Synthesis and Technique in Inorganic Chemistry
Third Edition

Gregory S. Girolami
University of Illinois, Urbana-Champaign

Thomas B. Rauchfuss
University of Illinois, Urbana-Champaign

Robert J. Angelici
Iowa State University

Introduction

• Safety
• Laboratory Procedures
• Research Notebook
• Standard References

Part I. Solid State Chemistry

Experiment 1--High-Temperature Synthesis of the Superconductor YBa₂Cu₃O₇

• Tube Furnace Preparation
• Superconductivity
• Iodometric Titrations

Experiment 2--The Layered Solids VOPO₄(H₂O)₂ and VO(HPO₄)(H₂O)_0.5

• Powder X-Ray Diffraction
• Oxidation of Alcohols to Ketones

Experiment 3--The Molecular Sieve Zeolite-X

• Sol-gel Synthesis
• High Pressure Synthesis
• Ion Exchange in Microporous Solids

Part II. Main Group Chemistry

Experiment 4--The Borane-Amine Adduct BH₃NH₂C(CH₃)₃

• Lewis Acids and Bases

Experiment 5--Buckminsterfullerene, C₆₀, and Its Electrochemistry

• Soxhlet Extraction
• Cyclic Voltammetry

Experiment 6--Vacuum-Line Synthesis of GeH₄

• Vacuum Line and Trap-to-Trap Purification
• Vapor Pressure and Molecular Weight Determination of a Volatile Compound
• Gas Phase IR Spectroscopy

Experiment 7--Tin Chemistry: Coordination Complexes and Organometallic Derivatives

• NMR Spectroscopy
• Linkage Isomerism

Experiment 8--Synthesis of (C₆H₅)₂PCH₂CH₂P(C₆H₅)₂ in Liquid Ammonia

• Synthesis in Liquid Ammonia

Experiment 9--Electrolytic Synthesis of K₂S₂O₈

• Electrolytic Preparation

Part III. Coordination Chemistry

Experiment 10--Ion Exchange Separation of Chromium Complexes

• Ion Exchange Chromatography

Experiment 11--Metal-Metal Quadruple Bonds

• Molecular Orbital Theory

Experiment 12--The Magnetic Susceptibility of Mn(acac)₃

• Magnetism of Transition Metal Complexes
• The Gouy Method
• The Evans Methods

Experiment 13--Cobalt Ammines and their Ligand Substitution Kinetics

• Conductivity of Ionic Complexes
• Kinetics of Aquation of [Co(NH₃)₅Cl]²⁺

Experiment 14--Optical Resolution of Co(en)₃³⁺

• Separation of Diastereomers by Crystallization
• Optical Rotations
• Suction Filtration

Experiment 15--Metal Dithiolenes and the Use of Quaternary Ammonium Salts

• Quaternary Ammonium Salts

Part IV. Organometallic Chemistry

Experiment 16--The Metal-Arene Complex [1,3,5-C₆H₃(CH₃)₃]Mo(CO)₃

• IR Spectra of Metal Carbonyls

Experiment 17--Organo-iron Chemistry: (C₅H₅)₂Fe₂(CO)₄ and (C₅H₅)Fe(CO)₂(CH₃)

• Schlenk Line Synthesis
• Infrared Spectra of Solutions

Experiment 18--The Metal Carbonyl Cluster Fe3(CO)₁₂

• Mass Spectrometry

Experiment 19--Microscale Synthesis of Vaska's Complex

• Microscale Synthesis
• Solid State IR Spectra

Experiment 20--The Air-Sensitive Sandwich Complex Nickelocene

• Glove Bag Manipulations
• Sublimation

Part V. Bioinorganic Chemistry

Experiment 21--Cobaloximes: Models of Vitamin-B₁₂ Coenzymes

• Enzyme Models

Experiment 22--Amino Acid Complexes: Stability Constants of Ni(glycinate)_n^{(2 - n)+}

• Amino Acid Chemistry
• pH Titrations
• pK_a and Successive Stability Constant Determination

Experiment 23--Bioinorganic Coordination Chemistry: Copper (II) Tetraphenylporphyrinate

• Porphyrin Chemistry
• Thin-Layer Chromatography
• Column Chromatography

Notes to the Instructor

Appendices

NMR and Mass Spectra

Index