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Tran, Nguyet T.; Powell, Douglas R.; Dahl, Lawrence F.

doi:10.1002/1521-3773(20001117)39:22<3945::aid-anie3945>3.0.co;2-a

Cited by 83 publications

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“…The different colors of 1 and 2 (red and black) arise from quantum size effect, which result from the dependency of the band gap on particle size. [14] 2 þSðSiMe3 Þ2 þPnPr3 CF 3 CO 2 …”

mentioning

confidence: 89%

“…The solution becomes dark and black crystals of 2 are formed [Eq. (2)]. Employment of PnBu 3 in an analogous reaction produces black crystals of 3 [Eq.…”

mentioning

confidence: 99%

“…Employment of PnBu 3 in an analogous reaction produces black crystals of 3 [Eq. (2)]. Depending on the reaction conditions, 2 is often produced together with black amorphous Ag 2 S. Attempts to recrystallize 2 and 3 from THF or CH 2 Cl 2 failed and produced Ag 2 S as the only isolatable material.…”

mentioning

confidence: 99%

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Syntheses and Crystal Structures of the New Ag–S Clusters [Ag70S16(SPh)34(PhCO2)4(triphos)4] and [Ag188S94(PR3)30]

Wang

Langetepe

Persau

et al. 2002

Angew. Chem. Int. Ed.

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Dedicated to Professor Achim M¸ller on the occasion of his 65th birthday Many investigations towards synthesis and structural characterization of large metal-rich clusters have been reported over the last few years. Particularly noteworthy are the oxometallates of molybdenum described by M¸ller et al.; only recently Na 48 [H x Mo 368 O 1032 (H 2 O) 240 (SO 4 ) 48 ]¥n 1000 H 2 O (x % 16; n % 1000), the largest known derivative of a heteropolyacid was structurally characterized. [1] Other examples of large cluster complexes are [Pd 145 (CO) x (PEt 3 ) 30 ] (x % 60) made by Dahl et al. [2] and [Ga 84 {N(SiMe 3 ) 2 } 20 Li 6 Br 2 (thf) 20 ] reported by Schnˆckel and Schnepf. [3] The synthesis of the larger Ag±S cluster complexes [Ag 14 S(SPh) 12 (PPh 3 ) 8 ] [4] and [HNEt 3 ] 4 -[Ag 50 S 7 (SC 6 H 4 tBu) 40 ] [5] was recently achieved by Jin et al.Over the last few years one of our major fields of interest was the synthesis of transition-metal clusters containing S, Se, Te, P, As, and Sb as bridging ligands, for example, copperchalcogenide clusters stabilized by tertiary phosphane ligands. [6] Reactions of transition-metal salts with Group 16 silyl derivatives E(SiMe 3 ) 2 or RESiMe 3 (R ¼ alkyl-or aryl-; E ¼ S, Se, Te) allows access to these clusters. [7] Addition of tertiary phosphanes to these reactions prevents the formation of the thermodynamically stable binary phase. [8] Compounds obtained by this route include: [Cu 146 Se 73 -(PPh 3 ) 30 ], [9] [Ag 172 Se 40 (SenBu) 92 (dppp) 4 ] [10] [Ag 38 Te 13 (TetBu) 12 (dppe) 6 ] (dppe ¼ bis(1,2-diphenylphosphanyl)ethane), [11] [Au 18 Se 8 -(dppe) 6 ]Cl 2 [12] , and [Zn 16 Te 13 (TePh) 6 (tmeda) 5 ] [13] (tmeda ¼ tetramethylethylenediamine). Herein we report the synthesis of the Ag±S clusters 1, 2, and 3 containing 120 and 282 heavy atoms, respectively, in the cluster core. ½Ag 70 S 16 ðSPhÞ 34 ðPhCO 2 Þ 4 ðtriphosÞ 4 1 ½Ag 188 S 94 ðPnPr 3 Þ 30 2 ½Ag 188 S 94 ðPnBu 3 Þ 30 3The reaction of a suspension of silver benzoate and triphos [1,1,1-tris{(diphenylphosphanyl)methyl}ethane] with a mixture of S(Ph)SiMe 3 and S(SiMe 3 ) 2 (2:1) at À20 8C in diglyme produces a deep red solution from which small red needles of 1 [Eq. (1)], can be isolated.Reaction of S(SiMe 3 ) 2 with silver trifluoroacetate and PnPr 3 at À40 8C in diglyme initially produces a red solution. After a few hours stirring, the reaction is allowed to warm up to room temperature. The solution becomes dark and black crystals of 2 are formed [Eq. (2)]. Employment of PnBu 3 in an analogous reaction produces black crystals of 3 [Eq. (2)]. Depending on the reaction conditions, 2 is often produced together with black amorphous Ag 2 S. Attempts to recrystallize 2 and 3 from THF or CH 2 Cl 2 failed and produced Ag 2 S as the only isolatable material. The different colors of 1 and 2 (red and black) arise from quantum size effect, which result from the dependency of the band gap on particle size. [14] 2 þSðSiMe3 Þ2 þPnPr3The molecular structures of complexes 1 and 2 in the solidstate were determined by X-ray crysta...

