Synthesis and Crystal Structure of Unprecedented Oxo/Hydroxo-Bridged Polynuclear Gallium(III) Aqua Complexes

Gerasko, О. А.; Mainicheva, Е. А.; Naumov, Dmitry Yu.; Kuratieva, Natalia V.; Sokolov, Maxim N.; Fedin, Vladimir P.

doi:10.1021/ic0502271

Cited by 45 publications

(37 citation statements)

References 15 publications

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“…36 ]·MeCN, [42] though quite unlike that of a hydrolytic Ga 32 array. [43] The structure is closely related to that of the recently reported [44] Co 32 (thiacalix [4]arene) 6 complex, although that appears to contain both Co II and Co III centres, whereas the present complex appears to contain only Ni II . The Co complex was prepared by a solvothermal method (at 130°C), which has the obvious advantage of rapid kinetics compared to the procedure we have used to obtain the Ni complex but this may also have led to the partial oxidation and extensive hydrolysis, explaining why a much simpler true Co II complex was obtained in our earlier work.…”

Section: Ni 6 (L)(lh) 2 (Lh 2 )·4mecn·6h 2 O ϵ [{Ni 4 (H 2 O)(l·mecn)supporting

confidence: 79%

“…Variata: Data were measured at room-temperature (293 K), crystal degradation occurring at "low"-temperature. Disordered tert-butyl group components 12,14,21,23,43,44 were modelled over pairs of sites, occupancies set at 0.5 after trial refinement. Large residues in difference maps were modelled as water molecule oxygen atoms (associated hydrogen atoms not located); significant residual density was insusceptible of meaningful modelling and was suppressed using "SQUEEZE".…”

Section: Variatamentioning

confidence: 99%

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Systematic Structural Coordination Chemistry of p‐tert‐Butyltetrathiacalix[4]arene: Further Complexes of Transition‐Metal Ions

et al. 2010

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Section: Ni 6 (L)(lh) 2 (Lh 2 )·4mecn·6h 2 O ϵ [{Ni 4 (H 2 O)(l·mecn)supporting

confidence: 79%

Section: Variatamentioning

confidence: 99%

Systematic Structural Coordination Chemistry of p‐tert‐Butyltetrathiacalix[4]arene: Further Complexes of Transition‐Metal Ions

et al. 2010

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“…[28][29][30][31] Previous studies in our group have evidenced the potential of using CB [6] for isolation of polynuclear Zr, Hf, Sr, U, Mo, Al, Ga, and In aqua complexes. [32][33][34][35] As a rule, polynuclear cationic metal aqua complexes are highly charged, and coordinated water mole-cules in these complexes possess rather strong acidic properties, which favor the formation of hydrogen bonds with the carbonyl oxygen atoms of cucurbit [6]uril. Last year we managed to isolate and structurally characterize a tetranuclear lanthanide complex with CB [6] from aqueous solutions of holmium(III) nitrate for the first time.…”

Section: Introductionmentioning

confidence: 99%

Tetranuclear Lanthanide Aqua Hydroxo Complexes with Macrocyclic Ligand Cucurbit[6]uril

et al. 2008

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Registro de acceso restringido Este recurso no está disponible en acceso abierto por política de la editorial. No obstante, se puede acceder al texto completo desde la Universitat Jaume I o si el usuario cuenta con suscripción. Registre d'accés restringit Aquest recurs no està disponible en accés obert per política de l'editorial. No obstant això, es pot accedir al text complet des de la Universitat Jaume I o si l'usuari compta amb subscripció. Restricted access item This item isn't open access because of publisher's policy. The full--text version is only available from Jaume I University or if the user has a running suscription to the publisher's contents.

