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Tables of Contents for Synthesis and Technique in Inorganic Chemistry
Chapter/Section Title
Page #
Page Count
Preface to the Third Edition
ix
2
Preface to the First Edition
xi
Introduction
1
16
Safety
1
6
Laboratory Procedures
7
4
Research Notebook
11
1
Standard References in Inorganic Chemistry
12
5
Part I. SOLID-STATE CHEMISTRY
17
30
EXPERIMENT 1. The 1-2-3 Superconductor YBa(2)Cu(3)O(7)
17
10
Tube Furnace Preparation
19
1
Superconductivity
20
1
Iodometric Titrations
21
6
EXPERIMENT 2. The Layered Solids VO(PO(4))(H(2)O)(2) and VO(HPO(4))(H(2)O)(0.5)
27
10
Oxidation of Alcohols to Ketones
29
1
Powder X-ray Diffraction
30
7
EXPERIMENT 3. The Molecular Sieve Zeolite-X
37
10
Ion Exchange in Microporous Solids
38
2
High-Pressure Synthesis
40
7
Part II. MAIN GROUP CHEMISTRY
47
56
EXPERIMENT 4. The Borane-Amine Adduct BH(3):NH(2)C(CH(3))(3)
47
8
Lewis Acids and Bases
48
7
EXPERIMENT 5. Buckminsterfullerene (C(60)) and Its Electrochemistry
55
10
Soxhlet Extraction
57
1
Cyclic Voltammetry
58
7
EXPERIMENT 6. Vacuum Line Synthesis of GeH(4)
65
10
Vacuum Line and Trap-to-Trap Purification
65
3
Gas-Phase Infrared Spectroscopy
68
7
EXPERIMENT 7. Tin Chemistry: Coordination Complexes and Organometallic Derivatives
75
10
Linkage Isomerism
75
2
Nuclear Magnetic Resonance Spectroscopy
77
8
EXPERIMENT 8. Synthesis of (C(6)H(5))(2)PCH(2)CH(2)P(C(6)H(5))(2) in Liquid Ammonia
85
8
Metal-Ammonia Solutions
85
8
EXPERIMENT 9. Electrolytic Synthesis of K(2)S(2)O(8)
93
10
Electrolytic Preparation
93
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