Organometallic Syntheses (eBook)

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2013 | 1. Auflage
640 Seiten
Elsevier Science (Verlag)
978-1-4832-9002-7 (ISBN)

Over 160 detailed and tested procedures for the preparation of specific organometallic compounds are given in Volume 4. Part I contains procedures for the synthesis of 76 types of transition metal organometallic compounds, and Part II procedures for the synthesis of 85 nontransition metal organometallic compounds. In both parts, the editors have sought to include procedures that give the safe, reliable synthesis of organometallic compounds that can lay some claim to significance in current chemical research. This significance may be based on various factors such as: (a) the synthesis describes the formation of an unusual or less common structural type; (b) the compound prepared is a useful intermediate in other syntheses; (c) the compound is a model reagent for investigating the mechanisms of various fundamental or industrial processes, such as the Fischer-Tropsch reaction; (d) the compound is a useful reagent in organic synthesis; and (e) the techniques employed in the synthesis of the compound are unusual and worthy of further application, such as metal-atom and electrochemical procedures.
Each specific or generalized procedure is organized into the following sections: an Introduction which discusses the available procedures and the reasons guiding the choice of the one selected; a Procedure section which strives to describe the modus operandi, the safety concerns and pitfalls in the preparation; a Properties section that offers further physical and chemical data on the product and, where appropriate, indications of how the compounds can be employed in research; and a Reference section which gives both leading literature citations and supplemental comments on the procedure.
Research laboratories in organometallic chemistry, organic chemistry, inorganic chemistry and molecular catalysis have in this book a rich source of information on the preparation of organometallic compounds.

Over 160 detailed and tested procedures for the preparation of specific organometallic compounds are given in Volume 4. Part I contains procedures for the synthesis of 76 types of transition metal organometallic compounds, and Part II procedures for the synthesis of 85 nontransition metal organometallic compounds. In both parts, the editors have sought to include procedures that give the safe, reliable synthesis of organometallic compounds that can lay some claim to significance in current chemical research. This significance may be based on various factors such as: (a) the synthesis describes the formation of an unusual or less common structural type; (b) the compound prepared is a useful intermediate in other syntheses; (c) the compound is a model reagent for investigating the mechanisms of various fundamental or industrial processes, such as the Fischer-Tropsch reaction; (d) the compound is a useful reagent in organic synthesis; and (e) the techniques employed in the synthesis of the compound are unusual and worthy of further application, such as metal-atom and electrochemical procedures.Each specific or generalized procedure is organized into the following sections: an Introduction which discusses the available procedures and the reasons guiding the choice of the one selected; a Procedure section which strives to describe the modus operandi, the safety concerns and pitfalls in the preparation; a Properties section that offers further physical and chemical data on the product and, where appropriate, indications of how the compounds can be employed in research; and a Reference section which gives both leading literature citations and supplemental comments on the procedure.Research laboratories in organometallic chemistry, organic chemistry, inorganic chemistry and molecular catalysis have in this book a rich source of information on the preparation of organometallic compounds.

