Inorganic Experiments 3E

A classic brought up to date with new experiments using the latest methods.
Modern spectroscopic techniques and current research topics make this an incomparable resource for undergraduate and graduate students, presenting a fascinating approach to inorganic chemistry by providing experiments that resemble real research. As a result, students learn to think in a research-oriented fashion and to research together in a group.
The experiments have been thoroughly tested and safety instructions are included, while hazardous substances are replaced by less harmful ones. This new edition also has a special focus on environmentally friendly experiments.

J. Derek Woollins obtained his PhD from the University of East Anglia (UK) under the supervision of Andrew Thomson and Roger Grinter. He carried out postdoctoral work with Bill Cullen (UBC, Vancouver), Barnett Rosenberg (MSU, Michigan) and Norman Greenwood (Leeds, England) before being appointed as a lecturer at Imperial College London. After 12 years at Imperial College he moved to Loughborough as the Chair in Inorganic Chemistry where he stayed for five years before moving to St. Andrews as the Chair in Synthetic Chemistry in 1999. He is currently Head of the School of Chemistry in St. Andrews.
He has played a major part in the development of P-Se heterocyles, synthesising the new reagent [Ph(Se)PSe2P(Se)Ph]. This compound is now commercially available and known as ‘Woollins Reagent’. He has published over 440 research papers in main group chemistry and two books.

1. Introducton.
1.1 Introduction (J. Derek Woollins).
1.2 General Spectroscopic Techniques and Report Writing (Petr Kilian).
2. Introductory Experiments.
2.1 Preparation and Investigation of Some Coordination Compounds (Manfred Bochmann).
2.2 Gravimetric Analysis of Hexaamminenickel (II) Tetrafluoroborate [Ni(NH3)6](BF4)2 (Manfred Bochmann).
2.3 Analysis of an Iron(III) Oxalate Complex (Manfred Bochmann).
2.4 Characterisation of a Cooper Oxalate Complex KaCub(C2O4)c · dH2O (Andrew W. G. Platt).
2.5 Synthesis of [NH4][BF4] and Synthesis and Titrimetric Analysis of [Zn(NH3)4][BF4]2 (Michael A. Beckett).
2.6 Iron (II) and Lead (II) Formates (Francisco J. Arnáiz, María R. Pedrosa, and Rafal Aguado).
2.7 Ammonium Dichromate, Chromium (III) Oxide, Potassium Chromate and Potassium Tetraperoxochromate(V) (Antonín Ružička and Zdirad Žák).
2.8 Vanadium Alum: An Experiment in Electrosynthesis (David T. Richens).
2.9 Linkage Isomerism: An Infra-Red Study (David T. Richens and Christopher Glidewell).
2.10 Preparation of Cooper (I) Iodide (F. J. Arnáiz, M. R. Pedrosa, and S. Arnáiz).
2.11 Deduction of the Coordination Mode of BH4 in Bis(triphenylphosphine) Copper(I) Borohydride (Ph3P)2CuBH4 (Andrew W. G. Platt).
2.12 Preparation and Identification of a Copper (I) Complex (Andrew W. G. Platt).
2.13 Synthesis and Characteristics of a Metal Hydride Complex (Andrew W. G. Platt).
2.14 Reactivity of Triphenylphosphine and Its Oxide Towards CuCl2 (Paul F. Kelly and Martin B. Smith).
2.15 Synthesis of a Thermochromic Copper Complex (Iain A. Smellie).
2.16 Preparation and Complexation of Tris(3,5-dimethypyrazoyl)hydroborate (Manfred Bochmann).
2.17 Tetraiodotin(IV) and its Triphenylphosphine Complex (Iain A. Smellie and J. Derek Woollins).
2.18 Silicon Oxygen Compounds and Siloxane Polymers (Paul D. Lickiss).
2.19 Preparation and NMR Identification of Two Phosphorus Esters (Christopher Glidewell).
2.20 Synthesis of Tropheylphosphine Oxide and Triphenylphosphine Sulfide (Iain Smellie).
2.21 Preparation of Sodium Trithionate, Na2S3O6 and Potassium Trithionate, K2S3O6 (Andrew G. Platt).
2.22 The Preparation of Potassium Peroxodisulfate, K2S2O8 (Zdirad Žák and Antonín Ružička).
2.23 Polyiodides, Me4Nix (Andrew W. G. Platt).
2.24 Interhalogen Compounds (Ivan P. Parkin).
2.25 Preparation of K[ICI4] (Iain Smellie).
2.26 Synthesis and Infrared Spectroscopic Characterisation of Boranes and Germanes (Ivan P. Parkin).
3. Intermediate Experiments.
3.1 Metal Acetylacetonate Complexes: Preparation and Characterisation (Christopher Glidewell).
3.2 Nickel Dihalide Phosphine Complexes (Ivan P. Parkin).
3.3 Nickel(II) Complexes of Some Schiff Base Ligands (Christopher J. Jones).
3.4 The Synthesis and Coordination Chemistry of Macrocyclic Complexes (Martin Schröder).
3.5 [Co(dinosaur)]Cl3: An Encapsulation Complex Prepared by a Template Reaction (David J. Otway).
