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SYNTHESES Volume XIV Editors AARON WOLD JOHN K INORGANIC SYNTHESES Volume XIV Editors AARON WOLD JOHN K. RUFF Professor of Engineering Associate Professor of Chemistry and Chemistry University of Georgia Brown University, Providence, R.I. Athens, Ca. INORGANIC SYNTHESES Volume XIV McCRAW-HILL BOOK COMPANY New York St. Louis San Francisco Diisseldorf Johannesburg Kualo Lumpur London Mexico Montreal New Delhi Panama Rio de Janeiro Singapore Sydney Toronto INORGANIC SYNTHESES, VOLUME XIV Copyright 0 1973 by McGraw-Hill, Inc. All Rights Rewved. Printed in the United States of America. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, recording, or otherwise. without the prior written permission of the publisher. Library of Congress Catalog Card Number 39-23015 07-07 1320-0 1234567890 KPKP 76543 To RONALD NYHOLM and DAVID WADSLEY CONTENTS Reface ........................................... xi Notice to Contributors ................................... xiii Chapter One PHOSPHORUS COMPOUNDS ............... 1 1 . Phosphine ....................................... 1 2 . tert-Butyldichlorophosphineand Di-tert-butylchlorophosphinc......... 4 A . tert-Butyldichlorophosphinc ......................... 5 B . Di-tert-butylchlorophosphinc ......................... 6 3. 1.2-Bis(phosphino)ethane ............................. 10 4 . Tctramcthyldiphosphineand Flexible Aliphatic (Dimethylphosphino) Ligands ........................... 14 A . TetramethyldiphosFhine............................. 15 B . 1,3.Bis(dimcthylphosphino)propanc ..................... 17 C. (l-Dimcthylphosphino)(3-dimcthylarsino)propane ............. 20 D . ( l-Dimethylphosphino)(3-dimcthylamino)propane ............. 21 5 . Amido(PhosphonitrilicChloride-Cyclic Trimcr) and 1 .l.Diamido(Phosphonitrilic Chloride-Cyclic Trimer) ............. 23 A . 1 .l.Diamido(Phosphonitrilic Chloride-Cyclic Trimcr) ........... 24 B . Amido(PhosphonitrilicChloride-Cyclic Trimer) ............... 25 Chapter Two NON-TRANSITION-METAL COMPOUNDS ..... 29 6. PcrchlorylFluoride ................................. 29 7 . Chlorodifluoroaminc and Difluorodiazene ..................... 34 A . Chlorodifluoroamine ............................... 35 B. Difluorodiazenc ................................. 36 8 . Dioxygenyl Salts ................................... 39 9 . Bis(trifluoromethy1) Sulfoxide ........................... 42 A . S-TrifluoromcthylTrifluoromonothioperoxyacctatc ............. 43 vii vii Contents B. Bis(trifluoromethy1) Sulfide ........................... 44 C. Bis(trifluoromethy1)sulfurDifluoride ..................... 45 D . Bisftrifluoromethyl) Sulfoxide ......................... 46 10 . Aluminum Trihydride-Diethyl Etherate ..................... 47 11. Trimethylammonium Tetraphenylborate ..................... 52 12 . Tetrakis(acetat0)di-p-amido-diborane ....................... 55 Chapter Three TRANSITION-METALCOMPLEXES ......... 57 13 . A General Nonaqueous Preparation of Cobalt(II1) and Nickel(I1) Diamine and Triamine Complexes ............................... 57 A . Cobalt Complexes ............................... 58 B. Nickel Complexes ............................... 61 14 . Dianionobis(ethylenediamine)cobalt(III) Complexes ............... 63 A . (Carbonato)bis(ethylenediamine)cobalt(III) Chloride and Bromide ... 64 B . trans-Dichlorobis(ethyienediamine)cobalt(III) Chloride ........... 68 C. cis-Dichlorobis(ethylenediamine)cobalt(III)Chloride ........... 70 D . cis-Aquachlorobis(ethylenediamine)cobalt(III)Sulfate ........... 71 E . cis-Bis(ethylenediamine)dinitrocobalt(III) Nitrite ............. 72 F . cis-Aquabis(ethylenediamine)hydroxocobalt(III) Dithionate ........ 74 G . cis-Diaquabis(ethylenediamine)cobalt(III) Bromide ............. 75 15 . Bis(ethy1enediamine)sulfito Complexes of Cobalt(II1) ............. 77 A . Disodium cis-Bis(ethylenediamine)disulfitocobalt(III) Nitrate and Perchlorate ................................... 77 B. cis-Azidobis(ethylenediamine)sulfitocobalt(III) ............... 78 C. Sodium truns-Bis(ethylenediamine)disulfitocobaltate(III) ......... 79 16. Nitrosyliron. -cobalt and -nickel Iodides ..................... 81 A . Iron Dinitrosyl Iodide ............................. 82 B. Cobalt Dinitrosyl Iodide ............................. 86 C. Nickel Nitrosyl Iodide ............................. 88 17 . Potassium Trichloro(ethylene)platinate(II) ..................... 90 18. Chlorobis(cyclooctene)rhodium(I) and -iridium(I) Complexes ......... 92 A . Chlorobis(cyclooctene)rhodium(I) ....................... 93 B. Di-p-chlorobis[bis(cyclooctene)iridium] ................... 94 19 . Cooper(1) Ammonium Tetrathiomolybdate(VI) ................. 95 Chaprer Four SOME SIGNIFICANT SOLIDS ............. 99 I . HALIDES AND OXYHALIDES ........................... 