Front Cover 1
Organometallic Syntheses 4
Copyright Page 5
Table of Contents 12
Editorial Advisory Board For Volumes 3 And 4 of Organometallic Syntheses 6
Introduction 8
Preface 10
PART I: TRANSITION METAL ORGANOMETALLIC COMPOUNDS 22
CHAPTER 1. BIS (CYCLOPENTADIENYL) AND MONO- AND BIS (PENTAMETHYLCYCLOPENTADIENYL) METHYL DERIVATIVES OF THE LANTHANIDES: THEIR METHYLLITHIUM ADDUCTS 24
INTRODUCTION 24
PROCEDURE 25
PROPERTIES 28
REFERENCES 28
CHAPTER 2. (.4-BUTADIENE) BIS (.-PENTAMETHYLCYCLOPENTADIENYL) THORIUM 29
INTRODUCTION 29
PROCEDURE 30
PROPERTIES 30
REFERENCES 31
CHAPTER 3. [(PHENYLZIRCONOCENYL) METHYLENE] TRIPHENYLPHOSPHORANE 32
INTRODUCTION 32
PROCEDURE 33
PROPERTIES 33
SPECTROSCOPIC DATA 34
REFERENCES 34
CHAPTER 4. BIS (.5-CYCLOPENTADIENYL) (DICARBONYL) TITANIUM (II) 35
INTRODUCTION 35
PROCEDURE 36
PROPERTIES 36
REFERENCES 36
CHAPTER 5. BIS (.5-CYCLOPENTADIENYL) VANADIUM (VANADOCENE) 38
PROCEDURE 39
PROPERTIES 40
REFERENCES AND NOTES 40
CHAPTER 6. (.5-CYCLOPENTADIENYL) NIOBIUM TETRACHLORIDE AND -TANTALUM TETRACHLORIDE 43
INTRODUCTION 43
PROCEDURE 43
PROPERTIES 44
REFERENCES 44
CHAPTER 7. (.5-PENTAMETHYLCYCLOPENTADIENYL) NIOBIUM TETRACHLORIDE AND -TANTALUM TETRACHLORIDE 45
INTRODUCTION 45
PROCEDURE 45
PROPERTIES 46
REFERENCES 46
CHAPTER 8. BIS (.5-CYCLOPENTADIENYL) NIOBIUM DICHLORIDE AND -TANTALUM DICHLORIDE 47
INTRODUCTION 47
PROCEDURE 47
PROPERTIES 47
PROCEDURE 48
PROPERTIES 48
REFERENCES 48
CHAPTER 9. BIS (.5-PENTAMETHYLCYCLOPENTADIENYL) NIOBIUM DICHLORIDE AND -TANTALUM DICHLORIDE 49
INTRODUCTION 49
PROCEDURE 49
PROPERTIES 50
REFERENCES 50
CHAPTER 10. OLEFIN COMPLEXES OF NIOBIUM HYDRIDE (III) AND TANTALUM HYDRIDE (III) 51
INTRODUCTION 51
PROCEDURE 51
PROPERTIES 53
REFERENCES 53
CHAPTER 11. BIS (.5-CYCLOPENTADIENYL) (ALLYL) COMPLEXES OF NIOBIUM AND TANTALUM 54
INTRODUCTION 54
PROCEDURE 54
PROPERTIES 55
REFERENCES 55
CHAPTER 12. BIS (.5-CYCLOPENTADIENYL) (ALLYL) COMPLEXES OF NIOBIUM AND TANTALUM 54
INTRODUCTION 56
PROCEDURE 56
PROPERTIES 58
REFERENCES 59
CHAPTER 13. MONO- AND BIS (DIENE) COMPLEXES OF TANTALUM 60
INTRODUCTION 60
PROCEDURE 60
PROPERTIES 63
REFERENCES 63
CHAPTER 14. TRIMETHYLSILYLCYCLOPENTADIENYLNIOBIUM DERIVATIVES 64
INTRODUCTION 64
PROCEDURE 64
PROPERTIES 65
Part II. CHLORO (TRIMETHYLPHOSPHINE) BIS (.5-TRIMETHYLSILYLCYCLOPENTADIENYL)- NIOBIUM (III) 65
INTRODUCTION 65
PROCEDURE 65
PROPERTIES 66
Part III. METHYLPEROXOBIS (.5-TRIBETHYLSILYLCYCLOPENTADIENYL) NIOBIUM (V) 66
INTRODUCTION 66
PROCEDURE 66
PROPERTIES 67
REFERENCES 67
CHAPTER 15. SODIUM HEXACARBONYLVANADATE (-I) 69
INTRODUCTION 69
PROCEDURE 69
PROPERTIES 70
REFERENCES 71
CHAPTER 16. HEXACARBONYLVANADIUM (O) 72
PROCEDURE 72
PROPERTIES 73
REFERENCES 74
CHAPTER 17. BIS (n5-CYCLOPENTADIENYL) CHROMIUM (CHROMOCENE) 75
PROCEDURE 75
PROPERTIES 77
REFERENCES 77
CHAPTER 18. BIS (TRIPHENYLPHOSPHINE) IMINIUM TETRACARBONYLNTTROSYLCHROMATE 79
INTRODUCTION 79
PROCEDURE 79
PROPERTIES 80
REFERENCES 80
CHAPTER 19. Cp (CO) 2Mo[NH(R)CH(py)], A MOLYBDENA-AZIRIDINE COMPLEX CONTAINING A MoNC THREE-MEMBERED RING 96
INRODUCTION 96
PROCEDURE 96
STEREOCHEMISTRY 97
PROPERTIES 97
SCOPE OF THE REACTION 97
REACTIONS OF C5H5 (CO) 2Mo[ NH (R) CH (py)] 97
REFERENCES 98
CHAPTER 20. TRANS-DICARBONYL (CYCLOPENTADIENYL) FORMYL (TRIPHENYLPHOSPHINE) MOLYBDENUM 99
INTRODUCTION 99
PROCEDURE 99
PROPERTIES 100
REFERENCES 100
CHAPTER 21. [.1-N,.1-P-4,5 DIMETHYL-2-(2'-PYRIDYL) PHOSPHININE] TETRACARBONYLCHROMIUM 101
INTRODUCTION 102
PROCEDURE 102
PROPERTIES 103
REFERENCES 104
CHAPTER 22. ISOCYANOMETHY LENETRIPHENYLPHOSPHORANE AND RELATED SPECIES 105
INTRODUCTION 105
1. ISOCYANOMETHYLTRIPHENYLPHOSPHONIUM CHLORIDE 105
2. ISOCYANOMETHYLTRIPHENYLPHOSPHONIUM HEXAFLUOROPHOSPHATE 106
3. PENTACAHBONYL (TRIPHENYLPHOSPHONIOMETHYLISOCYANIDE) TUNGSTEN HEXAFLUOROPHOSPHATE 107
