INORGANIC SYNTHESES Volume 23 Board of Directors
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INORGANIC SYNTHESES Volume 23 Board of Directors DUWARD F. SHRIVER Norrhwesrern University HENRY F. HOLZCLAW, JR. University of Nebraska BODIE E. DOUGLAS University of Pirrsburgh JAY H. WORRELL University of Sourh Florida JOHN P. FACKLER, JR. Texas A&M University SMITH L. HOLT, JR. Oklahoma State University Future Volumes 24 JEAN’NE SHREEVE University of Idaho 25 HERBERT D. KAESZ University of California, Los Angeles 26 HARRY R. ALLCOCK Pennsylvania State University 27 STEVEN D. ITTEL E. I. du Ponr de Nemours and Co. 28 ALVIN P. GINSBERG Bell Laboratories 29 ROBERT J. ANGELIC1 Iowa Srare University International Associates MARTIN A. BENNETT Australian National University FAUSTO CALDEWO University of Pisa E. 0. FISCHER Technische Universirar Miinchen SACK LEWIS Cambridge University LAMBERTO MALATESTA University of Milan RENE POILBLANC University of Toulouse HERBERT ROESKY University of Goningen F. G. A. STONE University of Brisrol GEOFFREY WILKINSON Imperial College of Science and Technology AKIO YAMAMOTO Tokyo Kogyo Daigaku (TokyoInstirure of Technology) Editor-in-Chief STANLEY KIRSCHNER Deportment of Chemistry Wayne State Universily Detroit, Michigan INORGANIC SYNTHESES Volume 23 A Wiley-Interscience Publication JOHN WILEY tk SONS New York Chichester Briskne Toronto Singapore Published by John Wiley & Sons, Inc. Copyright 0 1985 by Inorganic Syntheses, Inc. All rights reserved. Published simultaneously in Canada. Reproduction or translation of any part of this work beyond that permitted by Section 107 or 108 of the 1976 United States Copyright Act without the permission of the copyright owner is unlawful. Requests for permission or further information should be addressed to the Permissions Department, John Wiley & Sons, Inc. Library of Congress Caralog Number: 39-23015 ISBN 0-471-81873-9 Printed in the United States of America 10 9 8 7 6 5 4 3 2 I HARRYR. ALLCOCKPennsylvania State University ROBERTJ. ANGELICIIowa State University JOHN C. BAILAR,JR. University of Illinois-Champaign-Urbana NEILBARTLETT University of California-Berkeley FREDBASOLO Northwestern University DARYLEH. BUSCHOhio State University GEORGEH. CADYUniversity of Washington F. A. COTTONTexas A&M University ALAN COWLEYUniversity of Texas MARCETTADARENSBOURG Texas A&M University BODIEE. DOUGLASUniversity of Pittsburgh JOHNP. FACKLER,JR. Texas A&M University W. CONARDFERNELIUS Kent State University ALVINP. GINSBERGBell Laboratories RUSSELLN. GRIMESUniversity of Virginia JACKHALPERN University of Chicago M. FREDERICKHAWTHORNE University of California-Los Angeles SMITH L. HOLT,JR. Oklahoma State University HENRYF. HOLTZCLAW,JR. University of Nebraska-Lincoln LEONARDV. INTERRANTEGeneral Electric Company STEVEND. ITTEL E. I. du Pont de Nemours and Co., Inc. WILLIAML. JOLLYUniversity of California-Berkeley HERBERTD. KAESZ University of California-Los Angeles J. J. KATZ Argonne National Laboratories STANLEYIRSCHNER Wayne State University JACOBKLEINBERG University of Kansas ALANG. MACDIARMIDUniversity of Pennsylvania THERALDMOELLER Arizona State University DONALDMURPHY Bell Laboratories ROBERTW. PARRYUniversity of Utah V vi Members GEORGEW. PARSHALLE. I. du Pont de Nemours and Co., Inc. EUGENEG. ROCHOWHarvard University JOHN K. RUFFUniversity of Georgia JEAN’NE SHREEVEUniversity of Idaho DUWARDF. SHRIVERNorthwestern University THOMASE. SLOANChemical Abstracts Service S. Y. TYREE,JR. College of William and Mary CHARLESH. VAN DYKECarnegie-Mellon University AARONWOLD Brown University JAY H. WORRELLUniversity of South Florida This volume is dedicated to the memory of EARL L. MUETTERTIES ( 1927- 1984) He was a chemist’s chemist and a friend to inorganic Syntheses PREFACE I welcome this opportunity to contribute to Inorganic Synrheses by editing this volume, because this series has been of considerable help to me and my col- leagues for more than thirty years. It is appropriate, I believe, to express my appreciation and the appreciation of Inorganic Syntheses to all those who were involved in producing this volume. Special thanks must go to the contributors and checkers, who provided and checked the substantive material of the volume. However, additional thanks must go to the members of Inorganic Syntheses who contributed their time and expertise to help with the editing, because, without this assistance, this volume would not be nearly so complete as it is. I would like especially to thank John Bailar, Therald Moeller, and Thomas Sloan, who were particularly helpful during the editing process. Further, I would also like to express my appreciation to Duward Shriver, for his help in providing guidance and for his editorial assistance, as well. I must extend my sincere appreciation to my secretary, Elena Drob, whose patience and efforts beyond the call of duty helped to make this volume possible. 