Inorganic Syntheses, Volume 33

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ISBN: 9780471208259 | 0471208256
Cover: Hardcover
Copyright: 5/2/2002

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The Inorganic Syntheses series provides inorganic chemists with detailed and foolproof procedures for the preparation of important and timely compounds. Volume 33 includes provocative contributions on syntheses of selected supramolecules, useful reagents/ligands, solid state materials/clusters, and other compounds of general interest.

Syntheses of Selected Supramolecules

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

(9)

1,2,4,5-Tetrakis(2-acetate-2-methylpropanamido)benzene (t-AcMPA-B)

(2)

1,2,4,5-Tetrakis(2-hydroxy-2-methylpropanamido)benzene, [H8(t-HMPA-B)]

(1)

Bistetraphenylphosphonium-di-cobalt(III)-k4:k4-[1,2,4,5-tetrakis(2-oxy-2-methylpropanamido)benzene] {[PPh4]2[Co(k4:k4-t-HMPA-B)]}

(2)

Tetraphenylphosphonium-di-cobalt(III)-k4:k4-[1,2,4,5-tetrakis(2-oxy-2- methylpropanamido)benzene) {[PPh4][Cok4:k4-t-HMPA-B)]}

(3)

A Luminescent Decanuclear Ruthenium(II) Polypyridine Complex: A Convergent Approach to a Dendritic Structure Employing the ``Complexes as Metals/Complexes as Ligands'' Synthetic Strategy

(8)

Bishexafluorophosphate-bisbipyridyl-2,3-bis(2-pyridylpyrazine)ruthenium(II) {[Ru(bPy)2(2,3-dpp))(PF6)2}

(2)

Tetrakis-hexafluorophosphate-bis-bisbipyridyl-2,3-bis(2- (2-pyridylpyrazine)ruthenium(II)-dichlororuthenium(II)({Cl2Ru[(μ-2,3-dpp)Ru(bPy)2]2}(PF6)4)

(1)

Icosakishexafluorophosphate-tris-bis-bisbipyridyl-2,3-bis(2- pyridylpyrazine)ruthenium(II)-2,3-bis(2-pyridylpyrazine) Ruthenium(II)[({Ru[(μ-2,3-dpp)Ru(μ-2,3-dpp)Ru(bPy)2]2}3)(PF3)20]

(2)

Dodecatungstoaluminic Acid and Its Monolacunary and Mixed-Addendum Derivatives

(8)

Dodecatungstoaluminic Acid H5[AlW12O40]

(2)

α-Pentasodium Dodecatungstoaluminate α-Na5(AlW12O40)

(1)

α-Nonapotassium Undecatungstoaluminate α-K9[AlW11O39]

(1)

α-Heptapotassium Vanadoundecatungstoaluminate α-K7[AlVIV,W11O40]

(1)

α-Hexapotassium Vanadoundecatungstoaluminate α-K6[AlVVW11O40]

(1)

Supramolecular Complexes of Bis(2,2'-bipyridine)osmium(II) and Ruthenium(II)

(13)

2,3-Bis(2-Pyridyl)quinoxaline (dpq)

(1)

2,3-Bis(2-pyridyl)benzoquinoxaline (dpb)

(1)

cis-Bis(2,2'-bipyridine)2,3-bis(2-pyridyl)pyrazineosmium(II) hexafluorophosphate Hydrate {[Os(bPy)2(dpp)](PF6)2 . HO}

(1)

cis-Bis(2,2'-bipyridine)2,3-bis(2-pyridyl)quinoxalineosmium(II) Hexafluorophosphate {[Os(bpy)2(dpq)](PF6)2}

(1)

cis-Bis(2,2'-bipyridine)2,3-bis(2-pyridyl) benzoquinoxalineosmium(II) Hexafluorophosphate ([Os(bPy)2(dpb)}(PF6)2}

(1)

cis-Tetrakis(2,2'-bipyridine)-μ-[2,3-bis(2-pyridyl)pyrazine] diosmium(II) Hexafluorophosphate Dihydrate {[(bPy)2Os(dpp)Os(bPy)2](PF6)4 . 2HO}

(1)

cis-Tetrakis(2,2'-bipyridine)-μ-[2,3-bis(2-pyridyl)quinoxaline] diosmium(II) Hexafluorophosphate Dihydrate ([(bPy)2Os(dpq)Os(bPy)2](PF6)4 . 2HO}

(1)

cis-Tetrakis(2,2'-bipyridine)-μ-[2,3-bis(2-pyridyl) benzoquinoxaline]diosmium(II) Hexafluorophosphate Trihydrate {[(bpy)2Os(dpb)Os(bpy)2](PF6}4 . 3H2O}

