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ÊéÃû Inorganic Syntheses
×÷ÕßGregory S. Girolam
Ò³Êý 334
³ö°æÉç wiley
ISBN 978-1-118-74487-1
Ŀ¼Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 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
xix6. 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(¦Ç5-pentamethylcyclopentadienyl) Complexes of Scandium . . . . . . 42
A. Bis(¦Ç5-pentamethylcyclopentadienyl)chloroscandium . . . . . . . . . . . 43
B. Bis(¦Ç5-pentamethylcyclopentadienyl)methylscandium . . . . . . . . . . 44
C. Bis(¦Ç5-pentamethylcyclopentadienyl)phenylscandium . . . . . . . . . . 45
D. Bis(¦Ç5-pentamethylcyclopentadienyl)(o-tolyl)scandium . . . . . . . . . 46
10. Bis(¦Ç5-pentamethylcyclopentadienyl) Complexes of Titanium,
Zirconium, and Hafnium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
A. Bis(¦Ç5-pentamethylcyclopentadienyl)dichlorotitanium(IV) . . . . . . 47
B. Bis(¦Ç5-pentamethylcyclopentadienyl)dichlorozirconium(IV) . . . . . 49
C. Bis(¦Ç5-pentamethylcyclopentadienyl)dichlorohafnium(IV) . . . . . . 50
11. Bis(¦Ç5-pentamethylcyclopentadienyl) Complexes of Niobium
and Tantalum . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
A. Bis(¦Ç5-pentamethylcyclopentadienyl)dichlorotantalum(IV) . . . . . . 53
B. Bis(¦Ç5-pentamethylcyclopentadienyl)dichloroniobium(IV) . . . . . . 55
12. Bis(¦Ç5-pentamethylcyclopentadienyl) Complexes of Molybdenum . . . 58
A. Bis(pentamethylcyclopentadienyl)dichloromolybdenum(IV) . . . . . 59
B. Bis(pentamethylcyclopentadienyl)dihydridomolybdenum(IV) . . . 61
13. (¦Ç5-Cyclopentadienyl)tricarbonylmanganese(I) Complexes . . . . . . . . . . 62
A. (¦Ç5-Cyclopentadienyl)tricarbonylmanganese(I) . . . . . . . . . . . . . . . . 63
B. (¦Ç5-Pentamethylcyclopentadienyl)tricarbonylmanganese(I) . . . . . . 63
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