The new thioaluminogermanate Na(AlS)(GeS) (1) was successfully synthesized by a direct combination reaction. The compound crystallizes in the monoclinic space group P2/ n (no. 14) with unit cell parameters a = 6.
View Article and Find Full Text PDFHigh surface area macroporous chalcogenide aerogels (chalcogels) MAuGeS (M = Co, Ni) were prepared from KAuGeS precursor and Co(OAc) or NiCl by one-pot sol-gel metathesis reactions in aqueous media. The MAuGeS-chalcogels were screened for catalytic intramolecular hydroamination of 4-pentyn-1-amine substrate at different temperatures. 87% and 58% conversion was achieved at 100 °C, using CoAuGeS- and NiAuGeS-chalcogels respectively, and the reaction kinetics follows the first order.
View Article and Find Full Text PDFSynthesis, structure, and olefin metathesis activity of a surface complex [(≡Si-O-)W(═O)(CH)-ImN] (4) (Im = 1,3-bis(2,6-diisopropylphenyl)imidazolin-2-iminato) supported on silica by a surface organometallic chemistry (SOMC) approach are reported. The reaction of N-silylated 2-iminoimidazoline with tungsten(VI) oxytetrachloride generated the tungsten oxo imidazolin-2-iminato chloride complex [ImNW(═O)Cl] (2). This was grafted on partially dehydroxylated silica pretreated at 700 °C (SiO) to afford a well-defined monopodal surface complex [(≡Si-O-)W(═O)Cl-ImN] (3).
View Article and Find Full Text PDFActa Crystallogr E Crystallogr Commun
December 2016
The title salt, [Mn(CHOS)]I, is made up from discrete [Mn(DMSO)] (DMSO is dimethyl sulfoxide) units connected through non-classical hydrogen bonds to linear I tetra-iodide anions. The Mn ion in the cation, situated on a position with site symmetry -3., is octa-hedrally coordinated by O atoms of the DMSO mol-ecule with an Mn-O distance of 2.
View Article and Find Full Text PDFTin(II) ketoacidoximates of the type [HON=CRCOO]2Sn (R = Me 1, CH2Ph 2) and (MeON=CMeCOO)3Sn](-) NH4(+)·2H2O 3 were synthesized by reacting pyruvate- and hydroxyl- or methoxylamine RONH2 (R = H, Me) with tin(II) chloride dihydrate SnCl2·2H2O. The single crystal X-ray structure reveals that the geometry at the Sn atom is trigonal bipyramidal in 1, 2 and trigonal pyramidal in 3. Inter- or intramolecular hydrogen bonding is observed in 1-3.
View Article and Find Full Text PDFActa Crystallogr E Crystallogr Commun
March 2015
In the title compound, [FeIr(C5H5)(C20H14N3)Cl3]·2CH3CN, the central Ir(III) atom is sixfold coordinated by three chloride ligands and three terpyridine N atoms in a slightly distorted octa-hedral fashion. The terpyridine ligand is functionalized at the 4'-position with a ferrocenyl group, the latter being in an eclipsed conformation. In the crystal, mol-ecules are stacked in rows parallel to [001], with the aceto-nitrile solvent mol-ecules situated between the rows.
View Article and Find Full Text PDFThe fundamental properties and ultimate performance limits of organolead trihalide MAPbX3 (MA = CH3NH3(+); X = Br(-) or I(-)) perovskites remain obscured by extensive disorder in polycrystalline MAPbX3 films. We report an antisolvent vapor-assisted crystallization approach that enables us to create sizable crack-free MAPbX3 single crystals with volumes exceeding 100 cubic millimeters. These large single crystals enabled a detailed characterization of their optical and charge transport characteristics.
View Article and Find Full Text PDFThe commercial polymeric anhydride poly(methyl vinyl ether-alt-maleic anhydride) (PVM/MA) is converted by reaction with NaOH to give poly(methyl vinyl ether-alt-mono-sodium maleate) (PVM/Na-MA). By addition of AgNO-solution, the formation of the silver(i) supramolecular polymer hydrogel poly[methyl vinyl ether-alt-mono-sodium maleate]·AgNO is reported. Freeze-dried samples of the hydrogel show a mesoporous network of polycarboxylate ligands that are crosslinked by silver(i) cations.
View Article and Find Full Text PDFWe present a promising approach in synthetic chalcogel chemistry that is extendable to a broad variety of inorganic spacers. Polychalcogenide aerogels with ion-exchange properties are demonstrated in cobalt polysulfide. The new materials show a broad range of pore sizes and high surface area of 483 m(2)/g.
View Article and Find Full Text PDFThe new compounds Rb(3)(AlQ(2))(3)(GeQ(2))(7) [Q = S (1), Se (2)] feature the 3D anionic open framework [(AlQ(2))(3)(GeQ(2))(7)](3-) in which aluminum and germanium share tetrahedral coordination sites. Rb ions are located in channels formed by the connection of 8, 10, and 16 (Ge/Al)S(4) tetrahedra. The isostructural sulfur and selenium derivatives crystallize in the space group P2(1)/c.
View Article and Find Full Text PDFThe first discrete anionic indium thiophosphate complexes are reported. The structures of K(6)[In(PS(4))(1.5)(PS(5))(1.
