Inorganic experiments / ed. by Woollins J.D. - 3rd rev. ed. - Weinheim: Wiley-VCH, 2010. - xxvi, 456 p.: ill. - ISBN 978-3-527-32472-9  Место хранения:   024 | Институт неорганической химии им. А.В.Николаева CO РАН | Новосибирск

Оглавление / Contents

1 Introduction ................................................. 1 1.1 Introduction ............................................ 3 J. Derek Woollins 1.2 General Spectroscopic Techniques and Report Writing ..... 5 Petr Kilian 2 Introductory Experiments .................................... 23 2.1 Preparation and Investigation of Some Coordination Compounds .............................................. 25 Manfred Bochmann 2.2 Gravimetric Analysis of Hexaamminenickel(ll) Tetrafluoroborate [Ni(NH3)6](BF4)2 ...................... 28 Manfred Bochmann 2.3 Analysis of an Iron(lll) Oxalate Complex ............... 33 Manfred Bochmann 2.4 Characterisation of a Copper Oxalate Complex KaCub (C2O4)c · dH2O .......................................... 38 Andrew W.G. Platt 2.5 Synthesis of [NH4][BF4] and Synthesis and Titrimetric Analysis of[Zn(NH3)4][BF4]2 ............................. 40 Michael A. Beckett 2.6 Iron(ll) and Lead(ll) Formates ......................... 43 Francisco J. Arnáiz, Maria R. Pedrosa, and Rafael Aguado 2.7 Ammonium Dichromate, Chromium(lll) Oxide, Potassium Chromate and Potassium Tetraperoxochromate(V) .......... 47 Antonin Ružička and Zdirad Žák 2.8 Vanadium Alum: An Experiment in Electrosynthesis ....... 51 David T. Richens 2.9 Linkage Isomerism: An Infra-Red Study .................. 54 David T. Richens and Christopher Clidewell 2.10 Preparation of Copper(l) Iodide ........................ 56 F.J. Arnáiz, M.R. Pedrosa, and S. Arnáiz 2.11 Deduction of the Coordination Mode of BH4 in Bis(triphenylphosphine) Copper(l) Borohydride (Ph3P)2CuBH4 ............................................ 58 Andrew W.G. Platt 2.12 Preparation and Identification of a Copper(l) Complex ................................................ 61 Andrew W.G. Platt 2.13 Synthesis and Characterisation of a Metal Hydride Complex ................................................ 63 Andrew W.G. Platt 2.14 Reactivity of Triphenylphosphine and Its Oxide Towards CuCl2 .......................................... 65 Paul F. Kelly and Martin B. Smith 2.15 Synthesis of a Thermochromic Copper Complex ............ 68 lain A. Smellie 2.16 Preparation and Complexation of Tris(3,5- imethylpyrazoyl)hydroborate ............................ 70 Manfred Bochmann 2.17 Tetraiodotin(IV) and its Triphenylphosphine Complex .... 73 lain A. Smellie and J. Derek Woollins 2.18 Silicon Oxygen Compounds and Siloxane Polymers ......... 75 Paul D. Lickiss 2.19 Preparation and N MR Identification of Two Phosphorus Esters ................................................. 79 Christopher Clidewell 2.20 Synthesis of Triphenylphosphine Oxide and Triphenylphosphine Sulfide ............................. 81 Iain Smellie 2.21 Preparation of Sodium Trithionate, Na2S3O6 and Potassium Trithionate, K2S3O6 ........................... 86 Andrew C. Platt 2.22 The Preparation of Potassium Peroxodisulfate, K2S2O8 .................................................. 89 Zdirad Žák and Antonin Ružička 2.23 Polyiodides, Me4NIX .................................... 92 Andrew W.G. Platt 2.24 Interhalogen Compounds ................................. 94 Ivan P. Parkin 2.25 Preparation of K[ICl4] ................................. 99 lain Smellie 2.26 Synthesis and Infrared Spectroscopic Characterisation of Boranes and Cermanes ............................... 101 Ivan P. Parkin 3 Intermediate Experiments 3.1 Metal Acetylacetonate Complexes: Preparation and Characterisation ...................................... 109 Christopher Glidewell 3.2 Nickel Dihalide Phosphine Complexes ................... 120 Ivan P. Parkin 3.3 Nickel(II) Complexes of Some Schiff Base Ligands ...... 124 Christopher J. Jones 3.4 The Synthesis and Coordination Chemistry of Macrocyclic Complexes ................................. 131 Martin Schröder 3.5 [Co(dinosar)]Cl3: An Encapsulation Complex Prepared by a Template Reaction ................................ 136 David J. Otway 3.6 Identification of Stereochemical (Geometrical) Isomers of [Mo(CO)4(L)2] by Infrared Spectroscopy ..... 