(1)

cis-Tetrakis(2,2'-bipyridine)-μ-[2,3-bis(2-pyridyl)pyrazine]ruthenium(II)-osmium(II) Hexafluorophosphate Dihydrate {[(bPy)2Os(dpp)Ru(bpy)2](PF6)4 . 2HO}

(1)

cis-Tetrakis(2,2'-bipyridine)-μ,-[2,3-bis(2-pyridyl)quinoxaline] ruthenium(II)-osmium(II) Hexafluorophosphate Trihydrate {[(bPy)2Os(dpq)Ru(bPy)2](PF6)4 . 3HO}

(1)

cis-Tetrakis(2,2'-bipyridine)- μ,-[2,3-bis(2-pyridyl) benzoquinoxaline]ruthenium(II)-osmium(II) Hexafluorophosphate Dihydrate {[bpy)2Os(dpb)Ru(bpy)2](PF6)4 . 2HO}

(3)

Binuclear Oxomolybdenum-Metalloporphyrin Complexes

(13)

5-(3,4-Dimethoxyphenyl)-10,15,20-tri-p-tolylporphyrin (3,4-OMe-TTP)

(2)

5-(2,3-Dimethoxyphenyl)-10,15,20-tri-p-tolylporphyrin (2,3-OMe-TTP)

(1)

5-(3,4-Dihydroxyphenyl)-10,15,20-tri-p-tolylporphyrin (3,4-OH-TTP)

(1)

5-(2,3-Dihydroxyphenyl)-10,15,20-tri-p-tolylporphyrin (3-OH-TTP)

(1)

[Hydrotris(3,5-Dimethyl-l-pyrazolyl)borato] oxomolybdenum(V)dichloride (LMoOCl2)

(1)

[Hydrotris(3,5-Dimethyl-I-pyrazolyl)borato] oxomolybdenum(V)ethyleneglycolate [LMoO(Eth-Gly)]

(1)

5-{3,4-Catecholato[hydrotris(3,5-dimethyl-I-pyrazolyl) borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphyrin (3,4-Mo-TTP)

(1)

5-{2,3-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato] oxomolybdenum(V)}- -10,15,20-tri-p-tolylporphyrin (2,3-Mo-TTP)

(1)

5-{3,4-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatozinc(II) [Zn(3,4-Mo-TTP)]

(1)

5-{2,3-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatozinc(II) [Zn(2,3-Mo-TTP)]

(1)

5-{3,4-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatoiron(III)chloride [FeCl(3,4-Mo-TTP)]

(1)

5-{2,3-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatoiron(III)chloride [FeCl(2,3-Mo-TTP)]

(1)

5-{3,4-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatoiron(III)bis(N-methylimidazole)adduct {Fe(N-MeIm)2[(3,4-Mo-TTP)]Cl}

(1)

5-{2,3-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatoiron(III)bis(N-methylimidazole) adduct {Fe(N-MeIm)4[(2,3-Mo-TTP)]Cl}

(1)

5-{3,4-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatocopper(II) [Cu(3,4-Mo-TTP)]

(1)

5-{2,3-Catecholato[hydrotris(3,5-dimethyl-1-pyrazolyl)borato]oxomolybdenum(V)}-10,15,20-tri-p-tolylporphinatocopper(II) [Cu(2,3-Mo-TTP)]

(2)

Iron Sandwich Polyoxoanion Compounds

(3)

Hexakistetrabutylammonium Octadecatungstotetrairon-diphosphate {(TBA)6 [Fe(H2O)2(PW9O34)2]}

(2)

Dodecasodium Triacontatungstotetrairontetraphosphate Hydrate {Na12(Fe(H2O) 2(P2W15O56)2] . 58H2O}

(1)

Dipyrryl and Porphyrinic Precursors to Supramolecular Conjugated (Porphinato)metal Arrays: Syntheses of Dipyrrylmethane and (5,15-diphenylporphinato)zinc(II)

(6)

2,2'-Dipyrrylmethane (C9H10N2)

(1)

5,15-Diphenylporphyrin

(1)

(5,15-Diphenylporphinato)zinc(II)

(1)

Synthesis of Dodecaoxohexadecacarboxylatotetraaquo-dodecamanganese Mn12O12(O2CR)16(H2O)4] (R = Me,Et,Ph,Cr) Complexes

(6)

[Mn12O12(O2CMe)16(H2O)4] . 4H2O . 2HO2CMe

(1)

[Mn12O12(O2CEt)16(H2O)3](H3O)

(1)

[Mn12O12(O2CPh)16(H2O)4]

(1)

[Mn12O12(O2CCH=CHCH3)16(H2O)3]

(2)

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

(3)

UO2(NO3)2[15-MCcu(II)N(pic)-15]

(1)

{Eu(NO3)2[15-MCcu(II)N(picHA)-15]}NO3

(1)

