ......... 86 v PAGE D. Reaction of Pt(pph3 ) 4 and SC12 ............ 86 E. Reaction of Pt(C0)2(PPh3)2 and SC12.............. 87 F. Reactions of trans-IrX(CO)(PPh3) 2 (X = Cl, Br, NCS) with S^Ci^ and S2Br2 ......... .......... 88 1. Preparation and Characterization of lrCl(CO)(PPh3 )2*SsCls........................ 88 2. Reaction of IrCl(CO)(PPh3 )2 with S2Br2....... 89 3 . Preparation and Characterization of IrBr(CO) (PPh3 )2 'S2Cl2........................ 90 4. Preparation and Characterization of Ir(NCS)(CO)(PPh3 )2*S2Cl2.................... 91 G. Reaction of [lr(diphos)2]Cl and S2C12.......... 91 H. Reaction of RhCl(CO) (PPh3 )2 and S^ l e ............. 92 I. Reaction of Pt(PPh3 ) 4 and S2C12............ 1..... 9? J. Reaction of Pt(C0)2(PPh3 )2 and S2C12....... 93 VII. RESULTS OF SULFUR DICHLORIDE AND DISULFUR DICHLORIDE REACTIONS....... 95 VIII. DISCUSSION OF SULFUR DICHLORIDE AND DISULFUR DICHLORIDE REACTIONS.................................. 98 A. General Reactivity of Sulfur Halides.............. 98 B. Sulfur Dlchlorlde,Reactions... .•.............. 99 1. Iridium Chemistry............................. 99 2. Rhodium
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