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Inorganic Syntheses, Volume 28, Reagents for Transition Metal Complex and Organometallic Syntheses

Robert J. Angelici (Editor-in-Chief)
ISBN: 978-0-471-52619-3
463 pages
December 1990
Inorganic Syntheses, Volume 28, Reagents for Transition Metal Complex and Organometallic Syntheses (0471526193) cover image
The volumes in this continuing series provide a compilation of current techniques and ideas in inorganic synthetic chemistry. Includes inorganic polymer syntheses and preparation of important inorganic solids, syntheses used in the development of pharmacologically active inorganic compounds, small-molecule coordination complexes, and related compounds. Also contains valuable information on transition organometallic compounds including species with metal-metal cluster molecules. All syntheses presented here have been tested.
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Chapter One COMPLEXES WITH WEAKLY COORDINATED LIGANDS.

1. Metal Complexes with Weakly Bonded Anions: General Considerations.

2. Carbonyl(η5-cyclopentadienyl) (tetrafluoroborato)molybdenum and -tungsten complexes: CpM(CO)2(L) (BF4) (M = Mo, W; L = CO, PPh3).

3. Pentacarbonyl(tetrafluoroborato)rhenium and -manganese and Reactions Thereof: M(CO)5(BF4) (M = Mn, Re).

4. Iridium(III) Complexes with the Weakly Bonded Anions [BF-4] and [OSO2CF-3].

5. cis-Chlorobis(triethylphosphine) (trifluoromethanesulnato)-platinum(II).

6. Tricarbonyltris(nitri1e) Complexes of Cr, Mo, and W: M(CO)3(NCEt)3 (M = Cr, Mo, W).

7. The Synthesis of Molybdenum and Tungsten Dinitrogen Complexes: MoCl4(L)2, MoCl3(L)3 (L = NCMe, THF), Mo(N2)2 (dppe)2, W(N2)2(dppe)2.

8. trans-Bis[ 1,2-ethanediylbis (diphenylphosphine)] bis-(isocyanomethane)tungsten(0): trans-[W(CNR)2(Ph2PCH2CH2PPh2)2].

9. Tricarbonyl(cycloheptatriene) molybdenum(0): Mo(CO)3(C7H8).

10. Tetracarbonyl(η2-Methyl Acry1ate)Ruthenium: Ru(CO)42-CH2 =C(H)(CO2Me)).

11. Reagents for the Synthesis of η-Diene Complexes of Tricarbonyliron and Tricarbonylruthenium.

12. Dihydridobis(solvent) bis(triphenylphosphine) iridium(III) Tetrafluoroborates: Ir(COD)(PPh3)+2, Ir(H)2(PPh3)2(L)+2 (L = acetone, H2O).

13. Bis(benzonitrile)dichloro Complexes of Palladium and Platinum: MCl2(NCPh)2 (M = Pd, Pt).

14. Acetonitrile Complexes of Selected Transition Metal Cations: Pd(NCMe)2+4, M(NO)2(NCMe)2+4 (M = Mo, W).

15. Tetrakis(acetonitrile)copper(l +) Hexafluorophosphate(1-): [Cu(NCMe)4]+.

16. Trifluoromethanesulfonates and Trifluoromethanesulfonato-O Complexes.

Chapter Two LOW-VALENT COMPLEXES OF Rh, Ir, Ni, Pd, and Pt.

17. Chlorotris(triphenylphosphine)rhodium(I) (Wilkinson's Catalyst): Rh(Cl)(PPh3)3.

18. trans-Carbonylchlorobis (triphenylphosphine)rhodium and Related Complexes: Rh(Cl)(CO)(PPh3)2.

19. Hydrido Phosphine Complexes of Rhodium(I): Rh(H)(PPh3)4, Rh(H)(CO)(PPh3)3.

20. Tetracarbonyldichlorodirhodium: [Rh(Cl)(CO)2]2.

21. Di-μ-chlorotetrakis(ethene) dirhodium(I): [Rh(Cl)(C2H4)2]2.

22. Di-μ-chloro-bis(η4-1,5-cyclooctadiene) dirhodium(I): [Rh(Cl)(COD)]2.

23. Chlorobis(cyclooctene)rhodium(I) and -iridium(I) Complexes: [M(Cl)(C8H14)2]2 (M = Rh, Ir).

24. trans-Carbonylchlorobis (triphenylphosphine) iridium: Ir(Cl)(CO)(PPh3)2.