4. PENTACARBONYL [(FLUORENE–9–YLIDENE) METHYLISOCYANIDE] TUNGSTEN 108
5. PENTACARBONYL [1-PHENYL-3H-4-(TRIPHENYLPHOSPHORANEYLIDENE)-5- IMIDAZOLIDINTHIONE-2-YLIDENE] TUNGSTEN 109
CHAPTER 23. N–ISOCYANOIMINETRIPHENYLPHOSPHORANE AND RELATED SPECIES 110
INTRODUCTION 110
1. N-ISOCYANOIMINETRIPHENYLPHOSPHORANE 110
2. PENTACARBONYL (ISOCYANOIMINETRIPHENYLPHOSPHORANE) CHROMIUM AND-TUNGSTEN 111
3. PENTACARBONYL (ISOPROPYLIDENE ISOCYANOAMINE) CHROMIUM 112
4. PENTACARBONYL (CYCLOHEXYLIDENE ISOCYANOAMINE) TUNGSTEN 113
5. PENTACARBONYL (ISODIAZOMETHANE) CHROMIUM 113
CHAPTER 24. ALKYL DERIVATIVES OF OCTAHEDRAL MOLYBDENUM AND TUNGSTEN CLUSTER COMPLEXES 115
INTRODUCTION 115
PROCEDURE 116
PROPERTIES 117
REFERENCES 118
CHAPTER 25. BIS (TERT.-BUTYL-.5-CYCLOPENTADIENYL) MANGANESE 119
PROCEDURE 119
PROPERTIES 121
REFERENCES 121
CHAPTER 26. TRISODIUM TETRACARBONYLMETALLATES (-III) OF MANGANESE AND RHENIUM, Na3[M(8)4] 123
INTRODUCTION 123
PROCEDURE 124
PROPERTIES 125
REFERENCES 126
CHAPTER 27. CIS-TETRACARBONYLFORMYL (TRIPHENYLPHOSPHINE) MANGANESE 127
INTRODUCTION 127
PROCEDURE 127
PROPERTIES 128
REFERENCES 128
CHAPTER 28. MER-TRICARBONYLFORMYLBIS (TRIPHENYLPHOSPHITE-P) MANGANESE 129
INTRODUCTION 129
PROCEDURE 129
PROPERTIES 130
REFERENCES 130
CHAPTER 29. METAL CARBONYL CATIONS WITH CYCLIC PI-HYDROCARBON LIGANDS 131
I. MANGANESE CYCLOHEXADIENYL COMPLEXES 131
II. MANGANESE CYCLOHEPTADIENYL COMPLEXES 135
III. RHENIUM CYCLOHEXADIENYL COMPLEXES 138
IV. DICARBONYL (ALKENE) (ARENE) MANGANESE COMPLEXES 140
ACKNOWLEDGMENT 142
REFERENCES 142
CHAPTER 30. TRICARBONYL [h3-OCTAHYDROTIRBORATO (1-)] MANGANESE, (CO)3MnB3H8 144
INTRODUCTION 144
PROCEDURE 144
PROPERTIES OF (CO)3MNB3H8 146
REFERENCES 147
CHAPTER 31. NIDO -2-TRICARBONYL-2-MANGANAHEXABORANE, NIDO -2-(CO)3-2-MnB5H10 148
INTRODUCTION 148
PROCEDURE 148
PROPERTIES OF 2-(CO)3-2-MnB5H10 149
REFERENCES 152
CHAPTER 32. NIDO-6-TRICARBONYL-6-MANGANATRIDECAHYDRODECABORATE, NIDO-6-(CO)3-6-MnB9H13-, AND ITS DERIVATIVES 153
INTRODUCTION 153
PROCEDURE 153
PROPERTIES 154
REFERENCES 156
CHAPTER 33. CIS-BIS (TRIFLUOROACETYL) TETRACARBONYLIRON AND CIS-BIS (TRIFLUOROMETHYL) TETRA-CARBONYLIRON 157
INTRODUCTION 157
1. CIS-BIS (TRIFLUOROACETYL) TETRACARBONYLIRON 158
2. CIS-BIS (TRIFLUOROMETHYL) TETRACARBONYLIRON 159
REFERENCES 160
CHAPTER 34. PERRA- AND RUTHENACYCLOPENTANES, AND .2- ETHENE COMPLEXES OF IRON AND RUTHENIUM 161
INTRODUCTION 161
2 A. Synthesis of tetracarbonyl (.2 -ethene) iron (2ax), tetracar- bonylferracyclopentane (3ax), and -bicyclo [4.3.0] nonane (4ax) 164
B. Synthesis of tetracarbonyl (.2 -ethene) ruthenium (2bx), tetra- carbonylruthenacyclopentane (3bx), and -bicyclo [4.3.0] nonane (4bx) 166
C. Synthesis of PPh3 substituted tricarbonyl (.2-ethene) iron (2ay), tricarbonylferracyclopentane (3ay), and -bicyclo [4.3.0] nonane 168
REFERENCES 171
CHAPTER 35. THIOCARBONYL IRON (O) COMPLEXES 172
INTRODUCTION 172
REFERENCES 173
CHAPTER 36. [(CARBONYLBIS ((DIISOPROPYLAMINO) PHOSPHIDO)] HEXACARBONYLDIIRON 175
INTRODUCTION 175
PROCEDURE 175
PROPERTIES 176
REFERENCES 177
CHAPTER 37. [(DIISOPROPYLAMINO) TRIPHOSPHINE] HEXACARBONYLDIIRON 178
INTRODUCTION 178
PROCEDURE 179
PROPERTIES 180
REFERENCES 181
CHAPTER 38. VINYLMETALLOCENES: VINYLFERROCENE,- RUTHENOCENE AND -OSMOCENE 1,1'-DIVINYLFERROCENE AND - RUTHENOCENE
INTRODUCTION 182
PROCEDURE 183
PROPERTIES 184
REFERENCES AND NOTES 185
CHAPTER 39. METHYL ESTERS OF FERROCENE THIO- AND DITHIO CARBOXYLIC ACIDS 188
INTRODUCTION 189
PROCEDURE 189
PROPERTIES 190
REFERENCES 191
CHAPTER 40. FERROCENYL PENTACARBONYLMANGANESE 192
INTRODUCTION 192
PROCEDURE 192
PROPERTIES 193
REFERENCES 194
CHAPTER 41. THERMALLY STABLE 19-ELECTRON Fe (I) AND RELATED COMPLEXES 195
C. (.5-cyclopentadienyl) ( .6-benzene) iron (I) 201
D. (.5-cyclopentadienyl) (.5-pentamethylmethylenecyclohexadienyl) iron (II) 202
