Inorganic Syntheses

This volume of Inorganic Syntheses spans the preparations of wide range of important inorganic, organometallic and solid-state compounds. The volume is divided into 6 chapters. The first chapter contains the syntheses of some key early transition metal halide clusters and the very useful mononuclear molybdenum(III) synthon, MoCl3(THF)3. Chapter 2 covers the synthesis of a number of cyclopentadienyl compounds, including a novel route to sodium and potassium cyclopentadienide, MC5H5. Chapter 3 details synthetic procedures for a range of metal-metal bonded compounds, including several with metal-metal multiple bonds. Chapter 4 contains procedures for a range of early and late transition metal compounds, each a useful synthon for further synthetic elaboration. Chapter 5 deals with the synthesis of a number of main group compounds and ligands, while Chapter 6 covers teaching laboratory experiments.

Auteur

Professor Gregory S. Girolami received his B.S. degrees in chemistry and physics from the University of Texas at Austin and his Ph.D. degree from the University of California at Berkeley. Thereafter, he was a NATO postdoctoral fellow with Sir Geoffrey Wilkinson at Imperial College of Science and Technology, and joined the Illinois faculty in 1983. Alfred P. Sattelberger is Argonne's Associate?Laboratory Director for Energy Engineering and Systems Analysis. He oversees the Energy Engineering and Systems Analysis?Directorate (EESA), which is responsible for Argonne's programs in energy?researchincluding energy storage, renewable energy, energy efficiency and nuclear energyand national security. Sattelberger obtained a Ph.D. in inorganic chemistry from Indiana University and was a National Science Foundation Postdoctoral Fellow at Case Western Reserve University.

Résumé
This volume of Inorganic Syntheses spans the preparations of wide range of important inorganic, organometallic and solid-state compounds. The volume is divided into 6 chapters. The first chapter contains the syntheses of some key early transition metal halide clusters and the very useful mononuclear molybdenum(III) synthon, MoCl3(THF)3. Chapter 2 covers the synthesis of a number of cyclopentadienyl compounds, including a novel route to sodium and potassium cyclopentadienide, MC5H5. Chapter 3 details synthetic procedures for a range of metal-metal bonded compounds, including several with metal-metal multiple bonds. Chapter 4 contains procedures for a range of early and late transition metal compounds, each a useful synthon for further synthetic elaboration. Chapter 5 deals with the synthesis of a number of main group compounds and ligands, while Chapter 6 covers teaching laboratory experiments.

Contenu
Preface v Dedication vii

Notice to Contributors and Checkers xv

Toxic Substances and Laboratory Hazards xvii

Chapter One TRANSITION METAL HALIDE COMPOUNDS 1

1. Octahedral Hexatantalum Halide Clusters 1

A. Tetradecachlorohexatantalum Octahydrate 3

B. Tetradecabromohexatantalum Octahydrate 4

C. Tetrakis(benzyltributylammonium) Octadecachlorohexatantalate 5

2. Octahedral Hexamolybdenum Halide Clusters 8

A. Tetradecachlorohexamolybdate Hexahydrate (Chloromolybdic Acid) 10

B. Hexamolybdenum Dodecachloride 12

3. Ether Complexes of Molybdenum(III) and Molybdenum(IV) Chlorides 15

A. Tetrachlorobis(diethyl ether)molybdenum(IV) 16

B. Trichlorotris(tetrahydrofuran)molybdenum(III) 17

4. Octahedral Hexatungsten Halide Clusters 19

A. Bis(hydroxonium) Tetradecachlorohexatungstate Heptahydrate (Chlorotungstic Acid) 21

B. Hexatungsten Dodecachloride 22

5. Trinuclear Tungsten Halide Clusters 24

A. Tritungsten Decachloride 26

B. Trisodium Tridecachlorotritungstate 27

C. Tris(benzyltributylammonium) Tridecachlorotritungstate 28

6. Crystalline and Amorphous Forms of Tungsten Tetrachloride 30

A. Crystalline Tungsten Tetrachloride by Solid-State Reduction 32

B. Amorphous Tungsten Tetrachloride by Solution-Phase Reduction 33

Chapter Two CYCLOPENTADIENYL COMPOUNDS 35

7. Sodium and Potassium Cyclopentadienide 35

A. Sodium Cyclopentadienide 36

B. Potassium Cyclopentadienide 37

8. (Pentafluorophenyl)cyclopentadiene and its Sodium Salt 38

A. (Pentafluorophenyl)cyclopentadiene 39

B. Sodium (Pentafluorophenyl)cyclopentadienide 41

9. Bis(5-pentamethylcyclopentadienyl) Complexes of Scandium 42

A. Bis(5-pentamethylcyclopentadienyl)chloroscandium 43

B. Bis(5-pentamethylcyclopentadienyl)methylscandium 44

C. Bis(5-pentamethylcyclopentadienyl)phenylscandium 45

D. Bis(5-pentamethylcyclopentadienyl)(o-tolyl)scandium 46

10. Bis(5-pentamethylcyclopentadienyl) Complexes of Titanium, Zirconium, and Hafnium 47

A. Bis(5-pentamethylcyclopentadienyl)dichlorotitanium(IV) 47

B. Bis(5-pentamethylcyclopentadienyl)dichlorozirconium(IV) 49

C. Bis(5-pentamethylcyclopentadienyl)dichlorohafnium(IV)50

11. Bis(5-pentamethylcyclopentadienyl) Complexes of Niobium and Tantalum 52

A. Bis(5-pentamethylcyclopentadienyl)dichlorotantalum(IV) 53

B. Bis(5-pentamethylcyclopentadienyl)dichloroniobium(IV) 55

12. Bis(5-pentamethylcyclopentadienyl) Complexes of Molybdenum 58

A. Bis(pentamethylcyclopentadienyl)dichloromolybdenum(IV) 59

B. Bis(pentamethylcyclopentadienyl)dihydridomolybdenum(IV) 61

13. (5-Cyclopentadienyl)tricarbonylmanganese(I) Complexes 62

A. (5-Cyclopentadienyl)tricarbonylmanganese(I) 63

B. (5-Pentamethylcyclopentadienyl)tricarbonylmanganese(I) 63

14. 1,10-Diaminoferrocene 65

A. 1,10-Dilithioferrocene N,N,N0,N0-Tetramethylethylenediamine 66

B. 1,10-Dibromoferrocene 67

C. One-Pot Preparation of 1,10-Dibromoferrocene from Ferrocene 68

D. 1,10-Diaminoferrocene 69

E. 1,10-Diaminoferrocenium Hexafluorophosphate 70

F. 1,10-Diaminoferrocenium Triflate 71

15. Mono(5-pentamethylcyclopentadienyl) Complexes of Osmium 72

A. Bromoosmic Acid 74

B. Bis(5-pentamethylcyclopentadienyl)tetrabromodiosmium(III) 75

C. (5-Pentamethylcyclopentadienyl)(1,5-cyclooctadiene)-bromoosmium(II) 76

Chapter Three COMPOUNDS WITH METALMETAL BONDS 78

16. Tetra(acetato)dimolybdenum(II) 78

17. Supramolecular Arrays Based on Dimolybdenum Building Blocks 81

A. Tetrakis(N,N0-di-p-anisylformamidinato)dimolybdenum(II) 84 B. Tris(N,N0-di-p-anisylforma...