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Inorganic Syntheses, Volume 29

Russell N. Grimes (Editor-in-Chief)
ISBN: 978-0-471-54470-8
456 pages
September 1992
Inorganic Syntheses, Volume 29 (0471544701) 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 MAIN-GROUP COMPOUNDS-GENERAL.

1. Xenon Difluoride.

2. Xenon Tetrafluoride.

3. Chlorine Pentafluoride.

4. Dioxygenyl Hexafluoroarsenate.

5. Peroxydisulfuryl Difluoride.

6. Krypton Difluoride.

7. Simple Preparation of Benzenethiolato and Benzeneselenolato Derivtives of Indium and Tin.

8. Tetrakis (2,4,6-trimethylpheny1)disilene (Tetramesityldisilene).

9. Monoorganotin Phosphinate Clusters: The Oxygen-Chpped Cluster [(n-BuSn(OH)O2PPh2)3O] [Ph2PO2] (1) and Its Conversion to the Cubic Cluster [n-BuSn(O)O2PPh2]4 (2).

10. (Tripheny1phosphoranylidene)sulfamoyl Chloride, Ph3PNSO2Cl.

11. Hexamethyldisilathiane, Me3Si-S-SiMe3.

12. Addition of Sulfur Trioxide to Pentafluorothio (SF5) (Pentafluoro-Λ6-Sulfanyl) Containing Fluoroolefins.

13. Pentafluoro(isocyanato)-λ6-Sulfane (SF5N=C=O).

14. Ambient-Pressure Superconducting Synthetic Metals β-(BEDT-TTF)2X, X = I-3; IBr-2, and AuI-2.

Chapter Two BORON COMPOUNDS.

15. Trimethylamine-tribromoborane, Me3N-BBr3.

16. 1,4-Di-tert-butyl-2,6-diisopropyl-3,5-bis(trimethylsilyl)-3,5-diaza-nido-hexaborane(6) (Me3Si)2N2B4(t-Bu)2(i-Pr)2.

17. Polycyclic Borazines.

18. 1,5-Cyclooctanediylborylsulfides.

19. 1,5-Cyclooctanediylborylselenides.

20. Trimethylamine-Diethyl-l-propynylborane and Diethyl-l-propynylborane, Me3,N-Et2BC triple bond CMe and Et2BC triple bond CMe.

21. Pentaethyl- 1,5-dicarba-closo-pentaborane(5) and Decaethyl-2,6,8,10-tetracarba-nido-decaborane1(10).

22. Trimethylsilyl-Substituted Derivatives of 2,3-Dicarba-nido-hexaborane(8) and Lithium, Sodium, and Dilithium Salts of the Carborane Dianion 2,3-Bis(trimethylsilyl)-2,3-dicarba-nido-hexaborate(2 - ).

23. 1,2-(1,2-Ethanyldiyl)-1,2-dicarbadodecaborane(12) (1,2-Ethano-o-carborane).

24. 7,9-Diselena-nido-undecaborane(9), B9H9Se2.

25. 6.9-Diselena-arachno-decaborane(10), B8H10Se2.

Chapter Three TRANSITION METAL COORDINATION COMPOUNDS.

26. Solvated and Unsolvated Anhydrous Metal Chlorides from Metal Chloride Hydrates.

27. Solid Solvates: The Use of Weak Ligands in Coordination Chemistry.

28. Niobium(III) and (IV) Halide Complexes.

29. Chromium(V) Fluoride and Chromium(VI) Tetrafluoride Oxide.

30. Ammonium Hexachloromolybdate(III).

31. Dioxobis(2,4-pentanedionato)molybdenum(VI), MoO2(acac)2, and μ-Oxodioxotetrakis (2,4-pentanedionato) dimolybdenum(V),Mo2O3(acac)4.

32. Decakis(acetonitrile)dimolybdenum(II) Tetrafluoroborate(1-), [Mo2 (NCMe)8(ax-meCN)0.5] [BF4]4.

33. Hexakis(dimethy1amido)ditungsten and Tungsten(IV) Chloride.

34. Tetracarbonyl[1,2-ethanediylbis (diphenylphosphine)] tungsten(0), fac-(Acetone)tricarbonyl [1,2-ethanediylbis (diphenylphosphine)] tungsten(0), and mer-Tricarbonyl [1,2-ethanediylbis(diphenylphosphine)] (phenylvinylidene)tungsten(0).