E. (.6-hexamethylbenzene)2 iron (I) hexafluorophosphate 203
F. (.5-hexamethylcyclohexadienyl) (.6-hexamethylbenzene) iron (I)10 204
G. (.10, µ2-C10 H8 {(.6 -C6Me6)Fe} 2+PF6 205
J. Bis [(.5-pentamethylcyclopentadienyl) iron (I) (biphenyl) hexafluorophos-phate 208
Acknowledgments 209
References 209
CHAPTER 42. .6-DIETHYL PHENYLMALONATE-.5- CYCLOPENTADIENYLIRON HEXAFLUOROPHOSPHATE 211
INTRODUCTION 211
PROCEDURE 211
DISCUSSION 212
REFERENCES 212
CHAPTER 43. (R,S)-1-5-.5-1-NITRO-6-EXO-(2-OXO-1-PROPYL)- CYCLOHEXADIENYL-.5-CYCLOPENTADIENYL-IRON 214
INTRODUCTION 214
PROCEDURE 215
DISCUSSION 215
REFERENCES 216
CHAPTER 44. .6-FLUORENONE-.5-CYCLOPENTADIENYLIRON HEXAFLUOROPHOSPHATE 217
INTRODUCTION 217
PROCEDURE 218
DISCUSSION 218
REFERENCES 220
CHAPTER 45. Alkanediyl Complexes of Iron and Other Transition Metals 221
1. 1,4-Butanediylbis (cyclopentadienyliron dicarbonyl) 221
2. 1,4-Butanediylbis(manganese pentacarbonyl) 223
3. 1,4-Butanediylbis (cyclopentadienyltungsten tricarbonyl) 225
References 226
CHAPTER 46. .5-CYCLOPENTADIENYLDICARB0NYL (PHENYLTHIOCARBENIUM) IRON HEXAFLUOROPHOSPHATE 228
INTRODUCTION 228
PROCEDURE 229
PROPERTIES 230
REFERENCES 230
CHAPTER 47. LITHIUM CARBONYL (CARBOXYLATO) (CYCLOPENTADIENYL) (TRIPHENYLPHOSPHINE) FERRATE (l-)1 233
INTRODUCTION 233
PROCEDURE 233
PROPERTIES 234
REFERENCES 234
CHAPTER 48. POTASSIUM CARBONYL (CARBOXYLATO) (CYCLOPENTADIENYL) (TRIPHENYLPHOSPHINE) FERRATE (1-)1 235
INTRODUCTION 235
PROCEDURE 235
PROPERTIES 236
REFERENCES 236
CHAPTER 49. HYDROGEN CARBONYL (CARBOXYLATO) (CYCLOPENTADIENYL) (TRIPHENYLPHOSPHINE) FERRATE (1-)1 237
INTRODUCTION 237
PROCEDURE 237
PROPERTIES 238
REFERENCES 238
CHAPTER 50. DINUCLEAR CYCLOPENTADIENYLRUTHENIUM CARBONYL COMPLEXES 239
1. µ-METHYLENE-µ-CARBONYL-CARBONYL (ACETONITRILE)-bis-[(.-CYCLO-PENTADIENYL) RUTHENIUM] 239
2. µ-METHYLENE-µ-CARBONYL-µ-bis (DIPHENYLPHOSPHINO) METHANE-bis-[(.-CYCLOPENTADIENYL) RUTHENIUM] 240
3. µ-METHYL-µ-CARBONYL-µ-bis-(DIPHENYLPHOSPHINO) METHANE-bis-[(.- CYCLOPENTADIENYL) RUTHENIUM]-TETRAFLUOROBORATE 242
4. [µ-METHYLIDYNE-µ-CARBONYL-µ-bis-(DIPHENYLPHOSPHINO) METHANE-bis-[(.- CYCLOPENTADIENY) RUTHENIUM]-HEXAFLUOROPHOSPHATE 243
5. µ-ETHYLIDENE-µ-CARBONYL-µ-bis-[CARBONYL (.-PENTAMETHYLCYCLO-PENTADIENYL) RUTHENIUM] 245
6. µ-VINYLIDENE-µ-CARBONYL-µ-bis-[CARBONYL (.-PENTAMETHYLCYCLO-PENTADIENYL) RUTHENIUM] 247
7. µ-VINYL-µ-CARBONYL-µ-bis[CARBONYL (.-PENTAMETHYLCYCLOPENTA-DIENYL) RUTHENIUM]-TETRAFLUOROBORATE 248
CHAPTER 51. ENDO- AND EXO-.3-ALLYL (CARBONYL) (.5-CYCLOPENTADIENYL) RUTHENIUM 250
INTRODUCTION 250
PROCEDURE 250
PROPERTIES 251
REFERENCES 251
CHAPTER 52. COMPLEXES WITHIN THE (.5-C5Me5)Os(CO)(L)X FAMILY 252
SUMMARY 252
INTRODUCTION 252
CHAPTER 53. SYNTHESIS OF ACTIVATED CLUSTERS OF [M3(CO)12] (M=Ru or Os) 257
INTRODUCTION 257
PROCEDURE 257
PROPERTIES 258
PROPERTIES 259
PROPERTIES 260
REFERENCES 260
CHAPTER 54. THE CHEMICAL ACTIVATION OF THE CLUSTER [Os6(CO) 18]: SYNTHESIS OF [Os6(CO) 18-n (NCMe)n] (n=1 or 2) 261
INTRODUCTION 261
A. PREPARATION OF HEPTADECACARBONYL (ACETONITRILE) HEXAOSMIUM 261
B. PREPARATION OF HEXADECACARBONYLBIS (ACETONITRILE) HEXAOSMIUM 262
CHAPTER 55. HIGH YIELD SYNTHESES OF THE TRANSITION METAL CLUSTER SALTS [N(PPh3) 2]2 [M4 (µ-H)2(CO)12] (M=Ru or Os) 264
GENERAL INTRODUCTION 264
PROCEDURE 265
PROPERTIES 266
INTRODUCTION 267
PROCEDURE 267
PROPERTIES 268
ACKNOWLEDGEMENTS 269
REFERENCES 269
CHAPTER 56. HETERONUCLEAR TRANSITION METAL CLUSTER COMPOUNDS CONTAINING ONE OR TWO GOLD ATOMS 270
INTRODUCTION 270
PROCEDURE 271
PROPERTIES 272
PROCEDURE 273
PROPERTIES 274
ACKNOWLEDGEMENTS 275
REFERENCES 275
CHAPTER 57. NONACARBONYL-µ-HYDRIDO [µ3-.3-1,3 DIMETHYL 3 ALLENYL) Triangulo-TRIRUTHENIUM (3 Ru-Ru) and NONACARBONYL-µ-HYDRIDO (µ3-.3-1,3 DIMETHYL ALLYL) Triangulo TRIRUTHENIUM (3 Ru-Ru) 276
INTRODUCTION 276
PROCEDURE 276
PROPERTIES 277
REFERENCES 278
