Ligand chelation, P–C bond cleavage, and phenyl-group transfer in the reaction between RCCo3(CO)9 and 1,8-bis(diphenylphosphino)naphthalene (dppn): Syntheses and X-ray diffraction structures of PhCCo3(CO)4(μ-CO)3(dppn) and PhCCo3(CO)8[η1-PPh(OH)C10H6P(O)Ph2]

2007 ◽  
Vol 692 (5) ◽  
pp. 968-975 ◽  
Author(s):  
William H. Watson ◽  
Srikanth Kandala ◽  
Michael G. Richmond
2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.


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).


2017 ◽  
Vol 41 (7) ◽  
pp. 423-426 ◽  
Author(s):  
Chunhong Zheng ◽  
Guanming Liao ◽  
Congbin Fan ◽  
Renjie Wang ◽  
Shouzhi Pu

An indole-containing diarylethene with a trifluoromethyl function at the meta-position of the phenyl group attached to the thiophene moiety was synthesised. Its structure was determined by single-crystal X-ray diffraction analysis and its photochemical properties in solution and in the single crystalline phases were studied. The compound showed relatively high fluorescent modulation efficiency and cyclisation quantum yield.


1989 ◽  
Vol 44 (5) ◽  
pp. 543-547 ◽  
Author(s):  
Herbert W. Roesky ◽  
Uwe Otten ◽  
Regine Herbst ◽  
Mathias Noltemeyer

The reactions of 1,1,2,2-tetrafluoroethane-1,2-bisulfenyl-chloride 1 and symmetrical azines 2 yield the conjugated trans-diazenes 3 as deep-coloured solids. Unsymmetrical azines 4 react with 1 under elimination of hydrogen chloride to give 1,3-dithiolane-substituted azine derivatives as pale-coloured liquids. The crystal structure of 3b has been determined by single crystal X-ray diffraction. A participation of the phenyl group in the conjugated system is not observed in 3b.


2004 ◽  
Vol 59 (11-12) ◽  
pp. 1570-1578 ◽  
Author(s):  
Carsten Strohmann ◽  
Eric Wack

Bis(lithiomethyl)germanes, R2Ge(CH2Li)2, tris(lithiomethyl)germanes, RGe(CH2Li)3, and tetrakis( lithiomethyl)germane, Ge(CH2Li)4, were prepared by the reductive C-S bond cleavage with lithium naphthalenide (LiC10H8) or lithium p,p’-di-tert-butylbiphenylide (LiDBB) and characterized by trapping with Bu3SnCl. The bis(lithiomethyl)germanes were used for the synthesis of 1,1-dimethyl-3,3-diphenyl-1-germa-3-silacyclobutane, 1,1-diethyl-3,3-diphenyl-1-germa-3-silacyclobutane, 1,1,3,3-tetraphenyl-1-germa-3-silacyclobutane and 1,1,3,3-tetraphenyl-1,3-digermacyclobutane. The single-crystal X-ray diffraction studies of methyltris(phenylthiomethyl)germane and tetrakis(phenylthiomethyl)germane, starting materials for the corresponding poly(lithiomethyl) germanes, indicate tetrahedrally arranged substituents at the germanium atoms.


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