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Information to Users INFORMATION TO USERS This manus&ipt has been reproduced from the microfilm master. UMI films the text directly from the original or copy submitted. Thus, some thesis and dissertation copies are in typewriter face, while others may be from any type of computer printer. The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality iilustrations and photographs, print bleedthrough, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send UMI a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. Oversize materials (e g., maps, drawings, charts) are reproduced by sectioning the original, beginning at the upper left-hand comer and continuing from left to right in equal sections with small overlaps. Photographs included in the original manuscript have been reproduced xerographically in this copy. Higher quality 6" x 9” black and white photographic prints are available for any photographs or illustrations appearing in this copy for an additional charge. Contact UMI directly to order. ProQuest Information and Learning 300 North Zeeb Road, Arm Arbor, Ml 48106-1346 USA 800-521-0600 UMÏ PARTI SYNTHESES AND CHARACTERIZATION OF HYDROGEN-BRIDGED LANTHANIDE(n)-BORON COMPLEXES PARTE SYNTHESES AND CHARACTERIZATION OF CYANIDE-BRIDGED LANTHANn)E(IH)-PALLADIUM COMPLEXES DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Soyoung Lim, B. S. ***** The Ohio State University 2001 Dissertation Committee: ! ApprovedApprovea ^ny Dr. Sheldon G. Shore, Advisor Dr. James A. Cowan _________ ^ l JFJAd^sor . Dr. Claudia Tutro Department of Chemistry UMI Number 3022525 UMI’ UMI Microform 3022525 Copyright 2001 by Bell & Howell Information and Learning Company. All rights reserved. This microform edition is protected against unauthorized copying under Title 17, United States Code. Bell & Howell Information and teaming Company 300 North Zeeb Road P.O. Box 1346 Ann Arbor, Ml 48106-1346 ABSTRACT Parti Hydrogen-bridged lanthanide(II)-boron complexes were synthesized and characterized. (CH3CN)%Ln[B3Hg]2 was prepared by the metathesis reaction between (NH3)xLnCl2, (Ln = Yb, Eu) and KP3H8] in liquid NH3 and subsequent displacement of NH3 with CH3CN. The preliminary structure of (CH3CN)4Yb[B3Hg]2, 1, is interesting since the two [B3Hg]' anions have different bonding modes. From NMR spectroscopic studies, the [B3Hg]* anion was determined to be fluxional even at 213 K. [Yb(CH3CN)g][Bi2Hi2], 2, and (CH3CN)6Yb[(p-H)2BnHu], 3, crystallized from the saturated CH3CN solution of (CH3CN)4Yb[B3Hg]2, 1. The oxidized species, [Eu(NH3)6(CH3CN)3][B3Hg]3, 7, was obtained from an CH3CN solution of (CH3CN)xEu[B3Hg]2,6. The organohydroborate derivatives, (THF)4Yb[(p-H)2BCgHi4]2. 8, and [(THF)4K]2[Eu{(p-H)2BCgHi4}4], 10, were synthesized by the metathesis reaction of (THF)xLnCl2, (Ln = Yb, Eu) with K[H2BCgHt4] in THF at room temperature. 2 and 7 are solvent-separated ion-pairs. 3 is the only structurally characterized metallaborane containing 11 boron atoms. For 3,8 and 10, the anions are coordinated to the Ln(ll) ions through three-center two-electron B-H-Ln bonds. Bridging hydride ion can be abstracted from the reaction of 8 with B(C6F$)3. For 10, unique agostic H-Eu and H-K interactions ii were observed. Crystal data for 2: monoclinic, Cc, a = 14.2260(10) A, 6 = 13.1350(10) A, c = 16.4780(10) A,/? = 90,000(30)®, Z = 4. Crystal data for 3: monoclinic, P 2i/c, a = 9.5097(10) A, 6 = 14.1574(10) A, c = 22.8192(10) A ,^ = 97.321(10)®, Z = 4. Crystal data for 7: hexagonal, P6^/m, a = b = 14.2797(10) A, c = 8.8740(10) k,a=fi = 90®, y = 120®, Z = 1. Crystal data for 8 : triclinic, PI, a = 9.8616(10) A, 6 = 10.2266(10) A, c = 10.4760(10) A, a = 69.873(10)®, p = 76.629(10)®, y = 66.116(10)®, Z = 2. Crystal data for 10: tetragonal, P 42/nmc, a = b = 13.4390(19) A, c = 20.421(4) A,a=p = y = 90®, Z = 4. Part II Cyanide-bridged lanthanide(III)-palladium complexes were prepared and characterized. The metathesis reaction between LnCb, (Ln = La, Gd) and K 2[Pd(CN) 4] with a 2 to 3 molar ratio in DMF at room temperature yielded two different types of one­ dimensional polymeric arrays: the double-strand Type B array, {(DMF)ioGd 2[Pd(CN) 4]3}-, 11, and the zigzag chain Type C array containing “diamond”-shaped metal cores, {(DMF)t 2La2[Pd(CN) 4]3}-, 12. Meanwhile, a zigzag single-strand array, {(DMF)sLn[Pd(CN) 4]Cl}-, (Ln = La, 13; Gd, 14) were synthesized by the metathesis reaction between LnCb and K 2[Pd(CN) 4] with a 1 to 1 molar ratio in DMF. Crystal data for 11; triclinic, P\,a = 9.2940(10) A, 6 = 11.1879(10) A, c = 16.4544(10) A, a = 81.462(10)“,^ = 76.945(10)®, y = 83.230(10)®, Z= 1. Crystal