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“…The different colors of 1 and 2 (red and black) arise from quantum size effect, which result from the dependency of the band gap on particle size. [14] 2 þSðSiMe3 Þ2 þPnPr3 CF 3 CO 2 …”

mentioning

confidence: 89%

“…The solution becomes dark and black crystals of 2 are formed [Eq. (2)]. Employment of PnBu 3 in an analogous reaction produces black crystals of 3 [Eq.…”

mentioning

confidence: 99%

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Syntheses and Crystal Structures of the New Ag–S Clusters [Ag70S16(SPh)34(PhCO2)4(triphos)4] and [Ag188S94(PR3)30]

Wang

Langetepe

Persau

et al. 2002

Angew. Chem. Int. Ed.

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“…It may therefore be interesting to emphasize their similarity with the molecular cluster Pd 145 (CO) 60 (PEt 3 ) 30 recently characterized by Dahl. The size of the metal core of this cluster is estimated to be of the same order of magnitude as these platinum phosphine colloids and it is noteworthy that this Pd 145 cluster adopts a non-periodic structure [40].…”

Section: Stabilization By Ligandsmentioning

confidence: 99%

Organometallic Nanoparticles of Metals or Metal Oxides

Chaudret

Philippot

2007

Oil & Gas Science and Technology - Rev. IFP

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*Dedicated to Yves Chauvin for his exceptional and exemplary contribution to organometallic chemistry and catalysis Ce manuscrit est dédié à Yves Chauvin pour sa contribution exceptionnelle et exemplaire à la chimie organométallique et à la catalyse Résumé -Revue sur la synthèse de nanoparticules de métaux et d'oxydes métalliques -Nous présentons dans cet article une revue sur la synthèse de nanoparticules de métaux et d'oxydes métalliques utilisant une approche organométallique et plus précisément des complexes de ligands hydrocarbures comme précurseurs. L'avantage principal de cette approche réside dans la décomposition facile de ces précurseurs qui peut être effectuée dans des conditions douces et qui ne génère aucun polluant potentiel des nanoparticules. Ceci permet le contrôle de la taille, de la forme et de l'état de surface des nanoparticules formées. Les résultats sont présentés par métaux et par mode de stabilisation (polymères, ligands, liquides ioniques). Nous présentons également quelques résultats concernant l'utilisation de cette approche pour la préparation de matériaux hybrides contenant des nanoparticules incluses dans des matrices minérales (membranes d'alumine, silice mésoporeuse). Enfin nous décrivons également une extension de cette approche pour la synthèse directe de nanoparticules en lit fluidisé. Abstract -Organometallic Nanoparticles of Metals or Metal Oxides

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“…Nach wenigen Stunden Reaktionszeit und anschlie˚endem Erw‰rmen auf Raumtemperatur nimmt die Lˆsung eine dunkle Farbe an, und schwarze Kristalle von 2 werden gebildet [Gl. (2)]. Auf analoge Weise kann 3 synthetisiert werden, das ebenfalls in Form schwarzer Kristalle kristallisiert [Gl.…”

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Synthesen und Kristallstrukturen der Ag-S-Clusterverbindungen [Ag70S16(SPh)34(PhCO2)4(triphos)4] und [Ag188S94(PR3)30]

Wang¹,

Langetepe²,

Persau³

et al. 2002

Angew. Chem.

