New procedures and compounds for students and professionals in the field of inorganic chemistry The Inorganic Syntheses series provides all users of inorganic substances with detailed and foolproof procedures for the preparation of important and timely compounds. In Volume 33, editor Dimitri Coucouvanis collects syntheses that present new or revised experimental procedures that are applicable to a variety of related compounds, as well as syntheses of individual compounds that are of interest or importance. Chapter topics are comprised of syntheses of selected supramolecules, useful…mehr
New procedures and compounds for students and professionals in the field of inorganic chemistry The Inorganic Syntheses series provides all users of inorganic substances with detailed and foolproof procedures for the preparation of important and timely compounds. In Volume 33, editor Dimitri Coucouvanis collects syntheses that present new or revised experimental procedures that are applicable to a variety of related compounds, as well as syntheses of individual compounds that are of interest or importance. Chapter topics are comprised of syntheses of selected supramolecules, useful reagents/ligands, solid state materials/clusters, and compounds of general interest, including mesityl-gold (I)complexes and zero valent binuclear nickel complexes, among many others All the syntheses presented have been tested. Inorganic, organic, and organometallic chemists, as well as materials scientists, instructors, and graduate students will find the research, methods, and compounds contained here invaluable to their scientific pursuits.Hinweis: Dieser Artikel kann nur an eine deutsche Lieferadresse ausgeliefert werden.
DIMITRI COUCOUVANIS, PhD, is Professor of Chemistry at the University of Michigan.
Inhaltsangabe
Chapter One SYNTHESES OF SELECTED SUPRAMOLECULES. 1. Toward Magnetic Building Blocks: Synthesis of a Planar Co(III)-cation Radical-cobalt(III) Complex of the Binucleating Ligand 1,2,4,5-Tetrakis(2-hydroxy-2-methylpropanamido)benzene. 2. A Luminescent Decanuclear Ruthenium(II) Polypyridine Complex: A Convergent Approach to a Dendritic Structure Employing the "Complexes as Metals/Complexes as Ligands" Synthetic Strategy. 3. Dodecatungstoaluminic Acid and Its Monolacunary and Mixed-Addendum Derivatives. 4. Supramolecular Complexes of BisBis(2,2'-bipyridine)osmium(II) and Ruthenium(II). 5. Binuclear Oxomolybdenum-Metalloporphyrin Complexes. 6. Iron Sandwich Polyoxoanion Compounds. 7. Dipyrryl and Porphyrinic Precursors to Supramolecular Conjugated (Porphinato)metal Arrays: Syntheses of Dipyrrylmethane and (5,15-diphenylporphinato)zinc(II). 8. Synthesis of Dodecaoxohexadecacarboxylatotetraaquo-dodecamanganese [Mn 12O12(O2CR)16(H2O)4] (R = Me,Et,Ph,Cr) Complexes. 9. Use of Picolinehydroximate Complexes in Preparation of Uranyl and Lanthanide 15-Metallacrown-5: UO2(NO3)2 [15-MCCu(II)N(pic)-15] and {Eu(NO3 )2[15-MCCu(II)N(pic)-15]}NO3. 10. Use of Salicyl- and Naphthoylhydroximate Complexes in Preparation of Manganese and Copper 12-Metallacrown-4 Complexes: Mn(II)(Acetate)2 [Mn(III)(salicylhydroximate)]4 and (Tetramethylammonium)2 [Cu(II)5 (naphthoylhydroximate)4]. Chapter Two USEFUL REAGENTS AND LIGANDS. 