3.6 Identification of Stereochemical (Geometrical) Isomers of [Mo(CO)4(L)2] by Infrared Spectroscopy (Michael A. Beckett).
3.7 Five Coordinate Complexes: [VO(acac)2] and [Cr(NH3)6][CuCl5] (Christopher P. Morley).
3.8 Preparation of trans-PtHCI(PPh3)2 and Measurement of its 1H, 31P and 195Pt NMR Spectra (William P. Griffith).
3.9 [MoO2Br2(H2O)2] . (diglyme) and [MoO2Br2(DMF)2] (Francisco J. Arnáiz, María R. Pedrosa , and Rafael Aguado).
3.10 Preparation of an Iron Dinitrogen Complex (Andrew W. G. Platt).
3.11 Preparation of Nitrosyl Complexes of Iron and Nickel (Andrew W. G. Platt).
3.12 Synthesis and Characterisation of Two Metal-Metal Bonded Dimolybdenum Complexes (William Levason, Thomas A Logothetis, and Gill Reid).
3.13 Cobalt Complexes of Dioxygen (David T. Richens and Christopher Glidewell).
3.14 Ferrocene, (η5-c5H5)2Fe, and its Derivatives (J. Derek Woollins).
3.15 The Use of Organolithium Reagents in the Preparation of Ferrocene Derivatives (Ian R. Butler).
3.16 Complexes of π-Bonding Arene Ligands (Andrew W. G. Platt).
3.17 Organotin Chemistry (Kieran C. Molloy ad Timothy T. Paget).
3.18 Transition Metal-Carbon Bonds in Chemistry and Biology (Christopher J. Jones).
3.19 Nickel-Catalysed Cross-Coupling of Alkylmagnesium with Haloarene (G. Brent Young).
3.20 Transition Metal Catalysis (Neil M. Boag).
3.21 Nitration of Cobalt(III) Acetylacetonate (David J. Otway).
3.22 Phenyllithium and Tetraphenylsilane (Petr Kilian).
3.23 Synthesis and Reactivity of Tertiary Phosphines (Neil M. Boag).
3.24 Two-stage Synthesis of Ph2P(O)(CH2)4P(O)Ph2 (Andrew G. Platt).
3.25 Inorganic Heterocycles: Cyclophosphazenes (Josef Novosad and Milan Alberti).
3.26 Inorganic (Carbon-Free) Chelate Rings: A Dithioimidodiphosphinato Ligand and Some of its Metal Complexes (Ionel Haiduc).
3.27 Inorganic (Carbon-Free) Chelate Rings II: Asymmetric Mixed-Donor P-N-P Ligand and its Palladium Complex (David J. Birdsall and Josef Novasad).
3.28 Amidosulfiric Acid, Trisilveramidosulfate Monhydrate and SO3 . N (CH3)3 Complexes (Antonín Ružička and Zdirad Žák).
3.29 Anomalous Paramegnetism in Some Iron (III) Chelates Studies by the Evans NMR Method (David J. Otway).
3.30 Cubic Molecular Aluminophisphonates (Jiri Pinkas).
3.31 Preparation and Optical Properties of Zinc Sulfide Quantum Dots (Andrew L. Hector).
3.32 Four Methods for Analysing First Order Kinetics (Véronique Pimienta, Dominique Lavabre, Jean-Claude Micheau, and Gaston Levy).
3.33 Molecular Orbital Calculations of Inorganic Compounds (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 (Edwin C. Constable).
4.2 4’-(4-Pyridyl)-2,2’:6’,2”-terpyridine: Coordination to Iron(II) and Protonation Studies (Catherine E. Housecroft, Edwin C. Constable, and Emma L. Dunphy).
4.3 Heteronuclear d-f Complexes Containing Binucleating Ligands (Francisco J. Arnáiz, Jean-Pierre Costes, and Javier García-Tojal).
4.4 Electronic Characterisation of a Transition Metal Complex Using Electrochemical UV/Vis and EPR Techniques (Lesley J. Yellowlees).