139 Michael A. Beckett 3.7 Five Coordinate Complexes: [VO(acac)2] and [Cr(NH3)6][CuCl5] ...................................... 142 Christopher P. Morley 3.8 Preparation of trans-PtHCl(PPh3)2 and Measurement ofits 1H, 31P and 195Pt NMR Spectra ..................... 145 William P. Griffith 3.9 [MoO2Br2(H2O)2] · (diglyme) and [MoO2Br2(DMF)2] ......... 149 Francisco J. Arnáiz, Maria R. Pedrosa, and Rafael Aguado 3.10 Preparation of an Iron Dinitrogen Complex ............. 153 Andrew W.G. Platt 3.11 Preparation of Nitrosyl Complexes of Iron and Nickel ................................................ 155 Andrew W.G. Platt 3.12 Synthesis and Characterisation of Two Metal-Metal Bonded Dimolybdenum Complexes ......................... 158 William Levason, Thomas A. Logothetis, and Gill Reid 3.13 Cobalt Complexes of Dioxygen .......................... 167 David T. Richens and Christopher Glidewell 3.14 Ferrocene, (η5-C5H5)2Fe, and its Derivatives ........... 170 J. Derek Woollins 3.15 The Use of Organolithium Reagents in the Preparation of Ferrocene Derivatives .............................. 173 Ian R. Butler 3.16 Complexes of я-Bonding Arene Ligands .................. 180 Andrew W.G. Platt 3.17 Organotin Chemistry ................................... 183 Kieran С. Molloy and Timothy T. Paget 3.18 Transition Metal-Carbon Bonds in Chemistry and Biology ............................................... 190 Christopher J. Jones 3.19 Nickel-Catalysed Cross-Coupling of Alkylmagnesium with Haloarene ........................................ 201 С. Brent Young 3.20 Transition Metal Catalysis ............................ 205 Neil M. Boag 3.21 Nitration of Cobalt(lll) Acetylacetonate .............. 209 David J. Otway 3.22 Phenyllithium and Tetraphenylsilane ................... 211 Petr Kilian 3.23 Synthesis and Reactivity of Tertiary Phosphines ....... 218 Neil M. Boag 3.24 Two-stage Synthesis of Ph2P(O)(CH2)4P(O)Ph2 ............ 222 Andrew G. Platt 3.25 Inorganic Heterocycles: Cyclophosphazenes ............. 226 Josef Novosad and Milan Alberti 3.26 Inorganic (Carbon-Free) Chelate Rings: A Dithioimidodiphosphinato Ligand and Some of its Metal Complexes ....................................... 229 lonel Haiduc 3.27 Inorganic (Carbon-Free) Chelate Rings II: Asymmetric Mixed-Donor P-N-P Ligand and its Palladium Complex .... 234 David J. Birdsall and Josef Novosad 3.28 Amidosulfuric Acid, Trisilveramidosulfate Monohydrate and SO3 · N (CH3)3 Complexes .............. 239 Antonin Ružička and Zdirad Žák 3.29 Anomalous Paramagnetism in Some Iron(lll) Chelates Studied by the Evans NMR Method ....................... 243 David J. Otway 3.30 Cubic Molecular Aluminophosphonates ................... 246 Jiri Pinkas 3.31 Preparation and Optical Properties of Zinc Sulfide Quantum Dots .......................................... 249 Andrew L. Hector 3.32 Four Methods for Analysing First Order Kinetics ....... 255 Véronique Pimienta, Dominique Lavabre, Jean-Claude Micheau, and Gaston Levy 3.33 Molecular Orbital Calculations of Inorganic Compounds ............................................. 261 Carole A. Morrison, Neil Robertson, Andrew Turner, Jano van Hemert, and Jos Koetsier 4 Advanced Experiments 4.1 2,2':6',2" - Terpyridine Complexes and Metal Directed Reactivity ................................... 271 Edwin С. Constable 4.2 4'-(4-Pyridyl)-2,2':6',2 "-terpyridine: Coordination to Iron(ll) and Protonation Studies ................... 274 Catherine E. Housecroft, Edwin С. Constable, and Emma L. Dunphy 4.3 Heteronuclear d-f Complexes Containing Binucleating Ligands ............................................... 283 Francisco J. Arnáiz, Jean-Pierre Costes, and Javier Carcia-Tojal 4.4 Electronic Characterisation of a Transition Metal Complex Using Electrochemical UV/Vis and EPR Techniques ............................................ 287 Lesley J. Yellowlees 4.5 Chlorotris(tert-butylimido)manganese(VII) ............. 290 Andreas A. Danopoulos and Geoffrey Wilkinson 4.6 Tetrakisphosphorane Iminato Complexes of Transition Metals ................................................ 293 Kurt Dehnicke 4.7 Magnetochemistry Experiments: Exchange Coupling in Copper(II)-Nickel(II) Bimetallic Complexes and Spin Transition in Iron Complexes .......................... 