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]

(5)

Preparation of Free-Base Hydroxylamine:KOH Solution

(1)

3-Hydroxy-2-naphthohydroxamic Acid (H3NHA)

(1)

(Tetraethylammonium)2[Cu(II)5(naphthoylhydroximate)4] dimethylformamide {(Et4N)2[Cu(II)12-MCCu(II)N(nha)-4]DMF}

(1)

Mn(II)(Acetate)2[Mn(III)(salicylhydroximate)]4{Mn(OAc)2[12-MCMn(III)N(shi)-4]}

(2)

Useful Reagents and Ligands

Homoleptic Transition Metal Acetonitrile Cations with Tetrafluoroborate or Trifluoromethanesulfonate Anions

(8)

Bistetrafluoroborate-Hexakisacetonitrile Metal(II){M(CH3CN)6(BF4)2} (M = Fe,Co,Ni)

(1)

Bistetrafluoroborate-Tetrakisacetonitrile Manganese(II){[Mn(CH3CN)4](BF4)2}

(1)

Bistetrafluoroborate-Tetrakisacetonitrile Copper(II){[Cu(CH3CN)4](BF4)2)

(1)

[M(CH3CN)x][BF4]2 from [M(H2O)x][BF4]2 (M= Mn,Fe,Co,Ni,Cu)

(1)

Bistetrafluoroborate-Tetrakisacetonitrile Chromium(II) [Cr(CH3CN)4](BF4)2 from Chromous Acetate [Cr2(O2CCH3)4]

(1)

Preparation of Acetonitrile Cations with Trifluoromethanesulfonate (Triflate) Anions

(1)

Anhydrous Metal Triflate Complexes

(1)

Metal Acetonitrile Complex Cations with Triflate Anions

(3)

Synthesis of [MII(NCMe)6]2+ (M = V,Cr,Mn,Fe,Co,Ni) Salts of Tetra[3,5-bis(trifluoromethyl)phenyl]borate

(8)

Potassium Tetra-3,5-bis(trifluoromethyl)phenylborate, (K{B[C6H3(CF3)2]4})

(1)

Silver Tetra-3,5-bis(trifluoromethyl)phenylborate (Ag{B[C6H3(CF3)2]4})

(1)

Hexakis(acetonitrile)manganese(II)bis-tetra-3,5-bis(trifluoromethyl)phenylborate ([MnII(NCMe)6]{B[C6H3(CF3)2]4}2)

(1)

Hexakis(acetonitrile)iron(II)bis-tetra-3,5-bis(trifluoromethyl) phenylborate ([FeII(NCMe)6]{B[C6H3(CF3)2]4}2)

(1)

Hexakis(acetonitrile)cobalt(II)bis-tetra-3,5-bis(trifluoromethyl) phenylborate ([CoII(NCMe)6][B[C6H3(CF3)2]4})

(1)

Hexakis(acetonitrile)nickel(II)bis-tetra-3,5-bis(trifluoromethyl)phenylborate ([NiII(NCMe)6]{B[C6H3(CF3)2]4})

(1)

Hexakis(acetonitrile)chromium(II)bis-tetra-3,5- bis(trifluoromethyl)phenylborate ([CrII(NCMe)6]{B[C6H3(CF3)2]4}2)

(1)

Hexakis(acetonitrile)vanadium(II)bis-tetra-3,5-bis(trifluoromethyl)phenylborate ([VII(NCMe)6]{B[C6H3(CF3)2]4}2)

(2)

Transition Metal p-Toluenesulfonates

(12)

Tetraaquotitanium(III)tris-p-toluenesulfonate

(1)

Titanium(Ill)tris-p-toluenesulfonate

(1)

Hexaaquovanadium(III)tris-p-toluenesulfonate

(1)

Vanadium(III)tris-p-toluenesulfonate

(1)

Pentaquooxovanadium(IV)bis-p-toluenesulfonate Hemihydrate

(1)

Tetraaquochromium(II)bis-p-toluenesulfonate

(1)

Hexaquochromium(IlI)tris-p-toluenesulfonate

(1)

Tetraquomanganese(II)bis-p-toluenesulfonate Hydrate

(1)

Hexaquoiron(II)bis-p-toluenesulfonate

(1)

Iron(III)tris-p-toluenesulfonate

(1)

Hexaquocobalt(II)bis-p-toluenesulfonate

100

(1)

Hexaquonickel(II)bis-p-toluenesulfonate

100

(1)

Cesium-p-toluenesulfonate

101

(1)

Preparation of Anhydrous Tosylate Salts

101

(2)

Salts of Binuclear Iron(II) and Iron(III) Dianions [(Fe2Cl6)2- and (Fe2OCl6)2-]

103

(4)