11. Homoleptic Transition Metal Acetonitrile Cations with Tetrafluoroborate or Trifluoromethanesulfonate Anions. 12. Synthesis of [MII(NCMe)6]2+ (M = V,Cr,Mn,Fe,Co,Ni) Salts of Tetra[3,5-bis(trifluoromethyl)phenyl]borate. 13. Transition Metal p-Toluenesulfonates. 14. Salts of Binuclear Iron(II) and Iron(III) Dianions [(Fe2Cl6)2- and (Fe 2OCl6)2-]. 15. Tetraethylammonium-Tetrathioperrhenate Et4N(ReS4). 16. Large-Scale Synthesis of Methyltrioxorhenium (CH3ReO3). 17. 4,5-Diaminocatechol: A Useful Building Block in Synthesis of Multimetallic Complexes. 18. A Convenient Synthesis of 1,5,9-Trithiacyclododecane (S3C9H18). Chapter Three SOLID-STATE MATERIALS AND CLUSTERS. 19. Synthesis of Quaternary Selenophosphates using Molten Salt Fluxes: Rb8 Hg4(Se2)2(PSe4)4, K4In2(PSe5)2(P2Se6), Rb4Ti2(P2Se7)(P2Se9)2, Rb4U4(Se)2 (Se2)4(PSe4)4. 20. Hydrothermal Synthesis of Sulfosalts: Ag3AsS3, Ag3SbS3, Ag7SbS6, Cu12 Sb4S13, CuInS2, FeIn2S4. 21. Open-Framework Solids of the Vanadium Oxide-Phosphate System. 22. Sulfur-Bridged Incomplete Cubane-Type Molybdenum and Tungsten Aqua Ions. 23. Sulfur-Bridged Cubane Type Mixed-Metal Clusters with Mo3MS4 (M = Fe,Co,Ni,Cu,In,Sn) and W3NiS4 Cores. 24. Molybdenum and Tungsten Clusters as Aqua Ions [M3Q4(H2O)9]4+ (M = Mo,W; Q = S,Se) and Related Chalcogen-Rich Trinuclear Clusters. Chapter Four COMPOUNDS OF GENERAL INTEREST. 25. The Diphenylmethylenethiophosphinate (MTP) Ligand in Gold(I), Platinum(II), Lead(II), Thallium(I), and Mercury(II) Complexes, sym-Au2 (MTP)2, (PPN)[Au(MTP)2], Au2Pt(MTP)4, Au2Pb(MTP)4, AuTl(MTP)4, Hg(MTP)2, Hg(MTP)2(AuCl)2, and HgIIAuI(MTP)2AuIIICl4. 26. Mesityl-gold(I) Complexes. 27. An Improved Synthesis of cis -Dithiocyanato-bis(4,4'-dicarboxy-2,2'-bpy) Ru(II) Sensitizer. 28. Dimethylsulfoxide Complexes of Platinum(II): K[PtCl3(Me2SO)], cis -[PtCl2L(Me2SO)] (L = Me2SO,MeCN), [PtCl( -Cl)(Me2SO)]2, and [Pt(Me2SO)4 ](CF3SO3)2. 29. Tetrasulfur-tetranitride (S4N4). 30. Hydrotris(methimazolyl)borate. 31. Arsenic(III)bromide. 32. Dichlorodioxo-bis(triphenylphosphine oxide)uranium(VI) [UO2Cl2(OPPh3)2 ]. 33. Chlorohydro-tris(pyrazol-1-yl)borato-bis(triphenylphosphine) ruthenium(II) {RuCl[k3-HB(pz)](PPh3)2} (pz = pyrazol-1-yl). 34. Octacarbonyl-di- -hydridodirhenium [Re2( -H)2(CO)8]. 35. Zero-Valent Binuclear Nickel Complexes. 36. Preparation of a Synthetic Ribonuclease: The Europium(III) Complex of 1-(4-nitrobenzyl)-4,7,10-Tris(carbamoylmethyl)-1,4,7,10- tetraazacyclododecane. 37. Carbonyl Halide Tungsten(II) Complexes of Tris(3,5-dimethylpyrazolyl)hydroborate. 38. A Luminescent Complex of Re(I): fac-[Re(CO)3(bpy)(py)](CF3SO3) (bpy = 2.2'-bipyridine; py = pyridine). 39. RSi(OH)3 and RSi(NH2)3 [R = 2,6-iPr2C6H3N(SiMe3)]: Synthesis of Stable Organosilanes with Three Functional Groups. 40. Fluorination with Me3SnF: Synthesis of Cyclopentadienyl-Substituted Group 4 Metal Fluoride Complexes. 41. Seven-Coordinate [MI2(CO)3(NCMe)2], [MI2(CO)3(NCMe)(PPh3)], and Alkyne [MI2(CO)(NCMe)( 2-RC2R)2] Complexes of Molybdenum(II) and Tungsten(II). 42. Chlorothiocarbonyl-bis(triphenylphosphine)iridium(I) [IrCl(CS)(PPh3)2 ]. Contributor Index. Subject Index. Formula Index.
