The Reaction of Cp*ReH6, Cp* = C5Me5, with Monoborane to Yield a Novel Rhenaborane. Synthesis and Characterization of arachno-Cp*ReH3B3H8

2002 ◽  
Vol 67 (6) ◽  
pp. 808-812 ◽  
Author(s):  
Sundargopal Ghosh ◽  
Alicia M. Beatty ◽  
Thomas P. Fehlner

The rhenaborane Cp*ReH3B3H8, which is generated by the reaction of Cp*ReH6 with BH3·THF, has been characterized spectroscopically in solution and by a single-crystal X-ray diffraction study in the solid state as a hydrogen-rich arachno-metallatetraborane.

2011 ◽  
Vol 66 (9) ◽  
pp. 947-952
Author(s):  
Meiling Xu ◽  
Yong Nie ◽  
Jinling Miao ◽  
Zhenwei Zhang ◽  
Bin Peng ◽  
...  

The reactions of the dithiolato-o-carborane salt (Et3NH)2(S2C2B10H10) (2) with alkyl halides BrCH2CH=CH2, BrCH2CH2CH2Cl and C6H5CH2Cl, afford the o-carboranyl-bisthioether derivatives 3a - c, which have been characterized by IR and NMR (1H, 13C, 11B) spectroscopy, mass spectrometry, and single-crystal X-ray diffraction (3c). The photoluminescent properties of the known compound 3c has been investigated. It exhibits a violet (chloroform solution) or blue (solid state) emission when excited with UV light.


1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.


2002 ◽  
Vol 57 (6) ◽  
pp. 621-624 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Heinrich Nöth ◽  
Thomas M. Klapötke ◽  
Max Suter

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.


2007 ◽  
Vol 62 (3) ◽  
pp. 427-438 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Luigi Busetto ◽  
Fabio Marchetti ◽  
Magda Monari ◽  
Stefano Zacchini ◽  
...  

The diiron aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (R = Xy1, 1a; R = Me, 1b; R = CH2Ph, 1c; Xy1 = 2,6-Me2C6H3) undergo replacement of the coordinated nitrile by halides, diethyldithiocarbamate, and dicyanomethanide to give [Fe2{μ-CN(Me) (R)}(μ-CO)(CO)(X)(Cp)2] complexes (R = Me, X = Br, 4a; R = Me, X = I, 4b; R = CH2Ph, X = Cl, 4c; R = CH2Ph, X = Br, 4d; R = CH2Ph, X = I, 4e; R = Xy1, X = SC(S)NEt2, 5a; R = Me, X = SC(S)NEt2, 5b; R = Xy1, X = CH(CN)2, 7), in good yields. The molecular structure of 5a shows an unusual η1 coordination mode of the dithiocarbamate ligand. Similarly, treatment of [M2{μ-CN(Me) (R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (M = Fe, R = Xy1, 1a; M = Fe, R = Me, 1b; M = Ru, R = Xy1, 2a; M = Ru, R = Me, 2b) with a series of phosphanes generates the cationic complexes [M2{μ- CN(Me)(R)}(μ-CO)(CO)(P)(Cp)2][SO3CF3] (M = Fe, R = Xy1, P = PPh2H, 6a; M = Fe, R = Xy1, P = PPh3, 6b; M = Fe, R = Xy1, P = PMe3, 6c; M = Fe, R = Me, P = PMe2Ph, 6d; M = Fe, R = Me, P = PPh3, 6e; M = Fe, R = Me, P = PMePh2, 6f; M = Ru, R = Xy1, P = PPh2H, 6g; M = Ru, R = Me, P = PPh2H, 6h), in high yields. The molecular structure of 6a has been elucidated by an X-ray diffraction study. The reactions of [Fe2{μ-CN(Me)(Xyl)}(μ-CO)(CO)(NCR′)(Cp)2][SO3CF3] [R′ = Me, 1a; R′ = tBu, 3] with PhLi and PPh2Li yield [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(Ph)(Cp)2] (8) and [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(PPh2)(Cp)2] (9), respectively. The molecular structure of 8 has been ascertained by X-ray diffraction. Conversely, the reaction of 1a with MeLi generates the aminoalkylidene compound [Fe2{C(Me)N(Me)(Xy1)}(μ-CO)2(CO)(Cp)2] (10).Finally, the acetone complex [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(OCMe2)(Cp)2][SO3CF3] (12) reacts with lithium acetylides to give complexes [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(C≡CR)(Cp)2] (R = p-C6H4Me, 11a; R = Ph, 11b; R = SiMe3, 11c), in high yields. Filtration through alumina of a solution of 11a in CH2Cl2 results in hydration of the acetylide group and C-Si bond cleavage, affording [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO){C(O)Me}(Cp)2] (12).


2010 ◽  
Vol 44-47 ◽  
pp. 2299-2306
Author(s):  
H.M.Noor Ul Huda Khan Asghar ◽  
M. Asghar ◽  
M.S. Awan

Polycrystalline spintronic material (Cd0.55Hg0.45Te) was synthesized by conventional solid state reaction. The samples ( = 5 mm and T = 1.5 mm) were prepared by uni-axial pressing. Samples were melted at 800°C for 3-2 hours. For chemical analyses, surface morphology and structural analyses, scanning electron microscopy (SEM) equipped with EDX system and X-ray diffraction studies were performed. XRD confirmed the cubic crystal structure. The Lattice constant of (Cd0.55Hg0.45Te) as determined by XRD was 0.6464 nm. The Miller indices (hkl) have been found by using crystallography method. The observed planes were (200), (210) and (331). The EDX analyses showed the typically compositions: Te 24.8% Cd 14.8% Al 5% and O2 46.4 % & C 9% (3 hours treatment) and Te 28.1% Cd 16% Al 4.1% and O2 39.3 %, Si 0.360% & C 12.1% (2 hours treatment) however we could not find any representative peak for Hg in all of the EDX analyses.


Science ◽  
2017 ◽  
Vol 355 (6323) ◽  
pp. 374-376 ◽  
Author(s):  
Chong Zhang ◽  
Chengguo Sun ◽  
Bingcheng Hu ◽  
Chuanming Yu ◽  
Ming Lu

Pentazole (HN5), an unstable molecular ring comprising five nitrogen atoms, has been of great interest to researchers for the better part of a century. We report the synthesis and characterization of the pentazolate anion stabilized in a (N5)6(H3O)3(NH4)4Cl salt. The anion was generated by direct cleavage of the C–N bond in a multisubstituted arylpentazole using m-chloroperbenzoic acid and ferrous bisglycinate. The structure was confirmed by single-crystal x-ray diffraction analysis, which highlighted stabilization of the cyclo-N5ˉ ring by chloride, ammonium, and hydronium. Thermal analysis indicated the stability of the salt below 117°C on the basis of thermogravimetry-measured onset decomposition temperature.


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