Di(tetraphenylphosphonium)hexachlorodiferrate(II) [(Fe2Cl6)(PPh4)2]

104

(1)

Di(tetraphenylphosphonium)(μ-oxo)bis(trichloroferrate(III) [(PPh4)2(Fe2OCl6)]

105

(1)

Di(tetraethylammonium)(μ-oxo)bis(trichloroferrate(III) (Et4N)2(Fe2OCl6)

105

(2)

Tetraethylammonium-Tetrathioperrhenate Et4N(ReS4)

107

(3)

Stock Ammonium Sulfide Solution (20%)

108

(1)

Tetraethylammonium-tetrasulfidorhenate [Et4N(ReS4)]

108

(2)

Large-Scale Synthesis of Methyltrioxorhenium (CH3ReO3)

110

(2)

Silver Tetraoxorhenate [Ag(ReO4)]

111

(1)

Methyltrioxorhenium (CH3ReO3)

111

(1)

4,5-Diaminocatechol: A Useful Building Block in Synthesis of Multimetallic Complexes

112

(7)

1,2-Dimethoxy-4,5-dinitrobenzene (4,5-Dinitroveratrole)

114

(1)

1,2-Dimethoxy-4,5-diaminobenzene (4,5-Diaminoveratrole)

115

(1)

1,2-Dihydroxy-4,5-diaminobenzenehydrobromide

115

(1)

[N,N'-Bis(3,3'-H-5,5'-H'-salicylidene)-4,5-dihydroxyphenylenediamine] [H2-(H4salphen)-(OH)2]

116

(1)

(N,N'-Bis(3,3'-t-butyl-5,5'-t-butylsalicylidene) 4,5- dihydroxyphenylenediamine]etherate ([H2-('Butyl4salphen)(OH)2]ether}

116

(1)

(N,N'-Bis(3-ethoxy-5-H-salicylidene)-4,5-dihydroxyphenylenediamine(pyridinium bromide) {[H2(EtO2H2salphen)(OH)2] . pyHBr}

117

(1)

[N,N'-Bis(3,3'-H-5,5'-H'-salicylidene)-4,5-dihydroxyphenylenediamino)nickel(II) {[NiII-(H4salphen)(OH)2]}

118

(1)

Bis-tetrabutylammonium-bis[N,N'-bis(3,3'-H-5,5'- H'-salicylidene)catecholatodiamino]nickel(II)-oxovanadium(IV) (Bu4)2(VO[NiII(H4salphen)(O)2]2}

118

(1)

Convenient Synthesis of 1,5,9-Trithiacyclododecane (S3C9H18)

119

(3)

1.5,9-Trithiacyclododecane

120

(2)

Solid-State Materials and Clusters

Synthesis of Quaternary Selenophosphates using Molten Salt Fluxes: Rb8Hg4(Se2)2(PSe4)4, K4In2(PSe5)2(P2Se6), Rb4Ti2(P2Se7)(P2Se9)2, Rb4U4(Se)2(Se2)4(PSe4)4

122

(8)

Diphosphoruspentaselenide (P2Se5)

123

(1)

Octarubidium-tetramercury-bisdiselenido-tetrakistetraselenophosphate Rb8Hg4(Se2)2(PSe4)4]

124

(1)

Tetrapotassium-diindium-bisphosphoruspentaselenide-diphosphorushexaselenide [K4In2(PSe5)2(P2Se6)]

125

(2)

Tetrarubidium-dititanium-diphosphorusheptaselenide-bisdiphosphorusnonaselenide [Rb4Ti2(P2Se7)(P2Se9)2]

127

(1)

Tetrarubidium-tetrauranium-bisselenidotetrakisdiselenido-tetrakistetraselenophosphate [Rb4U4(Se)2(Se2)4(PSe4)4]

128

(2)

Hydrothermal Synthesis of Sulfosalts: Ag3AsS3, Ag3SbS3, Ag7SbS6, Cu12Sb4S13, CuInS2, FeIn2S4

130

(9)

Trisilver Arsenic Trisulfide (Proustite; Ag3AsS3)

132

(4)

Trisilver Antimony Trisulfide (Pyrargyrite; Ag3SbS3)

136

(1)

Heptasilver Antimony Hexasulfide (Argrodite; Ag7SbS6)

136

(1)

Dodecacopper Tetraantimony Decatrisulfide (Tetrahedrite; Cu12Sb4S13)

137

(1)

Copper Indium Disulfide (Roquesite; CuInS2)

137

(1)

Iron Diindium Tetrasulfide (Indite; FeIn2S4)

138

(1)

Open-Framework Solids of the Vanadium Oxide-Phosphate System

139

(5)

