Inorganic Syntheses, Volume 27

ISBN-13: 9780471509769 / Angielski / Twarda / 1991 / 464 str.

Ginsberg; Alvin P. Ginsberg

Opis

This volume presents more than 200 checked procedures, bringing the total number of procedures covered by the series to over 3,000. The syntheses appear in 68 numbered sections, grouped into nine chapters that correspond to current areas of research. Noteworthy is the inclusion of syntheses of the early transition-metals polyoxoanions, a class of compounds notably difficult to prepare in pure form. The compounds synthesized are useful, not only to inorganic chemists, but to organic, polymer and solid state chemists, biochemists and materials scientists.

Spis treści

Chapter One TRANSITION METAL POLYHYDRIDE COMPLEXES.

1. Molecular Hydrogen Complexes of Mo and W.

2. Molybdenum and Tungsten Phosphine Polyhydrides.

3. Heptahydridobis (triphenylphosphine) rhenium(VII) and Octahydridotetrakis (triphenylphosphine) dirhenium(IV).

4. Tetrahydrid ( ⁵–pentamethylcyclopentadienyl) iridium.

5. Tris[1,3–bis(diphenylphosphino) propane]–heptahydridotriiridium(2 + ) Bis(tetrafluoroborate) and Bis[1,3–bis (diphenylphosphino) propane]–pentahydridodiiridium(1 + ) Tetrafluotoborate.

6. Heterobimetallic Hydride Complexes.

7. –Hydrido–tetrakis(tertiary phosphine) diplatinum Cations.

Chapter Two TRANSITION METAL CHALCOGENIDE COMPLEXES.

8. Tetraphenylphosphonium Salts of [Mo₂(S)_n(S₂)_6–n]^2– Thioanions and Derivatives.

9. Molybdenum–Sulfur Clusters.

10. Bis( ⁵–methylcyclopentadienyl) titanium Pentasulfide, Bis( ⁵–methylcyclopentadienyl) divanadium Pentasulfide, and

Bis( ₅–methylcyclopentadienyl) divanadium Tetrasulfide.

11. Cyclometallapolysulfanes (and Selanes) of Bis( ⁵–cyclopentadienyl) Titanium(IV), Zirconiurn(IV), Molybdenum(IV), and Tungsten(IV).

12. Bis(hydrogensulfido) Complexes of Bis( ⁵–cyclopentadienyl) Titanium(IV) and Tungsten(IV).

13. ( –Disulfido–S) ( –disulfido– ²: ²) Bis( ⁵–pentamethyl– cyclooentadienyl) ( –thio)dichromium (Cr–Cr).

Chapter Three EARLY TRANSITION METAL POLYOXOANIONS.

14. Introduction to Early Transition Metal Polyoxoanions.

15. Tetrabutylammoniurn Isopolyoxometalates.

16. , , and –Dodecatungstosilicic Acids: Isomers and Related Lacunary Compounds.

17. Vanadium(V) Substituted Dodecatungstophosphates.

18. Potassium Octadecatungstodiphosphates(V) and Related Lacunary Compounds.

19. The Aquatrihexacontaoxobis [trioxoarsenato(III)]– henicosatungstate(6–) Anion Isolated as the Acid or as the Rubidium Salt.

20. The Sodium Pentaphosphato(V) Triacontatungstate Anion Isolated as the Ammonium Salt.

21. Tetracontatungstotetraarsenate(III) and Its Cobalt(II) Complex.

22. Ammonium Sodium Henicosatungstononaantimonate(III), (NH₄)₁₈[NaSb₉W₂₁O₈₆] 24H₂O.

23. Bis( ₅–organophosphonato–O, O′, O") –penta– –oxo–pentakis (dioxomolybdates, –tungstates) (4–) (Pentametallobisphosphonates).

24. Tetrakis(tetrabutylammonium) ₃–[ ⁵–Cyclopentadienyl) –trioxotitanate(IV)] –A– –1, 2, 3 –trivanadononatungstosilicate(4–), [(C₄H₉)₄N]₄ [A– –( ⁵–C₅H₅) TiSiW₉V₃O₄₀]. 

Chapter Four LANTHANIDE AND ACTINIDE COMPLEXES.

25. Lanthanide Trichlorides by Reaction of Lanthanide Metals with Mercury(II) Chloride in Tetrahydrofuran.

26. Bis(phenylethynyl)ytterbium(II) from Ytterbium Metal and Bis(phenylethyny1)mercury.

27. Bis[bis(trimethylsilyl)amido] bis(diethyl ether)ytterbium and (Diethyl ether) bis( ⁵–pentamethylcyclopentadienyl) ytterbium.

28. Cyclooctatetraene lanthanide Complexes: Lu(C₈H₈)Cl(thf) and Lu(C₈H₈) [o–C₆H₄CH₂N(CH₃)₂](thf).

29. Bis( ⁵–pentamethylcyc1opentadienyl) bis(tetrahydrofuran)–samarium(II).

30. tert–Butylbis( ⁵–cyclopentadienyl) (tetrahydrofuran)–neodymium.

