X-Ray crystal structure of the 1 : 2 adduct of aluminium trichloride with acetonitrile; an interesting example of auto-complex formation

Author(s):  
Judith A. K. Howard ◽  
Lesley E. Smart ◽  
Christopher J. Gilmore
1987 ◽  
Vol 42 (7) ◽  
pp. 828-834 ◽  
Author(s):  
W. Frank ◽  
B. Dincher

Abstract The crystalline compounds [(CH3C6H5)2Hg,][AlCl4]2 (1), [(1,2-(CH3)2C6H4)2Hg2][AlCl4]2(2), [(1,3,5-(CH3)3C6H3)2Hg2][AlCl4]2 (3), [1,2,4,5-(CH3)4C6H2Hg2][AlCl4]2 (4) and [((CH3)6C6)2Hg2][AlCl4]2-CH3C6H5 (5) have been prepared from mercury(I)chloride, aluminium trichloride and the corresponding arenes and characterized by elem ental analysis. The crystal structure of 5 has been determ ined from single crystal X-ray diffraction data and refined to R - 0.093 for 3269 unique reflections. Crystal data: monoclinic, space group P21/c, a = 2116(1), b = 1095.1(7), c = 1880(1) pm, β - 104,9(1)°, Z = 4. Each atom of a central Hg2 unit (Hg -Hg distance 251.5 pm) is asymmetrically complexed by hexamethylbenzene, the Hg - Carene distances being in the range from 241 to 340 pm. Two distorted AlCl4 tetrahedra complete a “molecular” [arene2Hg2][AlCl4]2 unit. The shortest Hg-Cl distances are 310 and 312 pm, respectively.


1987 ◽  
Vol 16 (12) ◽  
pp. 2317-2320 ◽  
Author(s):  
Fumio Toda ◽  
Koichi Tanaka ◽  
Jose Elguero ◽  
Luigi Nassimbeni ◽  
Margaret Niven

1988 ◽  
Vol 17 (6) ◽  
pp. 1061-1064 ◽  
Author(s):  
Fumio Toda ◽  
Koichi Tanaka ◽  
Jose Elguero ◽  
Zafra Stein ◽  
Israel Goldberg

1990 ◽  
Vol 68 (7) ◽  
pp. 1140-1144 ◽  
Author(s):  
Stephen John Angyal ◽  
Donald Chadwick Craig ◽  
Jacques Defaye ◽  
Andrée Gadelle

Di-D-fructose 2′, 1:2,1′-dianhydrides form complexes with metal cations if the two anomeric carbon atoms have the same configuration. Such anomers have the central 1,4-dioxane ring in a flexible form; complex formation involves O-1, O-1′, O-3, and O-3′, as confirmed by the X-ray crystal structure of the strontium complex of the β,β-dipyranose anomer. The α,β-anomers, and dianhydrides containing only furanose rings, do not form such complexes. Keywords: difructose dianhydrides, complex formation with cations, crystal structure of complex, chromatographic separation on ion-exchange resins.


2008 ◽  
Vol 62 (4) ◽  
Author(s):  
Stefan Stucky ◽  
Nadine Koch ◽  
Uwe Heinz ◽  
Kaspar Hegetschweiler

Abstract3,5-Bis(2-hydroxyphenyl)-1H-1,2,4-triazole (H2La) and 4-[3,5-bis(2-hydroxyphenyl)-1H-1,2,4-triazol-1-yl]benzoic acid (H3Lb) have been prepared, and crystal structure of the intermediate 2-(2-hydroxyphenyl)-4H-1,3-benzoxazin-4-one has been determined. Temperature dependent 1H NMR spectroscopic measurements of H2La indicated dynamic behavior with the equilibrium between the two asymmetric tautomers. For H3Lb, pD-dependent 1H NMR spectroscopic measurements showed small but characteristic shifts in the range of 0 ≤ pD ≤ 1, indicative of a triazole nitrogen atom protonation; the corresponding pK a of 0.98 ± 0.04 was determined by spectrophotometric titrations. (H2O, 26°C, 1 M KCl/HCl). Formation of [FeIII(La)]+ (pH 2.5) and [FeIII(La)2]− (pH > 6) was verified by UV-Vis spectroscopy. Complex formation of H3Lb with Al3+ and VO2+ was investigated by 1H NMR spectroscopic titration and cyclic voltammetry, respectively. Single crystals of the phenoxo bridged [VVO(HLb)(EtO)]2·2EtOH were characterized by X-ray structural analysis.


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