1,3-Diammoniumpropane-bisaquo-bishydroxo-bisphosphato-trisvanadyl(IV) {[H3N(CH2)3NH3] [(VO)3(OH)2(H2O)2(PO4)2]}

140

(3)

[HN(CH2CH2)2NH]K1.35[V5O9(PO4)2]xH2O

143

(1)

[H2N(CH2CH2)2NH2][(VO)3(HPO3)4(H2O)2]

143

(1)

Sulfur-Bridged Incomplete Cubane-Type Molybdenum and Tungsten Aqua Ions

144

(6)

Sulfur-Bridged Incomplete Cubane-Type Molybdenum Aqua Ion, [Mo3S4(H2O)9]4+(Mo3), in Solution and [MO3S4(H2O)9](CH3C6H4SO3)4+ . 9H2O (Mo3pts)

145

(1)

Nonaaquotrimolybdenum-tetrasulfide, [Mo3S4(H2O)9]4+ (Mo3), in Solution

145

(2)

Nonaaquotrimolybdenum-tetrasulfide-tetrakis-p-toluenesulfonate-nonahydrate, [MO3S4(H2O)9](CH3C6H4SO3)4 . 9H2O (Mo3pts)

147

(1)

Sulfur-Bridged Incomplete Cubane-Type Tungsten Aqua Ion, [W3S4(H2O)9]4+ (W3), in Solution and [W3S4(H2O)9](CH3C6H4SO3)4 . 9H2O (Wpts)

147

(1)

Nonaaquotritungsten-tetrasulfide, [W3S4(H2O)9]4+(W), in Solution

147

(1)

Nonaaquotritungsten-tetrasulfide-tetrakis-p-toluenesulfonate-nonahydrate, [W3S4(H2O)9] (CH3CH6SO3)4 . 9H2O (W3pts)

148

(2)

Sulfur-Bridged Cubane Type Mixed-Metal Clusters with Mo3MS4 (M = Fe,Co,Ni,Cu,In,Sn) and W3NiS4 Cores

150

(12)

Molybdenum-iron Cluster Aqua Ion, [Mo3FeS4(H2O)10]4+ (Mo3Fe), in Solution and [Mo3FeS4(H2O)10](CH3C6H4SO3)4 . 7H2O(Mo3Fepts)

152

(1)

Decaaquotrimolybdenum-iron-tetrasulfide, [Mo3FeS4(H2O)10]4+(Mo3Fe), in Solution

152

(2)

Decaaquotrimolybdenum-iron-tetrasulfide-tetrakis-p-toluenesulfonate-heptahydrate, [Mo3FeS4(H2O)10](CH3C6H4SO3)4 . 7H2O (Mo3Fepts)

154

(1)

Molybdenum-cobalt Cluster Aqua Ion, [(H2O)9Mo3S4CoCoS4Mo3(H2O)9]8+ (Mo3Co-D), in Solution and [(H2O)9Mo3S4CoCoS4Mo3(H2O)9(CH3C6H4SO3)8 . 18H2O (Mo3Co-Dpts)

155

(1)

Bisnonaaquotrimolybdenum-cobalt-tetrasulfide, [(H2O)9Mo3S4CoCoS4Mo4(H2O)9]+ (Mo3Co-D), in Solution

155

(1)

Bisnonaaquotrimolybdenum-cobalt-tetrasulfide-octakis-p-toluenesulfonate-octadecahydrate, [(H2O)9Mo3S4CoCoS4Mo3(H2O)9] (CH3C6H4SO3)8 . 18H2O (Mo3Co-Dpt)

155

(1)

Molybdenum-nickel Cluster Aqua Ion, [Mo3NiS4(H4O)10]4+(Mo3Ni) in Solution and [Mo3NiS4(H2O)10] (CH3C6H4SO3)4 . 7H2O (Mo3Nipts)

156

(1)

Decaaquotrimolybdenum-nickel-tetrasulfide, [Mo3NiS4(H2O)10]4+ (Mo3Ni), in Solution

156

(1)

Decaaquotrimolybdenum-nickel-tetrasulfide-tetrakis-p-toluenesulfonate-heptahydrate, [Mo3NiS4(H2O)10] (CH3C6H4SO3)4 . 7H2O (Mo3Nipts)

156

(1)

Molybdenum-copper Cluster Aqua Ion Decaaquo Trimolybdenum-copper-tetrasulfide, [Mo3CuS4(H2O)10]4+ (Mo3Cu), and Bisnonaaquotrimolybdenum-copper-tetrasulfide, [(H2O)9Mo3S4CuCuS4Mo3(H2O)9]8+(Mo3Cu-D), in Solution and Bisnonaaquotrimolybdenum-copper-tetrasulfide-octakis-p-toluenesulfonate-icosahydrate, [(H2O)9Mo3S4CuCuS4Mo3(H2O)9] (CH3C6H4SO3)8 . 20H2O (Mo3Cu-Dpts)