1 wish to call special attention to the Special Hazard Notice Appendix at the back of this volume. Finally, I wish to mention the dedication of this volume to Earl Muetterties, whose untimely passing has saddened us all. He was the Editor of Volume 10 of this series and continued to contribute to the success of later volumes. STANLEYKIRSCHNER Derroir. Michigan December 1984 ~ Revious volumes of Inorganic Synrhescs are available. Volumes I-XVI can be ordered from R. E. Krieger Publishing Co., Inc., P.O.Box 9542, Melbourne, Florida 32901; Volume XVII is available from McGraw-Hill, Inc.; ind Volumes XVIII-XXII can be obtained from John Wiley & Sons, Inc. ix NOTICE TO CONTRIBUTORS AND CHECKERS The Inorganic Syntheses series is published to provide all users of inorganic substances with detailed and foolproof procedures for the preparation of important and timely compounds. Thus, the series is the concern of the entire scientific community. The Editorial Board hopes that all chemists will share in the re- sponsibility of producing Inorganic Syntheses by offering their advice and as- sistance in both the formulation of and the laboratory evaluation of outstanding syntheses. Help of this kind will be invaluable in achieving excellence and pertinence to current scientific interests. There is no rigid definition of what constitutes a suitable synthesis. The major criterion by which syntheses are judged is the potential value to the scientific community. An ideal synthesis is one that presents a new or revised experimental procedure applicable to a variety of related compounds, at least one of which is critically important in current research. However, syntheses of individual com- pounds that are of interest or importance are also acceptable. Syntheses of compounds that are readily available commercially at reasonable prices are not acceptable. Corrections and improvements of syntheses already appearing in Inorganic Syntheses are suitable for inclusion. The Editorial Board lists the following criteria of content for submitted man- uscripts. Style should conform with that of pvious volumes of Inorganic Syntheses. The introductory section should include a concise and critical summary of the available procedures for synthesis of the product in question. It should also include an estimate of the time required for the synthesis, an indication of the importance and utility of the product, and an admonition if any potential hazards are associated with the procedure. The Procedure should present detailed and unambiguous laboratory directions and be written so that it anticipates possible mistakes and misunderstandings on the part of the person who attempts to du- plicate the procedure. Any unusual equipment or procedure should be clearly described. Line drawings should be included when they can be helpful. All safety measures should be stated clearly. Sources of unusual starting materials must be given, and, if possible, minimal standards of purity of reagents and solvents should be stated. The scale should be reasonable for normal laboratory operation, and any problems involved in scaling the procedure either up or down should be discussed. The criteria for judging the purity of the final product should be xi xii Notice to Contributors and Checkers delineated clearly. The section on Properties should supply and discuss those physical and chemical characteristics that are relevant to judging the purity of the product and to permitting its handling and use in an intelligent manner. Under References, all pertinent literature citations should be listed in order. A style sheet is available from the Secretary of the Editorial Board. The Editorial Board determines whether submitted syntheses meet the general specifications outlined above. Every procedure will be checked in an independent laboratory, and publication is contingent upon satisfactory duplication of the syntheses. Each manuscript should be submitted in duplicate to the Secretary of the Editorial Board, Professor Jay H. Worrell, Department of Chemistry, University of South Florida, Tampa, FL 33620. The manuscript should be typewritten in English. Nomenclature should be consistent and should follow the recommen- dations presented in Nomenclature of Inorganic Chemistry, 2nd Ed., Butter- worths & Co., London, 1970 and in Pure Appl. Chem., 28, No. 1 (1971). Abbreviations should conform to those used in publications of the American Chemical Society, particularly Inorganic Chemisrry. Chemists willing to check syntheses should contact the editor of a future volume or make this information known to Professor Worrell. TOXIC SUBSTANCES AND LABORATORY HAZARDS Chemicals and chemistry are by their very nature hazardous. Chemical reactivity implies that