View Article and Find Full Text PDFThe new thiophosphate salt K(4)In(2)(PS(4))(2)(P(2)S(6)) (1), the selenophosphate salts K(5)In(3)(mu(3)-Se)(P(2)Se(6))(3) (2), K(4)In(4)(mu-Se)(2)(P(2)Se(6))(3) (3), and the mixed seleno-/thiophosphate salt K(4)In(4)(mu-Se)(P(2)S(2.36)Se(3.64))(3) (4) are described.
View Article and Find Full Text PDFThe synthesis and structures of the three new compounds, KPbPS(1.84)Se(2.16) (1), RbPbPS(1.
View Article and Find Full Text PDF1,1'-Difunctionalised ferrocene derivatives have been studied, which contain groups suitable for chemisorption on gold substrates, namely -NC, -PR(2) as well as a range of sulfur-containing units like -NCS, -SR, and thienyl. Thin films on gold have been fabricated from solution with most of these adsorbate species. Film thickness, composition and structure were investigated primarily by X-ray photoelectron and near-edge X-ray absorption fine-structure spectroscopy.
View Article and Find Full Text PDFThe first reactions of the trinuclear oxygen-centred iron carboxylate [Fe(3)(mu(3)-O)(mu(2)-piv)(6)(H(2)O)(3)](piv) (piv=(t)BuCOO(-)) with the neutral ligand precursor [RP(S)(mu-S)](2) (R=4-anisyl) are reported.
View Article and Find Full Text PDFThe structures of the new compounds [Cu8(Ph2As2Se2)2(PhAsSe2)2(dppm)4] (1) (dppm = bis-diphenylphosphinomethane), [Cu4(Ph2As2Se2)2(PPh3)4] (2), [{K(18-crown-6)}2(PhAsSe3)] (3), [Na12(PhAsSe3)6(15-crown-5)6] (4) and 1/x[Na2(PhAsSe3)(thf)(H2O)3]x (5) are reported. 2-5 were prepared by reactions of metal thiolates with [(PhAs)2(mu-Se)(mu-Se2)].
View Article and Find Full Text PDFDisorder of silver atoms and high cation mobility are commonly observed and closely coupled features in silver chalcogenides. The ligand-stabilized cluster [Ag28(micro6-S)2{ArP(O)S2}12(PPh3)12] (1) (Ar=4-anisyl), with a total of 666 atoms, displays in its X-ray structure highly localized disorder at two core silver atoms. To explore the nature of this disorder, we have applied density functional methods to its internal structure and flexibility.
View Article and Find Full Text PDFThree reactions of Cu(i) thiolates and Woollins' reagent (W.R.) give rise to novel copper complexes with unusual P/Se anions.
View Article and Find Full Text PDFThe aim of this paper is to introduce a synthetic concept suitable for the preparation of a broad variety of compounds. The so-called anhydride route (in this article the term anhydride is used for compounds derived from corresponding acids by formal loss of H2O, H2S and H2Se) has so far led to a range of unusual Group 15/16 ligands in oligomeric and polymeric environments. Commonly, reactions of neutral precursor molecules, for example, [{RP(S)(mu-S)}2] (R=4-anisyl) Lawesson's reagent or [{PhP(Se)(mu-Se)}2] Woollins's reagent and metal salts are performed to result in novel coordination compounds in which ligands and metal atoms form coordination oligomers and polymers.
View Article and Find Full Text PDFA route to organometallic polymers and oligomers is described using metal complexes with P/S-ligands as examples.
View Article and Find Full Text PDFTreatment of [Et4N]2[WSe4] with a 1:1 mixture of AgNO3 and PCy3 (Cy = cyclohexyl) in the absence of iodide afforded a linear trinuclear compound [(mu-WSe4)(AgPCy3)2] (1). A similar reaction in the presence of iodide gave rise to the isolation of the cubanelike compound [(mu3-WSe4)Ag3(PCy3)3(mu3-I)] (2). Treatment of [Et4N]2[WSe4] with AgI in the presence of bidentate phosphine ligands bis(diphenylphosphino)amine (dppa) and bis(diphenylphosphino)methane (dppm) afforded the tetranuclear compounds [(mu3-WSe4)Ag3(mu-I)(mu-dppa)2] (3) and [(mu3-WSe4)Ag3(mu3-I)(mu-dppm)2] (4), respectively, which exhibit an open butterfly configuration.
View Article and Find Full Text PDFThe characterisation of a series of compounds obtained from Woollins' reagent (W.R.) offers a novel approach to organometallic coordination polymers.
View Article and Find Full Text PDFThe synthesis of [(PhAs)2(micro-S2)(micro-S)] and its reactions to form novel Cu(I) complexes are reported, together with a new cleavage reaction of disulfides by Cu(I) thiolates and tertiary phosphines.
View Article and Find Full Text PDFNine new compounds containing PS ligands of the types [P(OtBu)S3]2-, [ArP(StBu)S2]- and [ArP(OtBu)S2]- are reported (Ar = 4-anisyl). It is demonstrated that the topology of alkali metal ion and ligand composition influence the structure of supramolecular arrangements.
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