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Inorganic Syntheses, Volume 33 Inorganic Syntheses, Volume 33. Edited by Dimitri Coucouvanis Copyright # 2002 John Wiley & Sons, Inc. ISBNs: 0-471-20825-6 (Hardback); 0-471-22450-2 (Electronic) INORGANIC SYNTHESES Volume 33 Board of Directors BODIE E. DOUGLAS University of Pittsburgh HERBERT D. KAESZ University of California, Los Angeles DARYLE H. BUSCH University of Kansas JAY H. WORRELL University of South Florida RUSSELL N. GRIMES University of Virginia ROBERT J. ANGELICI Iowa State University DONALD W. MURPHY AT&T Bell Laboratories LEONARD V. INTERRANTE Rensselaer Polytechnic Institute ALAN H. COWLEY University of Texas, Austin Future Volumes 34 JOHN R. SHAPLEY University of Illinois, Urbana 35 ALFRED SATTELBERGER Los Alamos National Lab 36 TOM RAUCHFUSS University of Illinois 37 TOBIN MARKS Northwestern University 38 LOU PIGNOLET University of Minnesota International Associates MARTIN A. BENNETT Australian National University, Canberra FAUSTO CALDERAZZO University of Pisa E. O. FISCHER Technical University, Munich M. L. H. GREEN Oxford University JACK LEWIS Cambridge University LAMBERTO MALATESTA University of Milan RENE POILBLANC University of Toulouse HERBERT W. ROESKY University of Go¨ttingen WARREN R. ROPER University of Auckland F. G. A. STONE Baylor University JAN REEDIJK Leiden University H. VAHRENKAMP University of Freiburg AKIO YAMAMOTO Tokyo Institute of Technology Editor-in-Chief DIMITRI COUCOUVANIS University of Michigan INORGANIC SYNTHESES Volume 33 A Wiley-Interscience Publication JOHN WILEY & SONS, INC. Designations used by companies to distinguish their products are often claimed as trademarks. In all instances where John Wiley & Sons, Inc., is aware of a claim, the product names appear in initial capital or ALL CAPITAL LETTERS. Readers, however, should contact the appropriate companies for more complete information regarding trademarks and registration. Copyright # 2002 by John Wiley & Sons, Inc., New York. All rights reserved. No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic or mechanical, including uploading, downloading, printing, decompiling, recording or otherwise, except as permitted under Sections 107 or 108 of the 1976 United States Copyright Act, without the prior written permission of the Publisher. Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 605 Third Avenue, New York, NY 10158-0012, (212) 850-6011, fax (212) 850-6008, E-Mail: PERMREQ @ WILEY.COM. This publication is designed to provide accurate and authoritative information in regard to the subject matter covered. It is sold with the understanding that the publisher is not engaged in rendering professional services. If professional advice or other expert assistance is required, the services of a competent professional person should be sought. ISBN 0-471-22450-2 This title is also available in print as ISBN 0-471-20825-6. For more information about Wiley products, visit our web site at www.Wiley.com. PREFACE Advances in Inorganic Chemistry over the last two decades reflect the new direc- tions our discipline is following. The present volume of Inorganic Syntheses attempts to place some emphasis in these directions. Many of the new areas of interest, are characterized by complexity in design and molecules containing specific functional groups. These characteristics, inspired by either metalloenzymology or the need for materials with specific properties and function, appear to be essential features of synthetic ‘‘supramole- cules’’ or clusters. Supramolecular syntheses have not been emphasized in an Inorganic Synth- eses volume in the past, however, as interest in this area increases, the need becomes apparent for synthetic methodology, and real examples of supramolecu- lar assemblies. There are various reasons why supramolecular methodology and specific syntheses of supramolecules were not emphasized previously in an Inor- ganic Syntheses volume. Included among these are: the inherent difficulty in the synthesis of multi-unit assemblies, the possible lack of general interest for spe- cific supramolecules and lack of a clear demonstration of utility and function for many of these molecules. In the first chapter of this volume are included procedures and methodology for the synthesis of molecules that may serve as magnetic building blocks, light gathe- ring units and ditopic activators or receptors. We expect this chapter of Volume 33 to inspire similar syntheses of new materials using similar methodologies. In the synthesis of new coordination compounds, whether classic or supramo- lecular, reagents that serve as convenient sources of metal ions or metal contain- ing groups are of the utmost importance. In Chapters 2 and 4 are included a number of molecules useful as reagents or building blocks. Low temperature solid state synthesis is an approach that shows great promise for the synthesis of materials with unusual interesting properties. Solid state synthesis has been the subject of Volume 30 of Inorganic Syntheses in the past. Continuing interes in solid state materials and particularly those obtained by relatively low temperature procedures has prompted us to include another ser- ies of such procedures and syntheses in Chapter 3 of this volume. I would like to thank those who submitted the syntheses for Volume 33 and also the checkers who often dedicated excessive time and great efforts in check- ing complicated procedures. To the few contributors that will not see their synth- eses in this volume, I apologize for not being able to find a person willing or able to check their syntheses. v vi Preface In the prescreening of manuscripts, the members of the Inorganic Syntheses board were very helpful in evaluating the contributions, making suggestions and proposing possible reviewers. Finally, the extensive, detailed, editorial screening of nearly every one of the manuscripts, by Duward Shriver, is appreciated and gratefully acknowledged. Dimitri Coucouvanis Ann Arbor, Michigan 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 impor- tant 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 respon- sibility of producing Inorganic Syntheses by offering their advice and assistance in both the formulation 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 com- pounds 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 manu- scripts. Style should conform with that of previous volumes of Inorganic Synth- eses. The introductory section should incude 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 section should present detailed and unambiguous laboratory directions and be written so that it anticipates pos- sible mistakes and misunderstandings on the part of the person who attempts to duplicate 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 shold 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 deli- neated clearly. The Properties section should supply and discuss those physical and chemical characteristics that are relevant to judging the purity of the product vii viii Notice to Contributors and Checkers and to permitting its handling and use in an intelligent manner. Under Refer- ences, 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 sumitted syntheses meet the general specifications outlined above. Every procedure will be checked in an independent laboratory, and publication is contingent on satisfactory duplication of the synth- eses. Each manuscript should be submitted in duplicate to the Secretary of the Edi- torial Board Professor Stanton Ching, Department of Chemistry, Connecticut College, New London, CT 06320. The manuscript should be typewritten in Eng- lish. Nomenclature
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