Inorganic Syntheses (Inorganic Syntheses 36)

Inorganic Syntheses (Inorganic Syntheses 36)

By: Gregory S. Girolami (editor_in_chief), Alfred P. Sattelberger (editor_in_chief)Hardback

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Description

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.

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Contents

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 METAL METAL 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-anisylformamidinato)di(chloro)-dimolybdenum(II,III) 86 C. cis-Bis(N,N0-di-p-anisylformamidinato)tetrakis(acetonitrile)-dimolybdenum(II) Bis(tetrafluoroborate) 87 D. ( 2-Succinato)bis[tris(N,N0-di-p-anisylformamidinato)-dimolybdenum(II)] 88 E. ( 2- 2, 2-Molybdato)bis[tris(N,N0-di-p-anisylformamidinato)-dimolybdenum(II)] 89 F. ( 2-N,N0-Diphenylterephthaloyldiamidato)bis[tris(N,N0-di-panisylformamidinato) dimolybdenum(II)] 90 G. Molecular Propeller: ( 3-Trimesate)tris[tris(N,N0-di-panisylformamidinato) dimolybdenum(II)] 91 H. Molecular Loop: closo-Bis( 2-malonato)bis[bis(N,N0-di-panisylformamidinato) dimolybdenum(II)] 92 I. Molecular Triangle: closo-Tris( 2-eq,eq-1,4-cyclohexanedicarboxylato) tris[bis(N,N0-di-p-anisylformamidinato)-dimolybdenum(II)]92 J. Molecular Square: closo-Tetrakis( 2-oxalato)tetrakis[bis(N,N0-di-p-anisylformamidinato)dimolybdenum(II)] 93 K. Molecular Cage: closo-Tetrakis( 3-trimesate)hexakis[bis(N,N0-di-p-anisylformamidinato)dimolybdenum(II)] 94 18. Dimolybdenum and Ditungsten Hexa(alkoxides) 95 A. Hexa(tert-butoxy)dimolybdenum(III) 96 B. Hexakis(2-trifluoromethyl-2-propoxy)dimolybdenum(III) 97 C. Sodium Heptachloropentakis(tetrahydrofuran)ditungstate(III) 98 D. Hexa(tert-butoxy)ditungsten(III) 99 E. Hexakis(2-trifluoromethyl-2-propoxy)ditungsten(III) 100 19. Linear Trichromium, Tricobalt, Trinickel, and Tricopper Complexes of 2,20-Dipyridylamide 102 A. Dichlorotetrakis(2,20-dipyridylamido)trichromium(II) 103 B. Dichlorotetrakis(2,20-dipyridylamido)tricobalt(II) 104 C. Dichlorotetrakis(2,20-dipyridylamido)trinickel(II) 105 D. Dichlorotetrakis(2,20-dipyridylamido)tricopper(II) 106 E. Bis(acetonitrile)tetrakis(2,20-dipyridylamido)trichromium(II) Bis(hexafluorophosphate) 107 F. Bis(acetonitrile)tetrakis(2,20-dipyridylamido)tricobalt(II) Bis(hexafluorophosphate) 108 G. Bis(acetonitrile)tetrakis(2,20-dipyridylamido)trinickel(II) Bis(hexafluorophosphate) 108 20. Bis(tetrabutylammonium) Octachloroditechnetate(III) 110 A. Tetrabutylammonium Pertechnetate(VII) 111 B. Tetrabutylammonium Oxotetrachlorotechnetate(V) 112 C. Bis(tetrabutylammonium) Octachloroditechnetate(III) 112 21. Diruthenium Formamidinato Complexes 114 A. Chlorotris(acetato)(N,N0-di-2,6-xylylformamidinato)-diruthenium(II,III) 115 B. trans-Chlorobis(acetato)bis(N,N0-di-2,6-xylylformamidinato)-diruthenium(II,III) 117 C. cis-Chlorobis(acetato)bis(N,N0-di-p-anisylformamidinato)-diruthenium(II,III) 118 D. Chloro(acetato)tris(N,N0-di-p-anisylformamidinato)-diruthenium(II,III) 119 E. Chlorotetrakis(N,N0-di-p-anisylformamidinato)-diruthenium(II,III) 120 22. Heptacarbonyl(disulfido)dimanganese(I) 122 23. Di(carbido)tetracosa(carbonyl)decaruthenate(2 ) Salts 124 A. Calcium Di(carbido)tetracosa(carbonyl)decaruthenate(2 ) 124 B. Bis[bis(triphenylphosphoranylidene)ammonium] Di(carbido)tetracosa(carbonyl)decaruthenate(2 ) 125 Chapter Four GENERAL TRANSITION METAL COMPOUNDS 127 24. Bis(1,2-bis(dimethylphosphano)ethane)tricarbonyltitanium(0) and Hexacarbonyltitanate(2 ) 127 A. Bis(1,2-bis(dimethylphosphano)ethane)-tricarbonyltitanium(0) 129 B. Bis[18-crown-6)(acetonitrile)potassium] Hexacarbonyltitanate(2 ) 131 25. Tungsten Benzylidyne Complexes 134 