Chapter One SYNTHESES OF SELECTED SUPRAMOLECULES. 1. Toward Magnetic Building Blocks: Synthesis of a Planar Co(III)-cation Radical-cobalt(III) Complex of the Binucleating Ligand 1,2,4,5-Tetrakis(2-hydroxy-2-methylpropanamido)benzene. 2. A Luminescent Decanuclear Ruthenium(II) Polypyridine Complex: A Convergent Approach to a Dendritic Structure Employing the "Complexes as Metals/Complexes as Ligands" Synthetic Strategy. 3. Dodecatungstoaluminic Acid and Its Monolacunary and Mixed-Addendum Derivatives. 4. Supramolecular Complexes of BisBis(2,2'-bipyridine)osmium(II) and Ruthenium(II). 5. Binuclear Oxomolybdenum-Metalloporphyrin Complexes. 6. Iron Sandwich Polyoxoanion Compounds. 7. Dipyrryl and Porphyrinic Precursors to Supramolecular Conjugated (Porphinato)metal Arrays: Syntheses of Dipyrrylmethane and (5,15-diphenylporphinato)zinc(II). 8. Synthesis of Dodecaoxohexadecacarboxylatotetraaquo-dodecamanganese [Mn 12O12(O2CR)16(H2O)4] (R = Me,Et,Ph,Cr) Complexes. 9. Use of Picolinehydroximate Complexes in Preparation of Uranyl and Lanthanide 15-Metallacrown-5: UO2(NO3)2 [15-MCCu(II)N(pic)-15] and {Eu(NO3 )2[15-MCCu(II)N(pic)-15]}NO3. 10. Use of Salicyl- and Naphthoylhydroximate Complexes in Preparation of Manganese and Copper 12-Metallacrown-4 Complexes: Mn(II)(Acetate)2 [Mn(III)(salicylhydroximate)]4 and (Tetramethylammonium)2 [Cu(II)5 (naphthoylhydroximate)4]. Chapter Two USEFUL REAGENTS AND LIGANDS. 11. Homoleptic Transition Metal Acetonitrile Cations with Tetrafluoroborate or Trifluoromethanesulfonate Anions. 12. Synthesis of [MII(NCMe)6]2+ (M = V,Cr,Mn,Fe,Co,Ni) Salts of Tetra[3,5-bis(trifluoromethyl)phenyl]borate. 13. Transition Metal p-Toluenesulfonates. 14. Salts of Binuclear Iron(II) and Iron(III) Dianions [(Fe2Cl6)2- and (Fe 2OCl6)2-]. 15. Tetraethylammonium-Tetrathioperrhenate Et4N(ReS4). 16. Large-Scale Synthesis of Methyltrioxorhenium (CH3ReO3). 17. 4,5-Diaminocatechol: A Useful Building Block in Synthesis of Multimetallic Complexes. 18. A Convenient Synthesis of 1,5,9-Trithiacyclododecane (S3C9H18). Chapter Three SOLID-STATE MATERIALS AND CLUSTERS. 19. Synthesis of Quaternary Selenophosphates using Molten Salt Fluxes: Rb8 Hg4(Se2)2(PSe4)4, K4In2(PSe5)2(P2Se6), Rb4Ti2(P2Se7)(P2Se9)2, Rb4U4(Se)2 (Se2)4(PSe4)4. 20. Hydrothermal Synthesis of Sulfosalts: Ag3AsS3, Ag3SbS3, Ag7SbS6, Cu12 Sb4S13, CuInS2, FeIn2S4. 