25. Bis(1, 5-cyclooctadiene)nickel(0): Ni(COD)2.

26. Complexes of Nickel(0): Ni(CN-t-Bu)4, Ni(PPh3)4.

27. Tetrakis(triethyl phosphite) nickel(0), palladium(0), and platinum(0) Complexes: M[P(OEt)3]4.

28. Tetrakis(triphenylphosphine) palladium(0): Pd(PPh3)4.

29. Tetrakis(tert-butyl isocyanide)di-μ-chlorodipalladium(1): Pd(dba)2, Pd2Cl2(CN-t-Bu)4.

30. Two-Coordinate Phosphine Complexes of Palladium(0) and Platinum(0): M(PR3)2(M = Pd, Pt).

31. Three-Coordinate Phosphine Complexes of Platinum(0): Pt(PR3)3.

32. Tetrakis(triethylphosphine) platinum(0): Pt(PEt3)4.

33. Tris- and tetrakis(triphenylphosphine) platinum(0): Pt(PPh3)3,4.

34. Olefin Complexes of Platinum: Pt(COD)2, Pt(C2H4)3, Pt(C2H4)2(PR3).

35. Ethene Complexes of Bis(trialkylphosphine) platinum(0): Pt(C2H4)(PR3)2.

Chapter Three SUBSTITUTED METAL CARBONYL COMPLEXES.

36. (η6-Arene) tricarbonylchromium Complexes: Cr(η6-Arene)(CO)3.

37. Zero-Valent Isocyanide Complexes of Chromium, Molybdenum, and Tungsten: M(CO)x(CNR)6-x (M = Cr, Mo, W).

38. cis-Bis(diethyldithiocarbamato) dinitrosylmolybdenum, Dibromotetracarbonylmolybdenum(II), and Di- and Tricarbonylbis (diethyldithiocarbamato) molybdenum(II): Mo(Br)2(CO)4, Mo(CO)2,3 [S2CNEt2], Mo(NO)2[S2CNEt2]2.

39. Hexacarbonnylbis (η5-cyclopentadienyl) dichrominum, molybdenum, and tungsten and Their Analogs: M25-C5H4R)2(CO)6 (M = Cr, Mo, and W; R = H, Me, or PhCH2).

40. Cyclopentadienyl Metal Carbonyl Dimers of Molybdenum and Tungsten: [CpM(CO)3]2, [CpM(CO)2]2 (M = Mo, W).

41. Pentacarbonylmanganese Halides: Mn(CO)5X (X = Cl, Br, I).

42. Pentacarbonylrhenium Halides: Re(CO)5X (X = C1, Br, I).

43. Pentacarbonylhydridorhenium: Re(CO)5H.

44. Tetracarbonyliron(0) Complexes Containing Group V Donor Ligands: Fe(CO)4(PR3).

45. Bis(phosphine) Derivatives of Iron Pentacarbonyl and Tetracarbonyl (tri-tert-butylphosphine)iron(0): Fe(CO)3(PR3)2.

46. Zero-Valent Iron Isocyanide Complexes: Fe(CO)x(CNR)5-x.

47. Dicarbonyl(η5-cyclopentadienyl) (thiocarbonyl)iron(1+) Trifluoromethanesulfonate (1 - ) and Dicarbonyl(η5-

cyclopentadienyl) [methylthio)thiocarbonyl]iron: CpFe(CO)2(CS)+, CpFe(CO)2 [C( =S)SMe].

48. Tetracarbonylbis(η5-cyclopentadienyl) diruthenium: [CpRu(CO)2]2.

Chapter Four METAL CARBONYL ANION COMPLEXES.

49. Sodium Hexacarbonylniobate(1 - ): Nb(CO)-6.

50. Dicarbonyl(η5-cyclopentadieny1) nitrosyl Complexes of Chromium, Molybdenum, and Tungsten: CpM(CO)-3, CpM(CO)2(NO) (M = Cr, Mo, W).

51. Acetylpentacarbonylmanganese and Acetylpentacarbonylrhenium: M(CO)-5, M(CO)5[C(=O)Me] (M = Mn, Re).

52. Sodium Carbonyl Ferrates, Na2[Fe(CO)4], Na2[Fe2(CO)8], and Na2[Fe3(CO)11], Bis[μ-nitrido-bis(triphenylphosphorus) (l + )] Undecacarbonyltriferrate(2 - ), [(Ph3P)2N]2[Fe3(CO)11].

53. Dicarbonyl(η5-cyclopentadienyl) (2-methyl-l-propenyl-kC1)iron and Dicarbonyl(η5-cyclopentadienyl)(η2-2-methyl-l-propene)iron(l + ) Tetrafluoroborate(1 - ): CpFe(CO)-2, CpFe(CO)2[CH2=CMe2]+.

54. μ-Nitrido-bis(triphenylphosphorus)1( + ) Tetracarbonylrhodate(1 - ) and μ-Nitrido-bis(triphenylphosphorus) (1 + ) Tetracarbonyliridate(1 - ): [(Ph3P)2N] [M(CO)4] (M = Rh, Ir).

Chapter Five METAL CLUSTER COMPLEXES.