31. Bis( ⁵–cyclopentadienyl) (tetrahydrofuran)– [(trimethylsilyl)methyl] lutetium and Bis( ⁵–cyclopentadienyl)– (tetrahydrofuran)p–tolyllutetium.

32. Hydrocarbon–Soluble Homoleptic Bulky Aryl Oxides of the Lanthanide Metals: [Ln(OAr^R)₃].

33. Bis[ ⁵–1, 3–bis(trimethylsilyl)cyclopentadienyl]– chlorolanthanide(III) Complexes, [{ LnCp′′₂( –Cl)}₂] and [LnCp"₂( –Cl)₂Li(thf)₂].

34. Bis[ ⁵–1, 3–bis(trimethylsilyl) cyclopentadienyl] halouranium(IV) and –Thorium(IV), [MCp"₂Cl₂] and [UCp"₂X₂].

35. Tris( ⁵–cyclopentadienyl) [(dimethylphenylphosphoranylidene)– methyl] uranium(IV).

Chapter Five TRANSITION METAL CLUSTER COMPLEXES.

36. Tetrairon Carbido Carbonyl Clusters.

37. Tetraethylammonium Dodecacarbonyltricobaltferrate(1 – ) and (Triphenylphosphine)gold (1 + ) Dodecacarbonyl– tricobaltferrate(1 –).

38. Chiral Trinuclear NiCoMo and MoRuCo clusters.

39 . Nonacarbonyl–tri– –hydrido– ₃–methylidyne–triruthenium and –osmium.

40. Anionic and Heteronuclear Triosmium Clusters.

41. Hexachlorododecakis (triphenylphosphine)– pentapentacontagold, Au₅₅[P(C₆H₅)₃]₁₂Cl₆.

42. A Platinum–Gold cluster: Chloro–1k Cl–bis(triethy1phosphine–1kP) bis(triphenylphosphine)–2kP, 3kP–triangulo– digoldplatinurn (1 + ) Trifluoromethanesulfonate.

Chapter Six PHOSPHORUS COMPLEXES AND COMPOUNDS.

43. Chloro( ²–tetrahedro–tetraphosphorus) bis(triphenyIphosphine)–rhodium(I).

44. Tetracarbonyl bis( ⁵–cyclopentadienyl) ( – ²–diphosphorus)– dimolybdenum(I) and Dicarbonyl ( ⁵–cyclopentadienyl)– ( ³–cyclo– triphosphorus) molybdenum(I)

45. Trilithium Heptaphosphide, Dilithiun Hexadecaphosphide, and Trisodium Henicosaphosphide.

46. Phosphorus Compounds Containing Sterically Demanding Groups.

47. Compounds with Unsupported P=P Bonds.

48. Tris(trimethylsily) phosphine and Lithium Bis(trimethylsilyl) –phosphide.bis(tetrahydrofuran).

49. (2,2–Dimethylpropylidyne)phosphine.

50. Triphosphenium Salts.

51. cis–1, 3–Di–tert–butyl–2, 4–dichloro–3, 2, 4–diazadiphosphetidine.

Chapter Seven TRANSITION METAL COMPLEXES OF BIOLOGICAL INTEREST.

52. Reversible Cobalt(II) and Iron(II) Dioxygen Carriers of Totally Synthetic Lacunar Cyclidene Complexes.

53. [Pt(1, 2–Cyclohexanediamine) (ascorbato–C², O⁵)].

Chapter Eight MISCELLANEOUS TRANSITION METAL COMPLEXES.

54. (Dithiocarbonato) [1, 1, l–tris(diphenylphosphinomethyl) ethane]–rhodium(III) Tetraphenylborate Solvate.

55. The Vaska–Type Rhodium Complexes, trans–RhX(CO)L2.

56. Potassium Hexaiodorhenate(IV).

57. Group 6 Pentacarbonyl Acetates as Their –Nitridobis(triphenylphosphorus)( 1 + ) Salts.

58. Bis(organoimido) Complexes of Tungsten(VI).

59. Relatively Air–Stable M(II) Saccharinates, M = V or Cr.

60. Pyridinium Fluorotrioxochromate(VI), (C₅H₅NH)[CrO₃F].

61. Dipotassium Trifluorosulfatomanganate(III).

62. cis–Dichlorobis (1,2–ethanediamine) platinurn(IV) Chloride.

63. Bis(1, 1, 1, 5, 5, 5–hexafluoro–2,4–pentanedionato) palladium and Its Complexes with 2, 2′–Bipyridine and Bis[2–(diphenylphosphino)ethyl] phenylphosphine.

Chapter Nine LIGANDS AND OTHER MAIN GROUP COMPOUNDS.

64. Hybrid Tertiary Phosphine Amine and Amide Chelate Ligands: N–[2–(diphenylphosphino)phenyl] benzamide and 2–(Diphenylphosphino)–N–phenylbenzamide.

65. 1, 1–Dimethyl–N–(trimethy1silyl)ethanamine.

66. Ethynylpentafluoro– ⁶–sulfane (SF₅C triplebond CH).

67. Iodine and Bromine Polysulfur Hexafluoroarsenate(V) and Hexafluoroantimonate(V).

68. Trimethylborane.

Sources of Chemicals and Equipment.

Index of Contributors.

Subject Index.

Formula Index.