Synthesis and Technique in Inorganic Chemistry : A Laboratory Manual

, by Girolami, Gregory S.; Rauchfuss, Thomas B.; Angelici, Robert J.

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ISBN: 9780935702484 | 0935702482
Cover: Lab Manual
Copyright: 7/1/1999

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Supplemental Materials

Preface to the Third Edition

(2)

Preface to the First Edition

Introduction

(16)

Safety

(6)

Laboratory Procedures

(4)

Research Notebook

(1)

Standard References in Inorganic Chemistry

(5)

Part I. SOLID-STATE CHEMISTRY

(30)

EXPERIMENT 1. The 1-2-3 Superconductor YBa(2)Cu(3)O(7)

(10)

Tube Furnace Preparation

(1)

Superconductivity

(1)

Iodometric Titrations

(6)

EXPERIMENT 2. The Layered Solids VO(PO(4))(H(2)O)(2) and VO(HPO(4))(H(2)O)(0.5)

(10)

Oxidation of Alcohols to Ketones

(1)

Powder X-ray Diffraction

(7)

EXPERIMENT 3. The Molecular Sieve Zeolite-X

(10)

Ion Exchange in Microporous Solids

(2)

High-Pressure Synthesis

(7)

Part II. MAIN GROUP CHEMISTRY

(56)

EXPERIMENT 4. The Borane-Amine Adduct BH(3):NH(2)C(CH(3))(3)

(8)

Lewis Acids and Bases

(7)

EXPERIMENT 5. Buckminsterfullerene (C(60)) and Its Electrochemistry

(10)

Soxhlet Extraction

(1)

Cyclic Voltammetry

(7)

EXPERIMENT 6. Vacuum Line Synthesis of GeH(4)

(10)

Vacuum Line and Trap-to-Trap Purification

(3)

Gas-Phase Infrared Spectroscopy

(7)

EXPERIMENT 7. Tin Chemistry: Coordination Complexes and Organometallic Derivatives

(10)

Linkage Isomerism

(2)

Nuclear Magnetic Resonance Spectroscopy

(8)

EXPERIMENT 8. Synthesis of (C(6)H(5))(2)PCH(2)CH(2)P(C(6)H(5))(2) in Liquid Ammonia

(8)

Metal-Ammonia Solutions

(8)

EXPERIMENT 9. Electrolytic Synthesis of K(2)S(2)O(8)

(10)

Electrolytic Preparation

(10)

Part III. COORDINATION CHEMISTRY

103

(58)

EXPERIMENT 10. Ion Exchange Separation of Chromium Complexes

103

(8)

Ion Exchange Chromatography

103

(2)

Ligand Exchange Reactions

105

(6)

EXPERIMENT 11. Metal-Metal Quadruple Bonds

111

(6)

Molecular Orbital Theory

112

(5)

EXPERIMENT 12. The Paramagnetic Complex Mn(acac)(3)

117

(14)

Magnetic Susceptibility

120

(3)

The Gouy Method

123

(2)

The Evans Method

125

(6)

EXPERIMENT 13. Preparation and Aquation of Co(NH(3))(5)Cl^(2+)

131

(12)

Electrical Conductance of Solutions of Ionic Compounds

133

(1)

Ligand Exchange Kinetics

134

(9)

EXPERIMENT 14. Optical Resolution of Co(en)(3)^(3+)

143

(8)

Optical Rotations

144

(2)

Resolution of Optical Isomers

146

(5)

EXPERIMENT 15. Metal Dithiolenes and the Use of Quaternary Ammonium Salts

151

(10)

Quaternary Ammonium Salts

152

(9)

Part IV. ORGANOMETALLIC CHEMISTRY

161

(50)

EXPERIMENT 16. The Metal-Arene Complex [1,3,5-C(6)H(3)(CH(3))(3)] Mo(CO)(3)

161

(10)

Infrared Spectra of Metal Carbonyls

163

(8)

EXPERIMENT 17. Organoiron Chemistry: (C(5)H(5))(2)Fe(2)(CO)(4) and (C(5)H(5))Fe(CO)(2)CH(3)

171

(10)

Schlenk Line Techniques

172

(1)

Infrared Spectra of Solutions

172

(9)

EXPERIMENT 18. The Metal Carbonyl Cluster Fe(3)(CO)(12)

181

(8)

Mass Spectrometry

183

(6)

EXPERIMENT 19. Microscale Synthesis of Vaska's Complex IrCl(CO)[P(C(6)H(5))(3)](2)

189

(8)

Oxidative Addition Reactions

190

(1)

Infrared Spectra of Solids

191

(6)

EXPERIMENT 20. The Air-Sensitive Sandwich Complex Nickelocene

197

(14)

Diels-Alder Additions

199

(3)

Sublimation

202

(1)

Glovebag Manipulations

203

(8)

Part V. BIOINORGANIC CHEMISTRY

211

(34)

EXPERIMENT 21. Cobaloximes: Models of Vitamin B(12)

211

(8)

Enzyme Models

211

(8)

EXPERIMENT 22. Amino Acid Complexes: Stability Constants of Ni(glycinate)(n)^((2-n)+)

219

(14)

Amino Acid Chemistry

219

(4)

pH Titrations of Metal Complexes

223

(10)

EXPERIMENT 23. Bioinorganic Coordination Chemistry: Copper(II) Tetraphenylporphyrinate

233

(12)

Metalloporphyrin Chemistry

233

(2)

Thin-layer and Column Chromatography

235

(10)

Notes to Instructor

245

(8)

Appendices

253

(16)

1. Approximate Concentrations and Densities of Commercial, Reagent Grade Acids and Bases

253

(1)

2. Expected Molar Conductance (Lambda)(M)) Ranges for 2, 3, 4, and 5 Ion Electrolytes in Some Common Solvents

254

(1)

3. Transmission Ranges of Cell Materials for Infrared and Ultraviolet-Visible Spectroscopy

255

(1)

4. Properties of Commercial Glasses

256

(1)

5. Common Solvents and Their Properties

257

(1)

6. Drying (Dehydrating) Agents

258

(1)

7. Natural Abundances and Nuclear Spins of Stable Isotopes

259

(3)

8. Baths for Cooling and Heating

262

(1)

9. SI Units

263

(2)

10. Selected Spectra

265

(4)

General Index

269

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Synthesis and Technique in Inorganic Chemistry : A Laboratory Manual

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