The selenium adducts of germa- and stanna-closo-dodecaborate can coordinate at platinum via the selenium atom and result in the products [Pt(dppp)(Se-TB(11)H(11))(2)](2-) (T = Ge, Sn) (dppp = 1,3-bis(diphenylphosphino)propane). The monomeric tin compound [Pt(dppp)(Se-SnB(11)H(11))(2)](2-) is converted to a dimeric complex [Pt(2)(dppp)(2)(μ(2),μ'(2)-η(2)-Se(2)SnB(11)H(11))]. The new compounds were characterized by NMR spectroscopy in solution ((1)H, (11)B, (13)C, (31)P, (77)Se, (119)Sn, (195)Pt), elemental analysis and single crystal X-ray diffraction.
An exploratory study of the structure and composition of furnace-ash deposits was carried out using optical metallography, electron microprobe analysis, scanning electron microscopy, and energy-dispersive X-ray analysis. The results of these analyses were supplemented by studies of particulate melting temperatures using hot-stage microscopy to measure melting temperatures, and energy-dispersive X-ray analyses to measure composition of melted particles. It was found that the general structure of the ash deposit was a matrix of glassy, spherical particles having a wide range of compositions in which unfused particles containing iron oxide and calcium oxide were dispersed. At the imprint of the tube surface a considerable concentration of calcium, sulfur, and iron was found. Near the fused outer surface of the deposit, the glassy materials had melted into a porous, glassy slag containing spherical globules of iron oxide combined with other materials. There were no systematic compositional gradients from the tube surface to the fused outer layer except for the sulfur layer found only at the tube surface. However, there were significant differences in composition from particle to particle, and these differences were similar to those found in the coal mineral matter as isolated by low-temperature ashing. Single particles of low-temperature ash were found having low fusion temperatures, in the range of fusion temperatures for particles in furnace ash. Thus, the glassy spheres found in furnace deposits could originate from single coal particles, without the need for interactions among coal particles or ash particles.
Homoleptic Coinage Metal Compounds of Group(IV)heteroborates. -The crystal structures of (III), (V), (VII), and (IX) are determined by single crystal XRD. (V)·2.5DMF and (IX)·6MeCN crystallize in the space group P1 with Z = 2 and Z = 1, respectively. (III)·2MeCN crystallizes in the space group Pnma with Z = 4, and (VII)·2MeCN in the space group P21/n with Z = 2. In the oligonuclear compounds (VII) and (IX) silver and gold aggregation occurs under formation of metal-metal bonds. Furthermore, the germa-closo-dodecaborate exhibits a hitherto unknown μ3-bridging coordination mode connecting three Ag atoms in (IX). -(SCHUBERT, H.; DIMMER, J.-A.; KUECHLE, F.-R.; EICHELE, K.; WESEMANN*, L.; Inorg. Chem. 50 (2011) 2, 664-670, http://dx.doi.org/10.1021/ic102118n ; Inst. Anorg. Chem., Eberhard-Karls-Univ., D-72076 Tuebingen, Germany; Eng.) -W. Pewestorf 13-023
Synthesis and Structure of Tetrameric German-closo-dodecaborate Silver Halides. -Compounds (III) and (VI) crystallize in the monoclinic space group C2/c with Z = 4 (single crystal XRD). The [{AgX(GeB11H11)}4] 8-(X: Cl, Br) exhibit cubane type structures with alternating Ag and X corners. (III) and (VI) are further characterized by 11 B NMR spectroscopy. -(DIMMER, J.-A.; WESEMANN*, L.; Z. Anorg. Allg. Chem. 637 (2011) 6, 643-645, http://dx.
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