A. Trichloro(1,2-dimethoxyethane)benzylidynetungsten(VI) 135 B. Chloro Bis[1,2-bis(diphenylphosphino)ethane]-benzylidynetungsten(IV) 136 26. Tungsten Oxytetrachloride and (Acetonitrile)tetrachlorotungsten Imido Complexes 138 A. Tungsten Oxytetrachloride 139 B. (Acetonitrile)tetrachloro(phenylimido)tungsten(VI) 140 C. (Acetonitrile)tetrachloro(2-propylimido)tungsten(VI) 141 D. (Acetonitrile)tetrachloro(2-propenylimido)tungsten(VI) 142 27. Tungsten Oxytetrachloride and Several Tungstate Salts 143 A. Tungsten Oxytetrachloride 144 B. Bis(tetrabutylammonium) Hexapolytungstate 145 C. Di(cetylpyridinium) Peroxoditungstate 146 D. Bis(tetrabutylammonium) Phenylphosphonatodiperoxotungstate 147 28. Bromotricarbonyldi(pyridine)manganese(I) 148 29. Bis(tetraethylammonium) fac-Tribromotricarbonylrhenate(I) and -Technetate(I) 149 A. Bis(tetraethylammonium) fac-Tribromotricarbonylrhenate(I) 151 B. Bis(tetraethylammonium) fac-Trichlorotricarbonyltechnetate(I) 152 30. Methyl(oxo)rhenium(V) Complexes with Chelating Ligands 155 A. Methyl(oxo)(1,2-ethanedithiolato)rhenium(V) Dimer 156 B. Methyl(oxo)bis(2-oxyquinoline)rhenium(V) 157 C. Methyl(oxo)(2,20-thiodiacetato)(triphenylphosphine)-rhenium(V) 158 31. Hexahydridoferrate(II) Salts 160 A. Tetrakis[bromobis(tetrahydrofuran)magnesium] Hexahydridoferrate(II) 161 B. Tetrakis[2-methyl-2-propoxomagnesium] Hexahydridoferrate(II) 163 32. Tris(allyl)iridium and -Rhodium 165 A. Allyllithium 166 B. mer-Trichlorotris(tetrahydrothiophene)iridium(III) 166 C. mer-Trichlorotris(tetrahydrothiophene)rhodium(III) 167 D. Tris(allyl)iridium(III) 168 E. Tris(allyl)rhodium(III) 170 33. Trinuclear Palladium(II) Acetate 171 Chapter Five MAIN GROUP COMPOUNDS AND LIGANDS 174 34. Monocarbaborane Anions with 10 or 12 Vertices 174 A. Tetraethylammonium arachno-6-Carba-decaboranate(14) 176 B. Tetraethylammonium closo-2-Carba-decaboranate(10) 177 C. Tetraethylammonium closo-1-Carba-decaboranate(10) 178 D. Tetraethylammonium closo-1-Carba-dodecaboranate(12) 179 E. Tetraethylammonium nido-6-Phenyl-6-carbadecaboranate(12) 180 F. Tetraethylammonium closo-2-Phenyl-2-carbadecaboranate(10) 181 G. Tetraethylammonium closo-1-Phenyl-1-carbadecaboranate(10) 182 H. Tetraethylammonium closo-1-Phenyl-1-carbadodecaboranate(12) 183 35. Tetrakis(5-tert-butyl-2-hydroxyphenyl)ethene 186 A. 5,50-Di-tert-butyl-2,20-dimethoxybenzophenone 187 B. Titanium Trichloride 1,2-Dimethoxyethane (1:1.5) 189 C. Tetrakis(5-tert-butyl-2-methoxyphenyl)ethene 189 D. Tetrakis(5-tert-butyl-2-hydroxyphenyl)ethene 192 36. Electrochemical Synthesis of Tetraethylammonium Tetrathiooxalate 195 37. Mid-Infrared Emitting Lead Selenide Nanocrystal Quantum Dots 198 A. Lead Selenide NQDs Emitting at 2.5 m (0.50 eV) 199 B. Lead Selenide NQDs Emitting at 2.8 m (0.44 eV) 200 C. Lead Selenide NQDs Emitting at 3.3 m (0.38 eV) 201 D. Lead Selenide NQDs Emitting at 3.5 m (0.35 eV) 201 Chapter Six TEACHING LABORATORY EXPERIMENTS 203 38. Tetra(acetato)dichromium(II) Dihydrate 203 39. Keggin Structure Polyoxometalates 210 A. Tri(ammonium) 12-Molybdophosphate 211 B. 12-Tungstosilicic Acid 212 C. 12-Tungstophosphoric Acid 214 D. 12-Molybdophosphoric Acid 215 40. Quadruply Metal Metal Bonded Complexes of Rhenium(III) 217 A. Tetrabutylammonium Perrhenate(VII) 218 B. Bis(tetrabutylammonium) Octachlorodirhenate(III) 219 C. Tetra(acetato)dichlorodirhenium(III) 221 41. Bis[bis(triphenylphosphoranylidene)ammonium] Undecacarbonyltriferrate(2

Product Details

  • publication date: 06/06/2014
  • ISBN13: 9781118744871
  • Format: Hardback
  • Number Of Pages: 336
  • ID: 9781118744871
  • weight: 572
  • ISBN10: 111874487X

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