CHAPTER 58. NONACARBONYL-µ-HYDRIDO (µ3-.2-t-BUTYLETYNYL) Triangulo-TRIRUTHENIUM (3 Ru-Ru) SILVIO AIME, LUCIANO MILONE and DOMENICO OSELLA 279
INTRODUCTION 279
PROCEDURE 279
PROPERTIES 280
REFERENCES 280
CHAPTER 59. NONACARBONYL-µ-DIHYDRIDO (µ3-.2-2-PENTYNE) Triangulo-TRIRUTHENIUM (3 Ru-Ru) SILVIO AIME, ROBERTO GOBETTO and DOMENICO OSELLA 281
INTRODUCTION 281
PROCEDURE 281
PROPERTIES 282
REFERENCES 282
CHAPTER 60. OCTACARBONYL (µ3-.4-1-METHYL, 2-ETHYL, 3,4-DIPHENYL-BUTA-1,3-DIENE-l,4 DIYL) TRIRUTHENIUM (2 Ru-Ru) 283
INTRODUCTION 283
PROCEDURE 283
PROPERTIES 284
REFERENCES 284
CHAPTER 61. IODOTETRACARBONYLCOBALT MIKLÓS TASIa, TIBOR RANGA and GYULA PÁLYIb 285
INTRODUCTION 285
PROCEDURES 286
REFERENCES AND NOTES 287
CHAPTER 62. ALKOXYCARBONYLCOBALT TETRACARBONYLS MIKLÓS TASIa and GYULA PÁLYIb 289
INTRODUCTION 289
PROCEDURES 291
REFERENCES 292
CHAPTER 63. (µ2-DIPHOSPHORUS) HEXACARBONYLDICOBALT (Co-Co) AND DERIVATIVES ANNA VIZI-OROSZ, GYULA PÁLYIa, and LÁSZLÓ MARKÓb 295
INTRODUCTION 295
PROCEDURES 297
REFERENCES 299
CHAPTER 64. .5-METHOXYCARBONYLCYCLOPENTADIENYL-.4-1, 5-CYCLOOCTADIENECOBALT 301
INTRODUCTION 301
PROCEDURE 301
NOTES 302
PROPERTIES 302
REFERENCES 303
CHAPTER 65. C5H5CO [(NO)2 NORBORNENE], THE PRODUCT OF A THREE COMPONENT SYNTHESIS 304
INTRODUCTION 304
SYNTHESIS 304
PROPERTIES 305
SCOPE OF THE REACTION 305
REACTIONS OF C5H5Co [(NO)2olefin] 305
REFERENCES 305
CHAPTER 66. PREPARATION AND REACTIONS OF (µ-CARBONYL) BIS-(.5-CYCLOPENTADIENYL) (µ-.2-HEXAFLUOROBUT-2-YNE) DIRHODIUM 306
INTRODUCTION 306
PROCEDURE 306
SPECTROSCOPIC PROPERTIES 307
PROCEDURE 307
PROPERTIES 308
PROCEDURE 308
PROPERTIES 309
REFERENCES 310
CHAPTER 67. METHYL-TRIS (TRIPHENYLPHOSPHINE) COBALT 311
INTRODUCTION 311
PROCEDURE 311
PROPERTIES OF THE PRODUCT 312
REFERENCES 312
CHAPTER 68. HIGH OXIDATION STATE RHODIUM AND IRIDIUM ORGANOMETALLICS: COMPLEXES OF Rh(IV), Rh(V) AND Ir(V) 314
INTRODUCTION 314
REFERENCES 319
CHAPTER 69. 2-ARYL-2-KETOETHYLCOBALOXIMES AND TRIFLUOROMETHYLCOBALOXIMES 320
INTRODUCTION 320
TRIFLUOROMETHYLCOBALOXIMES 323
ACKNOWLEDGEMENT 326
REFERENCES AND NOTES 326
CHAPTER 70. ORGANOCOBALT CORRINS 327
ORGANOCOBALAMINS 328
ORGANOCOBINAMIDES 332
ORGANOCOBINAMIDES FROM ORGANOCOBALAMINS 334
TRIFLUOROMETHYLCOBALAMIN35 335
ACKNOWLEDGEMENT 337
REFERENCES AND NOTES 337
CHAPTER 71. RHODIUM (I) ARYLDIISOCYANIDE POLYMERS 339
EQUATION 339
INTRODUCTION 339
PROCEDURE 340
PROPERTIES 340
REFERENCES 341
Chapter 72. Preparation of Pentafluorophenyl Derivatives of Nickel, Cobalt, Iron, Palladium, and Platinum via the Corresponding Highly Reactive Metal Powder 342
Preparation of Metal Slurries 342
INTRODUCTION 343
EXPERIMENTAL PROCEDURES 344
LITERATURE REFERENCES 351
CHAPTER 73. BISLIGAND METALLACYCLOALKANES BY OXIDATIVE COUPLING OF ACTIVATED ALKENES WITH NICKEL (O), PALLADIUM (O) AND PLATINUM (O) COMPOUNDS 353
INTRODUCTION 353
A. BIS (DIMETHYLPHENYLPHOSPHINE)-5-PALLADA-3,3,7,7-TETRAMETHYL-ANTI-TRICYCLO [4.1.0.02,4] HEPTANE 354
B. BIS (DIMETHYLPHENYLPHOSPHINE)-3,3,6,6,9,9,13,13-OCTAMETHYL- 11-PALLADA-ANTI, SYN, ANTI, SYN-PENTACYCLO [10.1.0.02,4.05,7.08,10] TRIDECANE 356
C. BIS (TRIMETHYLPHOSPHINE)-5-PLATINA-3,3,7,7-TETRAMETHYL-ANTI-TRICYCLO [4.1.0.02,4] HEPTANE 357
D. 2,2'-BIPYRIDINE-3,4-BIS (METHYLENE) NICKELACYCLOPENTANE 358
E. 2,2'-BIPYRIDINE-4-NICKELA-DISPIRO [2.2.2.1.] NONANE 359
F. 1,2-BIS (DIMETHYLPHOSPHINO) ETHANE-4-NICKELA-DISPIRO [2.2.2.1.] NONANE 360
G. BIS (TRIMETHYLPHOSPHINE) (OCTA-1,7-DIENE-3,6-DIYL-1,8-DICARBOXYLIC ACID DIMETHYL ESTER) PLATINUM 361
REFERENCES 363
CHAPTER 74. YLIDE AND METHANIDE PENTAFLUOROPHENYL-GOLD (I) AND GOLD (III) COMPLEXES 365
GENERAL INTRODUCTION 365
1. Methyltriphenylphosphonium bromopentafluorophenylaurate (I) 367
2. Pentafluorophenyl (triphenylphosphonium-methylid) gold (I) 368
3. Chloro (triphenylphosphonium-methylid) gold (I) 369
4. Bis (diphenylphosphino) methanidegold (I) dimer 370
5. [Bis (diphenylphosphino) methanide gold (I)] pentafluorophenylgold (I) dimer 371