4.5 Chlorotris (tert-butylimido) manganese(VII) (Andreas A. Danopoulos and Geoffrey Wilkinson).
4.6 Tetrakisphosphorane Iminato Complexes of Transition Metals (Kurt Dehnicke).
4.7 Magnetochemistry Experiments: Exchange Coupling in Copper(II)-Nickel(II) Bimetallic Complexes and Spin Transition in Iron Complexes (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(II) and Related Specieis – The Use of Melt Syntheses (Duncan W. Bruce).
4.9 Structural, Electrical and Magnetic Properties of Perovskite Ceramics (Colin Greaves).
4.10 Polyoxomolybdate Clusters: Nanoscopic Wheels and Balls (Leroy Cronin, Ekkehard Diemann, and Achim Müller).
4.11 Reaction of Alkali Metal Polyselenides and Polytellurides with Group 6 Metal Carbonyls (Joseph W. Kolis).
4.12 Chlorothionitrene and Cyclothiazeno Complexes of Tungsten (Kurt Dehnicke).
4.13 Sulfur-Rich Homocycles and Heterocycles: Titanocene Pentasulfide, cyclo-Heptasulfur and 1,2,3,4,5,6.7-Heptathionane (Jörg Albertsen and Ralf Steudel).
4.14 N-Ferrocenyl Amine and Some Reactive Derivatives (Max Herbehold, Heidi E. Maisel, and Bernd Wrackmeyer).
4.15 1,1’-Bis(trimethylsilylamino)ferrocene – A Useful Precursor to 1,n-Diaza-[n]ferrocenphanes (Max Herberhold, Elena V. Klimkina, and Bernd Wrackmeyer).
4.16 Organometallic Molybdenum Compounds (Manfred Bochmann and Petr Klian).
4.17 Migratory Insertion Reactions in Organo Transition-Metal Chemistry (Mark J. Winter).
4.18 A Transition-Metal Alkylidyne Complex (Stephen Anderson, Darren Cook, and Anthony F. Hill).
4.19 The Synthesis of η6-Arenetricarbonyl Chromium(0) Complexes (David A. Widdowson).
4.20 Preparation of the Iron Tricarbonyl Complex of Methyl-2-Acetamidoacrylate (M. Elena Lasterra-Sanchez and Susan E. Gibson).
4.21 Halfsandwich Carbonyl Vanadium Complexes (Max Herberhold and Mattias Schrepfermann).
4.22 Covalent and Ionic Metallocene Hexafluoroarsenate Complexes (Inis C. Tornieporth-Oetting and Thomas M. Klapötke).
4.23 The Prepara of rac-Ethylene-1,2-bis(1-indenyl)zirconium Dichloride and Dibenzyl Complexes (Manfred Bochmann and Simon J. Lancaster).
4.24 One-Pot Preparation of Ru3(CO)12 from RuCl3 . 3 H2O (Guy Lavigne, Catherine Saccavini, and Remi Chauvin).
4.25 Synthesis of Well-defined Organometallic Hydroxides: [LCaOH]2, LAI(ME)OH and LGeOH (Herbert W. Roesky).
4.26 Alumazene – Inorganic Benzene Analogue (Jiri Pinkas).
4.27 Preparation of [Bu4N][B3H8] and the Formation of RuH[B3H8](CO)(PPh3)2 (Anthony F. Hill and J. Derek Woollins).
4.28 Vacuum Line Techniques: Preparation of SiF4 and SiF4(C5H5N)2 (J. Derek Woollins).
4.29 Amino- and Nitrotetrazoles: Nitrogen-rich Heterocycles (Davin G. Piercey and Thomas M. Klapötke).
4.30 Ammonium 5-Nitro-1 H-Tetrazolate-Hemihydrate (Franz Xaver Steemann and Thomas M. Klapötke).
4.31 Arsenium Cations: Carbene Analogues (Neil Burford and Trenton M. Parks).
4.32 Preparation and Structure of the Acetyl Chloride-Antimony Pentrachloride Complex (Peter N. Gates).
4.33 Preparation and Some Reactions of the Folded P2N4S2 Ring (Tristram Chivers, Daniel D. Doxsee, and Robert W. Hilts).
4.34 Sulfur-Nitrogen Heterocycles and [SNBr0.4]x Polymer (J. Derek Woollins).
4.35 Selenium-Nitrogen and Tellurium-Nitrogen Compounds (Herbert W. Roesky and Judith Gindl).
4.36 Nitride Chlorides of Selenium(III) and Selenium(IV): Se2NCl3 and Se2NCl5 (Kurt Dehnicke).
4.37 The Synthesis and Ring-Opening Polymerisation Behaviour of a [1]Silaferroceneophane (Ian Manners).
Index.