157

(1)

Bisnonaaquotrimolybdenum-copper-tetrasulfide-octakis-p-toluenesulfonate- icosahydrate, [(H2O)9Mo3S4CuCuS4Mo3(H2O)9](CH3CH6SO3)8 . 20H2O (Mo3Cu-Dpts)

157

(1)

Molybdenum-indium Cluster Aqua Ion Dodecaaquo Trimolybdenum-indium-tetrasulfide, [Mo3InS4(H2O)12]5+ (Mo3In), in Solution and Di-p-toluenesulfonato-decaaquo- trimolybdenum-indium-tetrasulfide-tris-p-toluenesulfonate-tridecahydrate, [Mo3InS4(CH3C6H4SO3)2(H2O)10] (CH3C6H4SO3)3 . 13H2O (Mo3Inpts)

158

(1)

Di-p-toluenesulfonato-decaaquo-trimolybdenum-tetrasulfide-tris-p-toluenesulfonate-tridecahydrate, [Mo3InS4(CH3C6SO3)2(H2O)10](CH3C6H4SO3)3 . 13H2O (Mo3Inpts)

159

(1)

Molybdenum-tin Cluster Aqua Ion Bis(nonaaquo Trimolybdenum-tetrasulfide)-tin, [(H2O)9Mo3S4SnS4Mo3(H2O)9]8+ (Mo3Sn-SW), and Dodecaaquotrimolybdenum- tin-tetrasulfide, [Mo3SnS4(H2O)12]6+ (Mo3Sn-OX),in Solution and is(nonaaquotrimolybdenum-tetrasulfide)-tin-octakis-p-toluenesulfonate-hexacosahydrate,[(H2O)9Mo3S4SnS4Mo3(H2O)9](CH3C6H4SO3)8 . 26H2O (Mo3Sn-SWpts)

159

(1)

Bis(nonaaquotrimolybdenum-tetrasulfide)-tin-octakis-p-toluenesulfonate-icosahexahydrate, (H2O)9Mo3S4SnS4Mo3(H2O)9](CH3C6H4SO3)8 . 26H2O (Mo3Sn-SWpts)

159

(1)

Dodecaaquotrimolybdenum-tin-tetrasulfide, [Mo3SnS4(H2O)12]6+ (Mo3Sn-OX), in Solution

160

(1)

Tungsten-nickel Cluster Aqua Ion Decaaquo Tritungsten-nickel-tetrasulfide, [W3NiS4(H2O)10]4+ (W3Ni), in Solution and Bisnonaaquotritungsten-nickel-tetrasulfide-octakis-p-toluenesulfonate-icosahydrate, [(H2O)9W3S4NiNiS4W3 (H2O)9](CH3C6H4SO3)8 . 20H2O (W3Ni-Dpts)

161

(1)

Bisnonaaquotritungsten-nickel-tetrasulfide-octakis-p-toluenesulfonate-icosahydrate [(H2O)9W3S4NiNiS4 W3(H2O)9](CH3C6H4SO3)8 . 20H4O (W3Ni-Dpts)

161

(1)

Molybdenum and Tungsten Clusters as Aqua Ions [M3Q4(H2O)9]4+(M = Mo,W;Q = S,Se) and Related Chalcogen-Rich Trinuclear Clusters

162

(9)

Heptachalcogenotetrabromotrimetallo Compounds, {M3Q7Br4)x, (M = Mo,W;Q = S,Se)

164

(1)

Nonaaquatetrasulfidotrimolybdenum(IV) [Mo3S4(H2O)9]4+ (First Method)

165

(1)

[Mo3S4(H2O)9]4+ (Second Method)

166

(1)

Preparation of (NH4)2[Mo3S13] . 2HO from {Mo3S7Br4}x

166

(1)

Bistetraethylammonium-heptasulfidohexabromotrimolybdate, (Et4N)2[Mo3S7Br4]x

166

(1)

Nonaaquatrimolybdenum-tetrasulfide, [Mo3S4(H2O)9]4+

167

(1)

W3S4(H2O)9]4+ (First Procedure)

167

(1)

[W3S4(H2O)9]4+ (Second Procedure)

167

(1)

(NH4)2[W3S16(NH3)3] . H2O from {W2S7Br4}x

168

(1)

[W3S4(H2O) ]+

168

(1)

[MoSe(H2O)9]4+

168

(1)

Preparation of [W3Se4(H2O)9]4+ from {W3Se7Br4}x

169

(2)

Compounds Of General Interest

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, AuTI(MTP)4, Hg(MTP)2, Hg(MTP)2(AuCl)2, and HgIIAuI(MTP)2AuIIIC14

171

(10)