6. Chlorobis (pentafluorophenyl) [bis (diphenylphosphino) methane] gold (III) 372
7. Bis (pentafluorophenyl) [bis (diphenylphosphino) methane] gold (III) 373
8. Bis (pentafluorophenyl) [bis (diphenylphosphino) methanido] gold (III) 374
9. Bis {[µ-bis (diphenylphosphino) methanido] [bis (pentafluorophenyl)] gold (III)} gold (I) perchlorate 375
PART II: NONTRANSITION METAL ORGANOMETALLIC COMPOUNDS 377
CHAPTER 75. C,O-DILITHIO-ACETALDEHYDE OXIME MONCEF BELLASSOUED AND MARCEL GAUDEMAR 378
INTRODUCTION 378
PROCEDURE 378
PROPERTIES 378
REFERENCES 379
CHAPTER 76. 1-(TRIMETHYLSILYL) EPOXYETHYLLITHIUM 380
INTRODUCTION 380
PROCEDURE 381
REFERENCES 382
CHAPTER 77. 1-(DIETHOXYPHOSPHINYL) EPOXYETHYLLITHIUM 383
INTRODUCTION 383
PROCEDURE 383
PROPERTIES 384
REFERENCES 384
CHAPTER 78. 3,4-DILITHIO-2,5-DIMETHYL-2,4-HEXADIENE ADALBERT MAERCKER, RALF DUJARDIN, AND FRANZ BRAUERS 385
INTRODUCTION 385
STRUCTURE 387
PROPERTIES 388
REFERENCES 388
CHAPTER 79. CIS-1,2-DILITHIOCYCLOOCTENE ADALBERT MAERCKER, THOMAS GRAULE, AND ULRICH GIRRESER 389
INTRODUCTION 389
PROCEDURE 389
PROPERTIES 390
REFERENCES 390
CHAPTER 80. PHENYLSULFONYL (TRIMETHYLSILYL) METHYLLITHIUM 391
INTRODUCTION 391
PROCEDURE 391
PROPERTIES 392
REFERENCES 392
CHAPTER 81. (E)-1-(PHENYLSULFONYL)-2-(TRIMETHYLSILYL) VINYLLITHIUM AND (Z)-1-(PHENYLSULFONYL)-2-(TRIMETHYLSILYL) VINYLLITHIUM 393
INTRODUCTION 393
PROCEDURE A 393
PROPERTIES 394
REFERENCES 395
CHAPTER 82. 1-(PHENYLSULFONYL)-2-(TRIMETHYLSILYL) ETHYLLITHIUM AND 1-(PHENYLSULFONYL)-2-(TRIMETHYLSILYL) ETHYLIDENEDILITHIUM 396
INTRODUCTION 396
PROCEDURE A 396
PROCEDURE B 397
PROPERTIES 397
REFERENCES 398
CHAPTER 83. (Z)-1-(TRIMETHYLSILYL)-1,2-EPOXY-1-OCTYLLITHIUM 399
INTRODUCTION 399
PROCEDURE 399
PROPERTIES 400
REFERENCES 401
CHAPTER 84. DILITHIUM BIPHENYLIDE 402
INTRODUCTION 402
PROCEDURE 403
PROPERTIES 404
REFERENCES 404
CHAPTER 85. 1-(TRIPHENYLSILYL) EPOXYETHYLLITHIUM 405
INTRODUCTION 405
PROCEDURE 405
PROPERTIES 407
REFERENCES 407
CHAPTER 86. TRIS (TRIMETHYLSILYL) SILYLLITHIUM. 3THF 408
INTRODUCTION 408
PROCEDURE 409
PROPERTIES 409
REFERENCES 410
CHAPTER 87. BIS (BROMOMAGNESIO) METHANE 412
INTRODUCTION 412
PROCEDURE 413
PROPERTIES 413
REFERENCES 414
CHAPTER 88. l,3-BIS (BROMOMAGNESIO)-2,2-DIMETHYLPROPANE 415
INTRODUCTION 415
PROCEDURE 415
PROPERTIES OF THE PRODUCT 417
REFERENCES 417
CHAPTER 89. 1-MAGNESACYCLOBUTABENZENE 419
INTRODUCTION 419
PROCEDURE 419
PROPERTIES 420
REFERENCES 420
CHAPTER 90. DIETHYL-, DI-n-BUTYL- AND DI-n-OCTYLMAGNESIUM FROM MAGNESIUM, HYDROGEN AND 1-ALKENES 422
INTRODUCTION 422
PROCEDURES 423
PROPERTIES 425
REFERENCES 426
CHAPTER 91. ORGANOMAGNESIUM INNER COMPLEXES: BIS (3-N,N-DIMETHYL-AMINOPROPYL)-, BIS (4-N,N-DIMETHYLAMINOBUTYL)- AND BIS (4-METHOXYBUTYL) MAGNESIUM 427
INTRODUCTION 428
PROCEDURES 428
PROPERTIES 430
REFERENCES 431
CHAPTER 92. MAGNESIUM ANTHRACENE · 3THF 433
INTRODUCTION 433
PROCEDURE 433
REFERENCES 435
CHAPTER 93. CYANOMETHYLZINC BROMIDE NICOLE GOASDOUE AND MARCEL GAUDEMAR 437
INTRODUCTION 437
PROCEDURE 437
PROPERTIES 437
REFERENCES 438
CHAPTER 94. ETHOXYLCARBONYLMETHYLZINC BROMIDE 439
INTRODUCTION 439
PROCEDURE 439
PROPERTIES 439
REFERENCES 440
CHAPTER 95. .-FUNCTIONALLY SUBSTITUTED ORGANOZINC COMPOUNDS 441
INTRODUCTION 441
PREPARATION 441
PROPERTIES 442
REFERENCES 443
CHAPTER 96. CYCLOPENTADIENYLZINC-TRANSITION METAL COMPOUNDS 444
INTRODUCTION 444
PREPARATIONS 444
REFERENCES 447
CHAPTER 97. DI (CYCLOPENTADIENYL) COMPOUNDS OF GROUP IIB METALS 449
INTRODUCTION 449
PREPARATION 449
PROPERTIES 451
REFERENCES 452
CHAPTER 98. NIDO-2,3,4,5-TETRACARBAHEXABORANE (6) 453
INTRODUCTION 453
PROCEDURE 453
PROPERTIES 454
ACKNOWLEDGEMENTS 454
REFERENCES 455
CHAPTER 99. TRIETHYLBOROXIN 456
INTRODUCTION 456
PROCEDURE 457
PROPERTIES 458
REFERENCES 459
CHAPTER 100. 1,2:1,2-BIS (ETHYLBORANEDIYL) DIOXYFUMARATE 460
INTRODUCTION 460
PROCEDURE 461