101 20 . Iron(I1) Halides ................................... 101 A . Iron(1I)Halides ................................. 102 B. Iron(I1) Iodide ................................. 104 21. Niobium(1V) Fluoride and Niobium(V) Fluoride .................. 105 A . Niobiurn(V) Fluoride ............................. 106 B . Niobium(1V) Fluoride ............................. 106 22 . Tungsten Oxyhalides ................................. 109 A . Tungsten(V1) Dichloride Dioxide ....................... 110 Contents ix B. Tungsten(V1) Tetrachloride Oxide ....................... 112 C . Tungsten(V) Trichloride Oxide ......................... 113 D. Tungsten(1V) Dichloride Oxide ........................ 115 E . Tungsten(V1) Dibromide Dioxide ....................... 116 F . Tungsten(VI) Tetrabromide Oxide ....................... 117 G . Tungsten(V) Tribromide Oxide ......................... 118 H. Tungsten(1V) Dibromide Oxide ......................... 120 1. Tungsten(V1) Diiodide Dioxide ...... ............... 121 23 . Indium(II1) Oxyfluoride ............................... 123 24 . Strontium Chloride Phosphate and Vanadate(V) ................. 126 A . Pentastrontium Chloride Tris(phosphate) ................... 127 B. Doped Strontium Chloride Phosphates ................... 128 C. Strontium Chloride Vanadate(V) ....................... 129 I1 . OXIDES ....................................... 131 25 . Niobium Monoxide ................................. 131 26 . Magnesium Chromite ................................. 134 A . Dichromium Tungsten(VI) Oxide. Cr, WO, ................. 135 B . Magnesium Chromium(II1) Oxide. MgCr, 0, ................. 136 27 . Silver Ferrate(II1) ................................... 139 28 . Barium Titanate. BaTiO, ............................... 142 29 . Bismuth Titanate. Bi,Ti30,, ........................... 144 30 . Cadmium Rhenium(V) Oxide. Cd, Re, 0, ..................... 146 31. Molybdenum(1V) Oxide and Tungsten(IV) Oxide Single Crystals ....... 149 m . CHALCoCENIDES ................................. 152 32. Rare-Earth Sesquisulfides. Ln, S, ......................... 152 33 . Cadmium Chromium(II1) Selenide. CdCr, Se, ................... 155 34 . Growth of Cobalt Disulfide Single Crystals .................... 157 35 . Chalcogenide Halides of Copper. Gold. Mercury. Antimony. and Bismuth ... 160 A . Antimony(II1) Iodide Sulfide ......................... 161 B. Copper Chalcogenide Halides ......................... 170 C . Cold Halide Tellurides ............................. 170 D. Mercury(I1) Halide Sulfide ........................... 171 E . Lead@) Chalcogenide Halides ......................... 171 F . Antimony and Bismuth Halide Sulfides ................... 172 N . PHOSPHIDES AND SILICIDES ......................... 173 36 . Pyrite Type of Silicon Diphosphide ......................... 173 37 . Single Crystals of Iron Monophosphide ....................... 176 38 . Copper-Solvent Flux Growth of Manganese Monosilicide ........... 182 V . Hydrides ....................................... 184 39 . Single-Crystal Cerium Hydrides ........................... 184 Index of Contributors ................................... 195 SubjectIndex ........................................ 199 FormulaIndex ....................................... 223 PREFACE This volume of INORGANICSYNTHESES has a large section (Chapter Four) devoted to solid-state syntheses. Many of the previous volumes have contained solid-state preparations, and it is our hope that this volume will encourage chemists working in this area to contribute manuscripts suitable for the series. An important aspect of Chapter Four is the inclusion of several syntheses which deal with the preparation and characterization of single crystals. The preparation of well-characterized single crys- tals, suitable for physical measurements, is essential if the results of such measurements are to be of interest either from an industrial or academic point of view. In addition to chemical analyses and spectral data, other physical measurements may be used to identify the nature of the products formed from solid-state reactions. These include microscopic identification, x-ray analyses, density determination, and magnetic, electrical, and optical measurements. These are chosen in sufficient combina- tion to provide ample evidence that the product is single-phase, stoichiometric, and homogeneous. The arrangement of the syntheses in the first part of Volume XIV is divided into three chapters, namely, Phosphorus Com- pounds, Non-Transition-Metal Compounds, and Transition-Metal Compounds. The reader is advised to seek particular compounds in the subject or formula indexes. The indexes at the end of this volume are cumulative from Volume XI through
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