21. Open-Framework Solids of the Vanadium Oxide-Phosphate System. 22. Sulfur-Bridged Incomplete Cubane-Type Molybdenum and Tungsten Aqua Ions. 23. Sulfur-Bridged Cubane Type Mixed-Metal Clusters with Mo3MS4 (M = Fe,Co,Ni,Cu,In,Sn) and W3NiS4 Cores. 24. Molybdenum and Tungsten Clusters as Aqua Ions [M3Q4(H2O)9]4+ (M = Mo,W; Q = S,Se) and Related Chalcogen-Rich Trinuclear Clusters. Chapter Four COMPOUNDS OF GENERAL INTEREST. 25. The Diphenylmethylenethiophosphinate (MTP) Ligand in Gold(I), Platinum(II), Lead(II), Thallium(I), and Mercury(II) Complexes, sym-Au2 (MTP)2, (PPN)[Au(MTP)2], Au2Pt(MTP)4, Au2Pb(MTP)4, AuTl(MTP)4, Hg(MTP)2, Hg(MTP)2(AuCl)2, and HgIIAuI(MTP)2AuIIICl4. 26. Mesityl-gold(I) Complexes. 27. An Improved Synthesis of cis -Dithiocyanato-bis(4,4'-dicarboxy-2,2'-bpy) Ru(II) Sensitizer. 28. Dimethylsulfoxide Complexes of Platinum(II): K[PtCl3(Me2SO)], cis -[PtCl2L(Me2SO)] (L = Me2SO,MeCN), [PtCl( -Cl)(Me2SO)]2, and [Pt(Me2SO)4 ](CF3SO3)2. 29. Tetrasulfur-tetranitride (S4N4). 30. Hydrotris(methimazolyl)borate. 31. Arsenic(III)bromide. 32. Dichlorodioxo-bis(triphenylphosphine oxide)uranium(VI) [UO2Cl2(OPPh3)2 ]. 33. Chlorohydro-tris(pyrazol-1-yl)borato-bis(triphenylphosphine) ruthenium(II) {RuCl[k3-HB(pz)](PPh3)2} (pz = pyrazol-1-yl). 34. Octacarbonyl-di- -hydridodirhenium [Re2( -H)2(CO)8]. 35. Zero-Valent Binuclear Nickel Complexes. 36. Preparation of a Synthetic Ribonuclease: The Europium(III) Complex of 1-(4-nitrobenzyl)-4,7,10-Tris(carbamoylmethyl)-1,4,7,10- tetraazacyclododecane. 37. Carbonyl Halide Tungsten(II) Complexes of Tris(3,5-dimethylpyrazolyl)hydroborate. 38. A Luminescent Complex of Re(I): fac-[Re(CO)3(bpy)(py)](CF3SO3) (bpy = 2.2'-bipyridine; py = pyridine). 39. RSi(OH)3 and RSi(NH2)3 [R = 2,6-iPr2C6H3N(SiMe3)]: Synthesis of Stable Organosilanes with Three Functional Groups. 40. Fluorination with Me3SnF: Synthesis of Cyclopentadienyl-Substituted Group 4 Metal Fluoride Complexes. 41. Seven-Coordinate [MI2(CO)3(NCMe)2], [MI2(CO)3(NCMe)(PPh3)], and Alkyne [MI2(CO)(NCMe)( 2-RC2R)2] Complexes of Molybdenum(II) and Tungsten(II). 42. Chlorothiocarbonyl-bis(triphenylphosphine)iridium(I) [IrCl(CS)(PPh3)2 ]. Contributor Index. Subject Index. Formula Index.
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