PROPERTIES 461
REFERENCES 462
CHAPTER 101. 9-IODO-9-BORABICYCLO [3.3.1] NONANE 463
INTRODUCTION 463
PROCEDURE 464
PROPERTIES 464
REFERENCES 465
CHAPTER 102. BIS (DIETHYLBORYL) SULFATE 466
INTRODUCTION 466
PROCEDURE 467
PROPERTIES 467
REFERENCES 468
CHAPTER 103. METHYL 4,6-O-ETHYLBORANEDIYL-2,3-BIS-O-DIETHYLBORYL a-D-GLUCOPYRANOSIDE 469
INTRODUCTION 469
PROCEDURE 470
PROPERTIES 471
REFERENCES 472
CHAPTER 104. 9-METHANESULFONYLOXY-9-BORABICYCLO [3.3.1] NONANE (MSBBN) 473
INTRODUCTION 473
PROCEDURE 474
PROPERTIES 474
REFERENCES 475
CHAPTER 105. 2,3: 5,6-BIS-O-ETHYLBORANEDIYL-a-D-MANNOFURANOSYL BROMIDE 476
INTRODUCTION 476
PROCEDURE 477
PROPERTIES 478
REFERENCES 479
CHAPTER 106. 1,1,2,5-TETRAMETHYL-3,4-DIETHYL-1,2-DIHYDRO-1,3-STANNABOROLE 480
INTRODUCTION 480
PROCEDURE 481
PROPERTIES 482
REFERENCES 482
CHAPTER 107. 1,1: 2,2–BIS (1,5-CYCLOOCTANEDIYL) DIBOROXANE 483
INTRODUCTION 483
PROCEDURE 484
PROPERTIES 484
REFERENCES 485
CHAPTER 108. FLUORO (DIMESITYL) BORANE 486
INTRODUCTION 486
PROCEDURE 486
PROPERTIES 487
REFERENCES 487
CHAPTER 109. DIMESITYL (MESITYLETHYNYL) BORANE 488
INTRODUCTION 488
PROCEDURE 489
PROPERTIES 491
REFERENCES 491
CHAPTER 110. TRIMESITYLBORIRENE 492
INTRODUCTION 492
PROCEDURE 493
PROPERTIES 493
REFERENCES 494
CHAPTER 111. 1,2-BIS (DIBROMOALUMINO) ETHANE 495
INTRODUCTION 495
PROCEDURE 496
PROPERTIES 496
REFERENCES 497
CHAPTER 112. 1,1,2,2-TETRACHLORODIMETHYLDISILANE 498
INTRODUCTION 498
PROCEDURE 498
PROPERTIES 498
REFERENCES 499
CHAPTER 113. 1,1-DIMETHYL-1-SILACYCLOPENT-3-ENE 500
4.1 INTRODUCTION 500
4.2 PROCEDURE 501
4.3 PROPERTIES OF 1,1-DIMETHYL-1-SILACYCLOPENT-3-ENE 502
REFERENCES 502
CHAPTER 114. 3-SILABICYLO [3.2.1] OCTANE AND ITS 3-GERMA AND 3-STANNA ANALOGUES 506
INTRODUCTION 506
PROCEDURE 506
PROPERTIES 508
REFERENCES 509
CHAPTER 115. 1,1,2,2-TETRAMETHYL-1,2-DISILACYCLOPENTANE 510
INTRODUCTION 510
PROCEDURE 510
PROPERTIES 511
REFERENCES 511
CHAPTER 116. 1,1,2,2-TETRAMETHYL-l,2-DISILACYCLOHEXANE 512
INTRODUCTION 512
PROCEDURE 512
PROPERTIES 513
REFERENCES 513
CHAPTER 117. a-(TRIMETHYLSILYL) BENZYL ALCOHOL 514
INTRODUCTION 514
PROCEDURE 515
PROPERTIES 515
REFERENCES 516
CHAPTER 118. PHENYLSULFONYL (TRIMETHYLSILYL) METHANE 517
INTRODUCTION 517
PROCEDURE 517
PROPERTIES 518
REFERENCES 518
CHAPTER 119. 1,4-BIS [TRIMETHYLSILYL]-l,3-BUTADIYNE 519
INTRODUCTION 519
PROCEDURE 519
PROPERTIES 520
REFERENCES 521
CHAPTER 120. (Z)-1-(PHENYLSULFONYL)-2-(TRIMETHYLSILYL) ETHENE 522
INTRODUCTION 522
PROCEDURE 522
PROPERTIES 523
REFERENCES 523
CHAPTER 121. (E)-1-(PHENYLSULFONYL)-2-(TRIMETHYLSILYL) ETHENE 524
INTRODUCTION 524
PROCEDURE A 524
PROPERTIES 525
REFERENCES 526
CHAPTER 122. 1-(PHENYLSULFONYL)-2-(TRIMETHYLSILYL) ETHANE 527
INTRODUCTION 527
PROCEDURE 527
PROPERTIES 528
REFERENCES 528
CHAPTER 123. DODECAMETHYLCYCLOHEXASILANE 529
INTRODUCTION 529
PROCEDURE 529
PROPERTIES 530
REFERENCES 530
CHAPTER 124. 1,1-DIMETHYL-3-PHENYL-2-(TRIMETHYLSILYL)-1-SILACYCLOPROPENE 531
INTRODUCTION 531
PROCEDURE 531
PROPERTIES 532
REFERENCES 532
CHAPTER 125. (TRIMETHYLSILYL) DIPHENYLPHOSPHINE 534
INTRODUCTION 534
PROCEDURE 534
PROPERTIES 535
REFERENCES 536
CHAPTER 126. 1-METHYL-1-(TRIMETHYLSILYL) DIBENZOSILOLE 537
INTRODUCTION 537
PROCEDURE 537
PROPERTIES 538
REFERENCES 538
CHAPTER 127. THE SYNTHESIS OF R (+) or S (-) a-NAPHTHYLPHENYLMETHYLSILANE 539
INTRODUCTION 539
PROCEDURE 539
PROPERTIES 540
REFERENCES 541
CHAPTER 128. EPOXYETHYL (TRIPHENYL) SILANE 542
INTRODUCTION 542
PROCEDURE A 542
PROCEDURE B 543
PROPERTIES 543
REFERENCES 544
CHAPTER 129. (E)-1-OCTENYL (TRIPHENYL) SILANE 545
INTRODUCTION 545
PROCEDURE 546
PROPERTIES 547
REFERENCES 547
CHAPTER 130. 1,1-DIMESITYL-3-PHENYL-2-(TRIMETHYLSILYL)-1-SILACYCLOPROPENE 548
INTRODUCTION 548
PROCEDURE 548
PROPERTIES 549
REFERENCES 549
CHAPTER 131. 1,1-DIMETHYL-2,3,4,5-TETRAPHENYLSILOLE 550
INTRODUCTION 550
PROCEDURE 550
PROPERTIES 551
REFERENCES 551