35. Nitrido and Oxo Complexes of Rhenium(V).

36. trans-Tricarbonylbis(phosphine)iron(0) Complexes: One-Pot Syntheses from Pentacarbonyliron.

37. Dicarbonyl-cis-dihydrido-trans-bis(phosphite)iron(II) Complexes: One-Pot Syntheses from Pentacarbonyliron.

38. Thionitrosyl Complexes of Ruthenium(II).

39. trans-Dichlorotetramine Complexes of Ruthenium(III).

40. trans-Dichlorobis (1,2-ethanediamine) cobalt(III) Chloride.

41. Resolution of the Dodecaamminehexa-μ-hydroxo-tetracobalt(III) Ion.

42. Tricarbonyl Phosphine, Phosphite, and Arsine Derivatives of Cobalt(I).

43. Decakis(acetonitrile)dirhodium(II) Tetrafluoroborate, [Rh2(NCMe)10] [BF4]4.

44. (2,2'-Bipyridine)dichloropalladium(II) and [N'-(2-Diaminoethyl)-1,2-ethanediamine] chloropalladium(II) Chloride.

45. trans-Dicarbonyl-di-β-iodo-diiododiplatinum(II), Pt2I4(CO)2.

46. Chlorohydridobis (trialkylphosphine) platinum(II) Complexes.

Chapter Four TRANSITION METAL ORGANOMETALLICS AND LIGANDS.

47. Large-Scale Syntheses of 1,2,3,4,5-Pentamethylcyclopentadiene.

48. Dichlorobis(η5-chlorocyclopentadienyl) titanium, (ClC5H4)2TiCl2.

49. η3-Allylhydridobis [ethylenebis(diphenylphosphine)]- molybdenum(II), MoH(η3-C3H5) [Ph2PCH2CH2PPh2]2.

50. Bis(η-cyclopentadienyl) molybdenum(IV) Complexes.

51. Cyclopentadienyl Rhenium Complexes.

52. Di-μ-chloro-bis [(η5-pentamethylcyclopentadienyl) chloro-ruthenium(III), [Cp*RuCl2]2 and Di-μ-methoxo-bis [(η-pentamethylcyclopentadienyl) diruthenium(II)], [Cp*RuOMe]2.

53. (η5-Pentamethylcyclopentadienyl) rhodium and -Iridium Compounds.

54. Bis(η5-cyclopentadienyl) bis(diethylamido) uranium(IV) and Tris(η5-cyclopentadienyl) (diethylamido)uranium(IV).

Chapter Five CLUSTER AND CAGE COMPOUNDS CONTAINING TRANSITION METALS.

55. Disodium tris(tetrabuty1ammonium) [β-hexatricontaoxo- (μ12-tetraoxosilicato) (10,11,12-triniobiumnonatungsten) ato-(7-)] (η5-pentamethylcyclopentadienyl) rhodate(5-), Na2(Bu4N)3 [Rh[β-Nb3SiWO40] (η5-C5Me5)].

56. η5-Cyclopentadienylchromium Complexes of Phosphorus, Tetracarbonyl-μ-Diphosphido-bis(η5-cyclopentadienylchromium), [CpCr(CO2)]2 (μ-η2-P2) and Dicarbonylcyclotriphosphido- (η5-cyclopentadienylchromium), CpCr(CO)23-P3).

57. η5-Cyclopentadienylchromium Complexes of Sulfur.

58. Sulfur-Bridged Dinuclear Molybdenum(V) Complexes with Mo2O3S and Mo2O2S2 Cores.

59. Sulfur-Bridged Cubane-Type (Mo4S4) and Incomplete Cubane - Type (Mo3O4-nSn; n = 1-4) Molybdenum Aqua Ions.

60. Preparation of Dinuclear and Trinuclear Ferraboranes, Fe2(CO)6B2H6 and Fe3H(CO)10BH2.

61. Preparation of the Metal and Hydrogen Rich Ferraborane, Fe3H(CO)9BH4.

62. Tetraammonium Hexakis [tetraethyl-2,3-dioxobutane-1,1,4,4-tetracarboxylato (2-)-O1', O2:O3,O4']tetrametalate(4-).

63. Mixed-Metal-Gold Phosphine Cluster Compounds.

Index of Contributors.

Subject Index.

Formula Index.

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