data for 12: triclinic, P\,a= 11.4762(10) A, 6 = 12.5675(10) A, c = 13.9467(10) A, a = 97.464(10)®, p = 109.508(10)®, y = 102.113(10)®, Z = l. Crystal data for 13: monoclinic, P2i/c, a = 7.5828(10) A, 6 = 22.1789(10) A,c = 17.8413(10) K P = 99.070(10)®, Z = 4. Crystal data for 14: monoclinic, PZi/n, a = 7.755(3) A, 6 = 17.810(7) A, c = 21.576(6) A, ^ = 92.72(3)®, Z = 4. iii Dedicated to my parents, my brother Cheho and my sister Jayoung IV ACKNOWLEDGMENTS I would like to sincerely thank Dr. Sheldon G. Shore for his guidance, enormous patience, encouragement, knowledge and support. I am deeply grateful to Dr. Shore’s group. To Drs. Shengming Liu, Jianping Liu, Edward A. Meyers and Bin Du for solving my crystal structures and teaching me crystallography. To Drs. Fu Chen Liu and Jianping Liu for helping me start research in the group. To Mr. Roman Kultyshev for helping me with various temperature NMR experiments. Especially to Ms. Christine E. Plenik for her careful prooAeading. I would like to express my special gratitude to all the group members for their help, encouragement and cherished friendship. I would like to extend sincere thanks to Dr. limit S. Ozkan and her group for letting me be introduced in the area of catalysis. I also need to thank Dr. Andrew Wojcicki and his group for guidance and help during my earlier graduate years. VITA November 6,1970 .......................Bom-Taegu, Korea 1993 ............................................B. S. Chemistry Education Kyungpook National University, Taegu, Korea 1994 -1999 ................................. Graduate Teaching Associate The Ohio State University 1999 - present .............................Graduate Research Associate The Ohio State University PUBLICATIONS 1. Sung-Ho Chun, Edward A. Meyers, Fu-Chen Liu, Soyoung Lim, Sheldon G. Shore. "Systematic syntheses of [Hg{M(CO) 4}2]^ [Hg{M(C 0 )4}]* (M = Fe, Ru, Os), and structures of [Hg{M(CO)4}2]^‘ (M = Ru, Os)" J. Organomet. Chem. 1998, 563,23. FIELDS OF STUDY Major Field: Chemistry VI TABLE OF CONTENTS Page Abstract...........................................................................................................................ii Dedication ......................................................................................................................iv Acknowledgments..........................................................................................................v Vita.................................................................................................................................vi List of Tables............................................................................................................... ix List of Figures................................................................................................................xi List of Schemes .............................................................................................................xv Chapters: Parti 1. Introduction....................................................................................................... l 1.1. The lanthanides ........................................................................................1 1.2. Divalent lanthanide chemistry ................................................................. 3 1.3. The lanthanide borides ........................................................................... 7 Statement of Problems.................................................................................. 15 2. Results and Discussion.....................................................................................17 2.1. (CH3CN)4Yb[B3H8]2,1 ..........................................................................17 2.2. [Yb(CH3CN)8][Bi2H,2].2 ..................................................................... 21 2.3. (CH3CN)6Yb[(p-H)2BiiHiil,3 ..............................................................30 2.4. (C5H5N)xYb[B3H8]2,4 .......................................................................... 39 2.5. (THF)xYb[B3H8]2,5 ............................................................................. .40 2.6. The formation of clusters..................................................................... .46 2.7. (CH3CN)xEu[B3H8 ]2 ,6 ........................................................................ .48 2.8. [E u(NH3)6(CH3CN)3][B3H8]3, 7 .............................................................49 2.9. (THF) 4Yb[(p-H) 2BC8Hu]2 ,8 ................................................................. 56 vu 2.10. Hydride ion abstraction reaction from (THF)4Yb[(ji-H)2BC8Hi4]2.8
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