CHAPTER 132. (E)-1,2-DIMESITYL-1,2-DI (t-BUTYL) DISILENE 552
INTRODUCTION 552
PROCEDURE 553
PROPERTIES 555
REFERENCES 556
CHAPTER 133. CHLOROTRIMETHYLGERMANE 557
INTRODUCTION 557
PROCEDURE 557
PROPERTIES 558
REFERENCES 558
CHAPTER 134. BIS (CHLOROMETHYL) DIMETHYLGERMANE 559
INTRODUCTION 559
PROCEDURE 559
PROPERTIES 560
REFERENCES 561
CHAPTER 135. 1,2-DICHLORO-1,1,2,2-TETRAMETHYLDIGERMANE 562
INTRODUCTION 562
PROCEDURE 562
PROPERTIES 563
REFERENCES 563
CHAPTER 136. MESITYLGERMANIUM CHLORIDES: MesGeCl3, Mes2GeCl2 , Mes3GeCl 565
INTRODUCTION 565
PROPERTIES 566
REFERENCES 567
CHAPTER 137. MESITYLGERMANIUM HYDRIDES: MesGeH3, Mes2GeH2, Mes3GeH 568
INTRODUCTION 568
PROCEDURE 568
PROPERTIES 570
REFERENCES 571
CHAPTER 138. 2,3,7,8-TETRAMETHYL-5-GERMASPIRO [4.4] NONA-2,7-DIENE 572
INTRODUCTION 572
PROCEDURE 572
PROPERTIES 573
REFERENCES 574
CHAPTER 139. TRICHLORO (2,4,6-TRI-TERT-BUTYLPHENYL) GERMANE 575
INTRODUCTION 575
PROCEDURE 575
PROPERTIES 576
REFERENCES 577
CHAPTER 140. TRIORGANOMETALLOMETHANES OF TIN AND LEAD 578
INTRODUCTION 578
PROCEDURE 578
PROPERTIES 580
REFERENCES 581
CHAPTER 141. BIS (TRIALKYLSTANNYL) ETHYNE 582
INTRODUCTION 582
PROCEDURE 583
PROPERTIES 584
REFERENCES 585
CHAPTER 142. 1.1-DIMETHYL-3-DIETHYLBORYL-4-ETHYL-1-STANNACYCLOPENTADIENE 586
INTRODUCTION 586
PROCEDURE 586
PROPERTIES 587
RFEERENCES 588
CHAPTER 143. 1-TRlMETHYLSILYL-3,4-BIS (TRIMETHYLSTANNYL)-3-DECEN-1-YNE: PREPARATION AND REACTIONS 589
INTRODUCTION 589
PROCEDURE 590
PROPERTIES 591
REFERENCES 592
CHAPTER 144. TRI-n-BUTYL ((E) -1-OCTENYL) TIN 593
INTRODUCTION 593
PROCEDURE 593
PROPERTIES 594
REFERENCES 594
CHAPTER 145. TRI-n-BUTYL ((E) -1,2-EPOXY-1-OCTYL) TIN 595
INTRODUCTION 595
PROCEDURE 595
PROPERTIES 596
REFERENCES 596
CHAPTER 146. TRIPHENYLTIN HYDROXIDE AND BIS (TRIPHENYLTIN) OXIDE 597
INTRODUCTION 597
PROCEDURE 597
PROPERTIES 598
REFERENCES 598
CHAPTER 147. TRIMETHYL (1-PROPYNYL) LEAD 599
INTRODUCTION 599
PROCEDURE 599
PROPERTES 600
REFERENCES 601
CHAPTER 148. DICHLOROBIS (TRIPHENYLPLUMBYL) METHANE 602
INTRODUCTION 602
PROCEDURE 602
PROPERTIES 603
REFERENCES 604
CHAPTER 149. TRIMETHYLARSINE 605
INTRODUCTION 605
PROCEDURE 605
PROPERTIES 607
REFERENCES 607
CHAPTER 150. DIBROMO (PHENYL) STIBINE 608
INTRODUCTION 608
PROCEDURE 608
PROPERTIES 609
REFERENCES 609
CHAPTER 151. DIMETHYL (p-TOLYLTELLURO) STIBINE 610
INTRODUCTION 610
PROCEDURE 610
PROPERTIES 611
REFERENCES 611
CHAPTER 152. PHENYLBIS (TRIMETHYLSILYL) STIBINE 612
INTRODUCTION 612
PROCEDURE 612
PROPERTIES 613
REFERENCES 613
CHAPTER 153. HEXAPHENYLCYCLOHEXASTIBINE 614
INTRODUCTION 614
PROCEDURE 614
PROPERTIES 614
REFERENCES 615
CHAPTER 154. TETRAMESITYLDISTIBINE 616
INTRODUCTION 616
PROCEDURES 616
PROPERTIES 618
REFERENCES 618
CHAPTER 155. DIPROPYL (p-TOLYLTELLURO) BISMUTH 619
INTRODUCTION 619
PROCEDURE 619
PROPERTIES 621
REFERENCES 621
CHAPTER 156. (2,2'-BIPHENYLYLENE) TRIPHENYLBISMUTH (5,5,5-TRIPHENYL-5H-DIBENZO-BISMOLE) 622
INTRODUCTION 622
PROCEDURE 622
PROPERTIES 623
REFERENCES 623
CHAPTER 157. BIS (2,2'-BIPHENYLYLENE) SELENIUM (5,5'-SPIROBI [DIBENZOSELENOPHENE]) 624
INTRODUCTION 624
PROCEDURE 624
PROPERTIES 626
REFERENCES 626
CHAPTER 158. BIS (3-CHLORO-2-PYRIDYL) DITELLURIDE 627
INTRODUCTION 627
PROCEDURE 627
PROPERTIES 628
REFERENCES 628
CHAPTER 159. TELLURANTHRENE 629
INTRODUCTION 629
PROCEDURE 629
PROPERTIES 630
REFERENCES 630
CHAPTER 160. BIS (2,2'-BIPHENYLYLENE) TELLURIUM (5,5'-SPIROBI [DIBENZOTELLURO-PHENE]) 631
INTRODUCTION 631
PROCEDURE 632
PROPERTIES 632
REFERENCES 633
INDEX OF METALS AND LIGANDS 634

Erscheint lt. Verlag	22.10.2013
Sprache	englisch
Themenwelt	Naturwissenschaften ► Chemie ► Anorganische Chemie
	Naturwissenschaften ► Chemie ► Organische Chemie
	Naturwissenschaften ► Chemie ► Physikalische Chemie
	Technik
ISBN-10	1-4832-9002-6 / 1483290026
ISBN-13	978-1-4832-9002-7 / 9781483290027

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