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Professor Achim M¸ller zum 65. Geburtstag gewidmet ‹ber die Synthese und Strukturaufkl‰rung von gro˚en metallreichen Clustermolek¸len wurde in den vergangenen Jahren mehrfach berichtet. Besonders spektakul‰r sind die von M¸ller et al. beschriebenen Oxometallate des Molybd‰ns. Erst k¸rzlich gelang z. B. die Strukturbestimmung von Na 48 [H x Mo 368 O 1032 (H 2 O) 240 (SO 4 ) 48 ]¥n H 2 O (x % 16, n % 1000), dem grˆ˚ten bisher bekannten Derivat einer Heteropolys‰u-re. [1] Weitere Beispiele f¸r gro˚e Clusterkomplexe sind das von Dahl et al. aufgekl‰rte [Pd 145 (CO) x (PEt 3 ) 30 ] [2] (x % 60) und das von Schnˆckel und Schnepf beschriebene [Ga 84 {N(SiMe 3 ) 2 } 20 Li 6 Br 2 (thf) 20 ]. [3] Die Synthese grˆ˚erer Silber-Schwefel-Clusterkomplexe gelang k¸rzlich Jin et al. in Form der Verbindungen [Ag 14 S(SPh) 12 (PPh 3 ) 8 ] [4] und [HNEt 3 ] 4 [Ag 50 S 7 -(SC 6 H 4 tBu) 40 ]. [5]Seit mehreren Jahren besch‰ftigen wir uns mit Clusterverbindungen der ‹bergangselemente, die S, Se, Te, P, As und Sb als Br¸ckenliganden enthalten. Beispiele daf¸r sind Kupferchalkogenidcluster, die von sch¸tzenden terti‰ren Phosphanen koordiniert sind. [6] Ein h‰ufig genutzter Ansatz zur Synthese von Chalkogen-verbr¸ckten Clusterkomplexen ist die Umsetzung von ‹bergangsmetallsalzen mit silylierten Chalkogenderivaten der Zusammensetzung E(SiMe 3 ) 2 oder RESiMe 3 (R ¼ Alkyl, Aryl; E ¼ S, Se, Te). [7] Dabei kann die Bildung der thermodynamisch stabileren bin‰ren Phase durch Zusatz von terti‰ren Phosphanen verhindert werden. [8] Mit dieser Methode wurden z. B. [Cu 146 Se 73 (PPh 3 ) 30 ], [9] [Ag 172 Se 40 -(SenBu) 92 (dppp) 4 ] [10] (dppp ¼ 1,3-Bis(diphenylphosphanyl)-propan),[Ag 38 Te 13 (TetBu) 12 (dppe) 6 ] (dppe ¼ 1,2-Bis(diphenylphosphanyl)ethan), [11] [Au 18 Se 8 (dppe) 6 ]Cl 2 [12] und [Zn 16 Te 13 -(TePh) 6 (tmeda) 5 ] [13] (tmeda ¼ Tetramethylethylendiamin) erhalten. Mit der hier beschriebenen Synthese von [Ag 70 S 16 (SPh) 34 (PhCO 2 ) 4 (triphos) 4 ] 1 und [Ag 188 S 94 (PR 3 ) 30 ] (R ¼ nPr (2), nBu (3)) gelang nun die Herstellung von Silber-Schwefel-Clustern mit 120 bzw. 282 Schweratomen im Clusterkern.Bei der Reaktion einer Suspension aus Silberbenzoat und triphos mit einer 2:1-Mischung aus S(Ph)SiMe 3 und S(SiMe 3 ) 2 bei À20 8C in diglyme (Diethylenglycoldimethylether) entsteht eine dunkelrote Lˆsung, aus der kleine rote nadelfˆr-mige Kristalle von 1 isoliert werden kˆnnen [Gl. (1)].Ph 3 CO 2 Ag þPhSðSiMe3 Þ=SðSiMe3 Þ2 þtriphos ! 1

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Cited by 83 publications

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Syntheses and Crystal Structures of the New Ag–S Clusters [Ag70S16(SPh)34(PhCO2)4(triphos)4] and [Ag188S94(PR3)30]

Syntheses and Crystal Structures of the New Ag–S Clusters [Ag70S16(SPh)34(PhCO2)4(triphos)4] and [Ag188S94(PR3)30]

Organometallic Nanoparticles of Metals or Metal Oxides

Synthesen und Kristallstrukturen der Ag-S-Clusterverbindungen [Ag70S16(SPh)34(PhCO2)4(triphos)4] und [Ag188S94(PR3)30]

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