55. Polynuclear Ruthenium Complexes: Ru3(CO)12, H4Ru4(CO)12.

56. Tri- and Tetranuclear Carbonyl-Ruthenium Clusters Containing Isocyanide, Tertiary Phosphine and Phosphite Ligands. Radical Ion-Initiated Substitution of Metal Cluster Carbonyl Complexes Under Mild Conditions: Ru3(CO)12-x(L)x, H4Ru4(CO)12-x(L)x.

57. Dodecacarbonyltriosmium: OS3(CO)12.

58. Some Useful Derivatives of Dodecacarbonyltriosmium: Os3(CO)11(NCMe), Os3(CO)10(NCMe)2.

59. μ-Nitrido-bis(triphenylphosphorus) ( 1 + )μ-carbonyl- decacarbonyl-μ-hydridotriosmate(1 - ): HOs3(CO)-11.

60. Decacarbonyldi-μ-hydridotriosmium: Os3(μ-H)2(CO)10.

61. Dodecacarbonyltetra-μ-hydrido-tetrahedro-tetraosmium: H4Os4(CO)12.

62. Tri-μ-carbonyl-nonacarbonyltetrarhodium: Rh4(CO)12.

63. Dodecacarbonyltetrairidium: Ir4(CO)12.

Chapter Six CYCLOPENTADIENYL COMPLEXES.

64. Dicarbonylbis(η5-cyclopentadienyl) Complexes of Titanium, Zirconium, and Hafnium: Cp'2M(CO)2 (Cp' = C5H5, C5Me5; M = Ti, Zr, Hf).

65. (η5-Cyclopentadienyl) hydridozirconium Complexes: Cp2ZrH2, Cp2Zr(H)(Cl).

66. Cyclopentadienyl Complexes of Titanium(III) and Vanadium(III): Cp2MCl (M = Ti, V).

67. Vanadocene, Bis(η5-cyclopentadienyl)vanadium: Cp2V, V2(μ-Cl)3(THF)2+6.

68. Dichlorobis(η5-cyclopentadienyi)niobium(IV): Cp2NbCl2.

69. Chloro(η5-cyclopentadienyl) bis(triphenylphosphine) -ruthenium(II): RuCl(PPh3)25-C5H5).

70. (η5-Pentamethy1cyclopentadienyl) cobalt Complexes: Cp*Co(CO)2, Cp*Co(C2H4)2.

71. Cyclopentadienylbis (trimethy1phosphine) and Cyclopentadienylbis (trimethy1phosphite) Complexes of Co and Rh: CpM(PMe3)2, CpM[P(OMe)3]2, (M = Co, Rh).

Chapter Seven LANTHANIDE AND ACTINIDE COMPLEXES.

72. Lanthanide Trichlorides by Reaction of Lanthanide Metals with Mercury(II) Chloride in Tetrahydrofuran: LnCl3(THF)x.

73. (η5-Cyclopentadienyl)lanthanide Complexes from the Metallic Elements: Cp3Ln (Ln = Nd, Sm), Cp2,Y(DME).

74. Bis(η5-pentamethylcyclopentadienyl) bis(tetrahydrofuran)-samarium(II): Cp*2Sm(THF)2.

75. Chlorotris(η5-cyclopentadienyl) Complexes of Uranium(IV) and Thorium(IV): Cp3MCl (M = U, Th).

Chapter Eight LIGANDS AND OTHER TRANSITION METAL COMPLEXES.

76. Trimethylphosphine: PMe3.

77. Phosphorus Trifluoride: PF3.

78. Cyclopentadienylthallium: CpTl.

79. 1,2,3,4,5-Pentamethylcyclopentadiene: C5Me5H.

80. Anhydrous Metal Chlorides.

81. Tungsten and Molybdenum Tetrachloride Oxides: MOCl4 (M = Mo, W).

82. Tungsten Chloro Phosphine Complexes: WCl4(PR3)2,3, WCl2(PR3)4.

83. Tetrabutylammonium Octachlorodirhenate(III): Re2Cl2-8.

84. Di-μ-chloro-bis[ tricarbonylchlororuthenium(II)]: [Ru(CO)3Cl2]2.

85. Dihydridotetrakis (triphenylphosphine) ruthenium(II): H2Ru(PPh3)4.

86. Tris(2,2'-bipyridine)ruthenium(II) Dichloride Hexahydrate: Ru(bipy)2+3.

87. Dichlorobis[μ-methylenebis (diphenylphosphine)]-dipalladium(I) (Pd-Pd): Pd2(dppm)2Cl2.

88. (η3-Allyl)palladium(II) Complexes: (η3-C3H5)2Pd2Cl2, (η3-C3H5) (η5-C5H5)Pd.

89. Cyclic Diolefin Complexes of Platinum and Palladium: MCl2(COD) (M = Pd, Pt).

90. Potassium Trichloro(ethene) platinate(II) (Zeise's Salt): K[PtCl3(C2H4)].

Index of Contributors.

Subject Index.

Formula Index.

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