297 Eugenio Coronado and J.J. Borrás-Almenar 4.8 Metal-Containing Liquid Crystals. The Synthesis of trans-bis(4-Alkyl-4'-cyano-1,1 -biphenyl) dichloroplatinum(ll) and Related Species - The Use of Melt Syntheses ..................................... 301 Duncan W. Bruce 4.9 Structural, Electrical and Magnetic Properties of Perovskite Ceramics ................................... 309 Colin Greaves 4.10 Polyoxomolybdate Clusters: Nanoscopic Wheels and Balls ................................................. 315 Leroy Cronin, Ekkehard Diemann, and Achim Müller 4.11 Reaction of Alkali Metal Polyselenides and Polytellurides with Croup 6 Metal Carbonyls ........... 322 Joseph W. Kolis 4.12 Chlorothionitrene and Cydothiazeno Complexes of Tungsten .............................................. 327 Kurt Dehnicke 4.13 Sulfur-Rich Homocycles and Heterocydes: Titanocene Pentasulfide, cyclo-Heptasulfur and 1,2,3,4,5,6,7- Heptathionane ......................................... 330 Jörg Albertsen and Ralf Steudel 4.14 N-Ferrocenyl Amine and Some Reactive Derivatives ...... 334 Max Herberhold, Heidi E. Maisel, and Bernd Wrackmeyer 4.15 l,l'-Bis(trimethylsilylamino)ferrocene - A Useful Precursor to l,n-Diaza-[n]ferrocenophanes ............. 341 Max Herberhold, Elena V. Klimkina, and Bernd Wrackmeyer 4.16 Organometallic Molybdenum Compounds ................... 353 Manfred Bochmann and Petr Klian 4.17 Migratory Insertion Reactions in Organo Transition- Metal Chemistry ....................................... 364 Mark J. Winter 4.18 A Transition-Metal Alkylidyne Complex ................. 369 Stephen Anderson, Darren Cook, and Anthony F. Hill 4.19 The Synthesis of η6-Arenetricarbonyl Chromium(0) Complexes ............................................. 372 David A. Widdowson 4.20 Preparation of the Iron Tricarbonyl Complex of Methyl-2-Acetamidoacrylate ............................ 375 M. Elena Lasterra-Sanchez and Susan E. Gibson 4.21 Halfsandwich Carbonyl Vanadium Complexes .............. 377 Max Herberhold and Matthias Schrepfermann 4.22 Covalent and Ionic Metallocene Hexafluoroarsenate Complexes ............................................. 383 Inis C. Tornieporth-Oetting and Thomas M. Klapötke 4.23 The Preparation of rac-Ethylene-1, 2-bis(1-indenyl)zirconium Dichloride and Dibenzyl Complexes ............................................. 386 Manfred Bochmann and Simon J. Lancaster 4.24 One-Pot Preparation of Ru3(CO)12 from RuCl3 · 3H20 .................... 391 Guy Lavigne, Catherine Saccavini, and Remi Chauvin 4.25 Synthesis of Well-defined Organometallic Hydroxides: [LCaOH]2, LAI(Me)OH and LCeOH ............. 396 Herbert W. Roesky 4.26 Alumazene-Inorganic Benzene Analogue .................. 402 Jiri Pinkas 4.27 Preparation of [Bu4N][B3H8] and the Formation of RuH[B3H8](CO)(PPh3)2 ................................... 405 Anthony F. Hill and J. Derek Woollins 4.28 Vacuum Line Techniques: Preparation of SiF4 and SiF4(C5H5N)2 ........................................... 409 J. Derek Woollins 4.29 Amino- and Nitrotetrazoles: Nitrogen-rich Heterocycles .......................................... 413 Davin С. Piercey and Thomas M. Klapötke 4.30 Ammonium 5-Nitro-1H-Tetrazolate-Hemihydrate ........... 417 Franz Xaver Steemann and Thomas M. Klapötke 4.31 Arsenium Cations: Carbene Analogues ................... 420 Neil Burford and Trenton M. Parks 4.32 Preparation and Structure of the Acetyl Chloride- Antimony Pentachloride Complex ........................ 425 Peter N. Gates 4.33 Preparation and Some Reactions of the Folded P2N4S2 Ring .................................................. 428 Tristram Chivers, Daniel D. Doxsee, and Robert W. Hilts 4.34 Sulfur-Nitrogen Heterocycles and [SNBr0.4]x Polymer .... 432 J. Derek Woollins 4.35 Selenium-Nitrogen and Tellurium-Nitrogen Compounds .... 436 Herbert W. Roesky and Judith Gindl 4.36 Nitride Chlorides of Selenium(lll) and Selenium(IV): Se2NCl3 and Se2NCl5 .................................... 440 Kurt Dehnicke 4.37 The Synthesis and Ring-Opening Polymerisation Behaviour of a [l]Silaferrocenophane .................. 444 Ian Manners Index ......................................................... 447