(Diphenylmethylenethiophosphinato)di-gold(I), [AuCH2P(S)Ph2]2

172

(2)

Bis(triphenylphosphoranylidene)ammonium (diphenylmethylenethiophosphinato)gold(I),(PPN){Au[CH2P(S)Ph2]2}

174

(1)

Tetrakis(diphenylmethylenethiophosphinato)digold(I) platinum(II) Au2Pt[CH2P(S)Ph2]4

175

(1)

Tetrakis(diphenylmethylenethiophosphinato)digold(I)lead(II) Au2Pb[CH2P(S)Ph2]4

176

(1)

Bis(diphenylmethylenethiophosphinato)gold(I)thallium(I), 2AuTl[CH2P(S)Ph2]2

177

(1)

Bis(diphenylmethylenethiophosphinato)mercury(II), Hg[CH2P(S)Ph2]2

177

(1)

Bis(diphenylmethylenethiophosphinato)mercury(II) dichloro-di-gold(I), Hg[CH2P(S)Ph2]2(AuCl)2

178

(1)

Bis(diphenylmethylenethiophosphinato)mercury(II)gold(I)-tetrachlorogold(III), HgIIAuI[CH2P(S)Ph2]2AuIIICl4

179

(2)

Mesityl-gold(I) Complexes

181

(4)

Mesityltriphenylarsine-gold(I) {[Au(mes)(AsPh3)]}

181

(1)

(Benzyl)triphenylphosphonium-chloromesitylaurate(I) {BrPPh3[Au(mes)Cl]}

182

(1)

Pentamesityl-gold(I) {[Au(mes)]5}

183

(2)

An Improved Synthesis of cis-Dithiocyanato-bis(4,4'-dicarboxy-2,2`-bpy)Rut(II) Sensitizer

185

(4)

cis-Dichloro-bis(4,4'-dicarboxy-2,2'-bpy)Ru(II) [RuL2(Cl)2]

185

(1)

cis-Dithiocyanato-bis(4,4'-dicarboxy-2.2'-bpy)Ru(II) [RuL2(NCS)2]

186

(3)

Dimethylsulfoxide Complexes of Platinum(II): K[PtCl3(Me2SO)], cis-[PtCl2L(Me2SO)1](L = Me2SOMeC), [PtCl(μ-Cl)(Me2SO)]2, and [Pt(Me2SO)4](CF3SO3)2

189

(7)

Potassium Trichloro(dimethylsulfoxide)platinate(II) (K[PtCl3{(CH3)2SO}])

191

(1)

cis-Dichlorobis(dimethylsulfoxide)platinum(II) (cis-[PtCl2{(CH3)2SO}2])

192

(1)

cis-Dichloro(acetonitrile)(dimethylsulfoxide)platinum(II) (cis-[PtCl2(CH3CN){(CH3)2SO}])

192

(1)

Di-μ-chloro-dichloro-bis(dimethylsulfoxide)diplatinum(II) ([PtCl(μ-cl){(CH3)2SO}]2)

193

(1)

Tetrakis(dimethylsulfoxide)platinum(II) bis(trifluoromethanesulfonate) [Pt{(CH3)2SO}2[(CH3)2SO2][SO3CF3]2

194

(2)

Tetrasulfur-tetranitride (S4N4)

196

(3)

Bis[bis(trimethylsilyl)amino]sulfide {[(Me3Si)2N]2S}

197

(1)

Tetrasulfur Tetranitride (S4N4)

198

(1)

Hydrotris(methimazolyl)borate

199

(4)

Hydrotris(methimazolyl)borate

200

(3)

Arsenic(III)bromide

203

(1)

Arsenic-tribromide (AsBr3)

203

(1)

Dichlorodioxo-bis(triphenylphosphine oxide)uranium(VI) [UO2Cl2(OPPh3)2]

204

(2)

Chlorohydro-tris(pyrazol-1-yl)borato-bis(triphenylphosphine) ruthenium(II) {RuCl[k4-HB(pz)3](PPh3)2} (pz = pyrazol-l-yl)

206

(2)

Octacarbonyl-di-μ-hydridodirhenium [Re2(μ-H)2(CO)8]

208

(2)

Zero-Valent Binuclear Nickel Complexes

210

(3)

Di(carbonyl)-(μ-carbonyl)bis[μ-bis(diphenylphosphino) methane]dinickel(0) [Ni2(μ-CO)(CO)2(μ-dpmm)2]

210

(1)

Di(isocyanomethane)-(μ-isocyanomethane)bis [μ-bis(diphenylphosphino)methane)di-nickel(0) (Ni2(μ-CNCH3)(CNCH3)2(μ-dpPm)2]

211

(2)