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“…Crystallization periods of months or even years are typical. [3][4][5][6] Owing to these difficulties, relatively few discrete Group 13 metal-hydroxide clusters have been synthesized, though several striking examples of aluminum [3,4,6,7] and gallium [1,5,8,9] complexes have been reported. Both hydrated clusters and those stabilized by organic ligands are known, with a larger variety of ligand-supported clusters having been isolated, owing to enhanced stability resulting from lower charge density.…”

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confidence: 99%

Synthesis of Heterometallic Group 13 Nanoclusters and Inks for Oxide Thin‐Film Transistors

et al. 2008

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We have recently reported high-yielding syntheses of two inorganic Group 13 metal-hydroxide nanoclusters: [Ga 13 (m 3 -OH) 6 (m-OH) 18 (H 2 O) 24 (NO 3 ) 15 ] ("flat" Ga 13 , 1, Figure 1) and [Al 13 (m 3 -OH) 6 (m-OH) 18 (H 2 O) 24 (NO 3 ) 15 ] ("flat" Al 13 ). [1,2] The {M(m 3 -OH) 6 M 6 (m-OH) 6 } central fragment of these clusters forms a planar core with six additional M(H 2 O) 4 groups bound to the core by two m-OH bridges. The outer metal ions alternate above and below the plane formed by the central seven metal ions. Prior synthetic preparation of Group 13 metal-hydroxide compounds such as these has proven difficult. Their syntheses often require caustic or acidic conditions and elevated temperatures and pressures to provide clusters, often in low yields. Crystallization periods of months or even years are typical. [3][4][5][6] Owing to these difficulties, relatively few discrete Group 13 metal-hydroxide clusters have been synthesized, though several striking examples of aluminum [3,4,6,7] and gallium [1,5,8,9] complexes have been reported. Both hydrated clusters and those stabilized by organic ligands are known, with a larger variety of ligand-supported clusters having been isolated, owing to enhanced stability resulting from lower charge density. [3] In the case of these inorganic and ligand-supported compounds, neither heterometallic nor indium-containing clusters are known. However, in the case of Keggin-Al 13 clusters, the central tetrahedral metal can be substituted, forming M 1 Al 12 structures (M = Al, Ga, or Ge, with others suggested).[10-13] To our knowledge, no heterometallic Group 13 metal-hydroxide clusters with multiple substitution have been reported. Furthermore, the lowyielding, challenging syntheses often associated with these clusters have prevented attempts at exploring applications requiring large quantities of such compounds. In order to address synthetic difficulties and to explore the use of these clusters as precursors for materials, we have developed an improved synthesis of heterometallic Group 13 nanoclusters.There has been recent interest in the use of nanoscale cluster precursors to synthesize new materials. [14][15][16][17] The difficult syntheses of Group 13 metal-hydroxide clusters have mostly prevented their use in these applications. Most solution precursors for printed oxide films involve controlled hydrolysis of metal-organic compounds and the condensation of metal-hydroxo sols that are then pyrolyzed to form the oxide. Such films are beset by a variety of density, defect, and segregation issues relating to the inhomogeneous nature of the sol, retention of significant organic components, or oxygen nonstoichiometry associated with organic burnout. From this perspective, soluble all-inorganic, heterometallic hydroxo clusters, such as the "flat" M 13 system, provide model precursors and an entirely inorganic, rapid, low-volume-loss condensation pathway, eliminating the aforementioned detrimental effects of organic moieties.Herein, we present a new heterometallic gallium-...

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Synthesis and Crystal Structure of Unprecedented Oxo/Hydroxo-Bridged Polynuclear Gallium(III) Aqua Complexes

Cited by 45 publications

References 15 publications

Systematic Structural Coordination Chemistry of p‐tert‐Butyltetrathiacalix[4]arene: Further Complexes of Transition‐Metal Ions

Systematic Structural Coordination Chemistry of p‐tert‐Butyltetrathiacalix[4]arene: Further Complexes of Transition‐Metal Ions

Tetranuclear Lanthanide Aqua Hydroxo Complexes with Macrocyclic Ligand Cucurbit[6]uril

Synthesis of Heterometallic Group 13 Nanoclusters and Inks for Oxide Thin‐Film Transistors

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