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INORGANIC SYNTHESES Volume XX Board of Directors FRED BASOLO Northwestern University WILLIAM L. JOLLY University of Colifornia HENRY F. HOLTZCLAW University o f Nebraska JAY H. WORRELL University of South Flori& BODIE E. DOUGLAS University of Pittsburgh DUWARD F. SHRIVER Northwestern University Future Volumes XXI JOHN P. FACKLER, JR. Case Western Reserve University XXll SMITH L. HOLT University of Georgia XXIll STANLEY KIRSCHNER Wayne State University International Associates E. 0. FISCHER Technische Universitat Munich JACK LEWIS Combridge University LAMBERTO MALATESTA University of Milan F. G. A. STONE University of Bristol GEOFFREY WILKlNSON Imperial College of Science and Technology London AKIO YAMAMOTO Tokyo Institute of Technology Yokohama MARTIN A. BENNETT Austrolian Notional University Editor-in-Chief DARYLE H. BUSCH ....... ................... Department of Chemistry The Ohio State University INORGANIC SYNTHESES Volume XX A Wiley-Interscience Publication JOHN WILEY & SONS New York Chichester Brisbcrne Toronto Published by John Wiley & Sons, Inc. Copyright 0 1980 Inorganic Syntheses, Inc. All rights reserved. Published simultaneously in Canada. Reproduction or translation of any part of this work beyond that permitted by Sections 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 Catalog Number: 39-23015 ISBN 0-4 71- 0 7715-1 Printed in the United States of America 10 9 8 7 6 5 4 3 2 1 To Paolo Chini 1928-1980 PREFACE Continuing the function of Inorganic Syntheses, this volume contains 57 numbered sections including almost 150 individual preparations, among which are some important intermediates, covering a number of broad, currently active areas of inorganic chemistry. These areas are divided into seven chapters. First, a series of offerings, featuring the double infusion technique and crystal growth in gels, treat solid materials and techniques of crystal growth. A variety of interesting and useful stoichiometrically simple compounds are presented in Chapter 2. They include such main group element derivatives as TeF, and SeO, Fz , and a number of transition element derivatives (e.g., trirhenium nonahalides) the important metal chromium (111) oxides (chromites), a neat preparation for copper(1) acetate, and the simplest method yet for anhydrous PtC1, (the third for this compound in Inorganic Syntheses). Chapter 3 contains an array of classic coordination compounds (ethylenediamine complexes of rhodium, P-diketonates of platinum(II)), and also some materials that have been of interest only in the more recent past (phosphine complexes of iron, a C 0 2 adduct, phosphite complexes of several metal ions). Syntheses are given for a number of rather exotic ligand complexes in Chapter 4. These include the clathrochelates of Coedken, the sepulchrates of Sargeson, the superphthalocyanine of Marks, and examples of compartmental ligands. A lengthy section is devoted to compounds of biological interest. Emphasis ranges from metal intercalation reagents, over synthetic macrocycles, corrin complexes and analogues, and porphyrins (including the 0, adduct of Collman’s picket-fence porphyrin) to complexes of dinitrogen. David Dolphin contributed a large group of syntheses on the complexes of the natural macrocycles and their close relatives. Organometallic compounds are soundly represented in Chapters 6 and 7. Chapter 6 contains a number of representative element organometallic compounds (hexamethyldisilaselenane, digermatellurane, digermoxane) and varieties of transition metal derivatives (e.g., halocyclopen