Preparation of a Synthetic Ribonuclease: The Europium(III) Complex of 1-(4-nitrobenzyl)-4,7,10-Tris(carbamoylmethyl)-1,4,7,10-tetraazacyclododecane

213

(5)

1-(4-Nitrobenzyl)-4,7,10-tetraazacyclododecane (NBC)

214

(1)

1-(4-Nitrobenzyl)-4,7,10-tris(carbamoylmethyl)-1,4,7,10-tetraazacyclododecane (NBAC)

215

(2)

1-(4-Nitrobenzyl)-4,7,10-tris(carbamoylmethyl)-1,4,7,10-tetraazacyclododecane europium(III)] [[Eu(NBAC)](CF3SO3)3]

217

(1)

Carbonyl Halide Tungsten(II) Complexes of Tris(3,5-dimethylpyrazolyl)hydroborate

218

(9)

Potassium-tris(3,S-dimethylpyrazolyl)hydroborate (KTp*)

219

(1)

3,5-Dimethylpyrazole

219

(1)

Potassium Tris(3,5-dimethylpyrazolyl) hydroborate. KTp*

220

(1)

Tetraethylammonium Tricarbonyl[tris-(3,5-dimethylpyrazolyl)hydroborato]-tungstate(0) {NEt4(Tp*W(CO)3]}

221

(1)

Tricarbonylhalo[tris(3,5-dimethylpyrazolyl)hydroborato] tungsten(11) [Tp*WX(CO)3] (X=Cl, Br)

222

(1)

Tp*WCl(CO)3

223

(1)

Tp*WBr(CO)3

223

(1)

Tricarbonyliodo[tris(3,5-dimethylpyrazolyl)hydroborato] tungsten(II) [Tp*WI(CO)3]

224

(1)

Dicarbonylhalo[tris(3,5-dimethylpyrazolyl)hydroborato] tungsten(II) [Tp*WX(CO)2] (X = Cl, Br, I)

225

(1)

Carbonyl(acetonitrile-k2N,C)tris(3,5-dimethylpyrazolyl) hydroborato]tungsten(II) [Tp*WI(MeCN-k2N,C)(CO)]

226

(1)

A Luminescent Complex of Re(I): fac-[Re(CO)3(bpy)(py)](CF3SO3) (bpy = 2.2'-bipyridine; py = Pyridine)

227

(3)

fac-Tricarbonyl(trispyridine)rhenium(I)trifluoromethanesulfonate {fac-[Re(CO)3(py)3](CF3SO3)}

228

(1)

fac-Tricarbonyl(2,2'bipyridine)(pyridine)rhenium(I) trifluoromethanesulfonate {fac-[Re(CO)3(bpy)(py)](CF3SO3)}

228

(2)

RSi(OH)3 and RSi(NH2)3 [R = 2,6-iPr2C6H3N(SiMe3)]: Synthesis of Stable Organosilanes with Three Functional Groups

230

(4)

[2,6-iPr2C6H3N(SiMe3)]Si(OH)3

231

(1)

[2.6-iPr2C6H3N(SiMe3)]Si(NH2)3

232

(2)

Fluorination with Me3SnF: Synthesis of Cyclopentadienyl-Substituted Group 4 Metal Fluoride Complexes

234

(5)

Pentamethylcyclopentadienyl(titanium trifluoride) [η5-C5Me5)TiF3]

234

(1)

Pentamethylcyclopentadienyl(zirconium trifluoride) {[(η5-C5Me5)ZrF3]4)

235

(1)

Pentamethylcyclopentadienyl(hafnium trifluoride) {[(η5-C5Me5)HfF3]4}

236

(1)

Pentamethylcyclopentadienyl(titanium oxofluoride){[(η5-C5Me5)TiFO]4}

236

(1)

Pentamethylcyclopentadienyl(titanium imidophenyl fluoride) {[(η5-C5H4Me)TiF(NPh)]2}

237

(1)

Bispentamethylcyclopentadienyl(titanium fluoride) (η5-C5Me5)2TiF

238

(1)

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)

239

(5)

Diiodo(tricarbonyl)bis(acetonitrile)molybdenum(II)/tungsten(II)

240

(1)

Diiodo(carbonyl)(acetonitrile)bis(diphenylacetylene) [tungsten(II)]

241

(1)

Diiodotricarbonyl(acetonitrile)triphenylphosphine [tungsten(II)]

242

(2)

Chlorothiocarbonyl-bis(triphenylphosphine)iridium(I) [IrCl(CS)(PPh)3]2

244

(3)

Contributor Index

247

(2)

Subject Index

249

(6)

Formula Index

255

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Inorganic Syntheses, Volume 33

Summary

Author Biography

Table of Contents

Supplemental Materials

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Inorganic Syntheses, Volume 33

Summary

Author Biography

Table of Contents

Supplemental Materials

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