Crystal structure of bis(ethylenediamine)cuprate ethylenediaminetetraacetate-zinc(II) tetrahydrate

All-Union Research Institute for Chemical Reagents and High-Purity Chemicals. Translated from Zhurnal Strukturnoi Khimii, Vol. 31, No. 5, pp. 140–143, September–October, 1990.     

Stereoselective electrocatalytic cyclization of 3-substituted 2,2-dicyanocyclopropane-1,1-dicarboxylic acid esters to form 6-substituted (1R,5R,6R)*-4,4-dialkoxy-5-cyano-2-oxo-3-azabicyclo[3.1.0]hexane-1-carboxylic acid esters

Electrolysis of 3-substituted 2,2-dicyanocyclopropane-1,1-dicarboxylic acid esters in alcohols in an undivided cell in the presence of NaBr or NaOAc afforded 6-substituted (1R,5R, 6R)*-4,4-dialkoxy-5-cyano-2-oxo-3-azabicyclo[3.1.0]hexane-1-carboxylic acid esters in 80–95% yields. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 102–107, January, 2006.     

Molecular Complexes of Phenols with Dicyclohexylamine

The Mannich reaction of 2,4-di-tert-butylphenol with dicyclohexylamine was found to involve formation of a stable 1:1 molecular complex between the phenol and amine. The complex does not change on melting, sublimation, and chromatography on silica gel. Its structure was determined by X-ray analysis. Stable 1:1 complexes of dicyclohexylamine with a series of substituted phenols were synthesized; exceptions were 2,6-disubstituted phenols with bulky substituents.     

N-Amino Derivatives of Condensed Imidazole Systems

The previously unknown 1-amino- and 3-aminonaphtho[1,2-d]imidazoles, 1-aminonaphtho[2,3-d]imidazole, 1-aminophenanthro[9,10-d]imidazole and the N-amino-N'-methylimidazolium picrates corresponding to them have been obtained by direct amination of a series of condensed imidazoles with O-picrylhydroxylamine. An X-ray structural investigation of 1-amino-3-methylnaphtho[1,2-d]imidazolium picrate showed that, in difference to 1-aminobenzimidazolium salts, a conformation exists in it in which the hydrogen atoms of the N-NH₂ group are directed to the side of the meso carbon atom.     

Chloroaqua Complexes [M3S4(H2O)9?xClx](4?x)+ (M = Mo, W; x = 4, 6, 7) and Their Supramolecular Compounds with Cucur[8]uril

Compounds of trigonal cluster chloroaqua complexes with cucurbit[8]uril were synthesized by slowly evaporating HCl solutions of chalcogenides heterometallic cubane cluster complexes of molybdenum and tungsten with cucurbit[8]uril in air; the complexes were characterized by X-ray diffraction analysis: (H₃O)₈[Mo₃S₄(H₂O)_2.5Cl_6.5]₂Cl(PdCl₄)·(C₄₈H₄₈N₃₂O₁₆)· 29H₂O (a = 13.3183(17) Å, b = 13.7104(18) Å, c = 18.225(3) Å; α = 80.263(3)°, β = 77. 958(3)°, γ = 87.149(4)°, V = 3207.4(7) ų, space group P , Z = 1, ρ(calc) = 1.900 g/cm³), (H₃O)₄ [Mo₃S₄(H₂O)₃Cl₆]₂·(C₄₈H₄₈N₃₂O₁₆)₃·68H₂O (a = 21.413(6) Å, c = 49.832(10) Å; γ = 120°, V = 19788(8) ų, space group R , Z = 3, ρ(calc) = 1.695 g/cm³), (H₃O)₆ [Mo₃S₄(H₂O)₃Cl₆]₂Cl₂·(C₄₈H₄₈N₃₂O₁₆)·12H₂O (a = 15.881(2) Å, b = 17.191(2) Å, c = 23.276(4) Å; β = 98.865(15)°, V = 6278.7(15) ų, space group P2₁/c, Z = 2, ρ(calc) = 1.638 g/cm³), [W₃S₄(H₂O)₅Cl₄]₂·(C₄₈H₄₈N₃₂O₁₆)₃·35H₂O (a = 21.038(3) Å; α = 61.20(1)°, V = 6762.0(14) ų, space group R , Z = 1, ρ(calc) = 1.582 g/cm³). The [Mo₃S₄(H₂O)₃Cl₆]²⁻ anion complex was isolated as three geometrical isomers.Original Russian Text Copyright © 2004 by E. V. Chubarova, D. G. Samsonenko, H. G. Platas, F. M. Dolgushin, A. V. Gerasimenko, M. N. Sokolov, Z. A. Starikova, M. Yu. Antipin, and V. P. Fedin__________Translated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 6, pp. 1049–1058, November–December, 2004.     

Heterometallic hafnocene(+4) aluminum hydride complex [(ηp5-C5H5)2Hf(H)(μ2-H)Al(H)Br(μ2-OC4H9)]2

The [Cp₂HfH₂Al(H)Br(OBu)]₂ complex (1) was prepared by the reaction of Cp₂HfBr₂ with AlH₃ in THF and characterized by X-ray crystallography. The formation of dinuclear complex 1 proceeds through the intermediate formation (as a result of cleavage of THF molecules) of the >Al(μ-OBu)₂Al< fragment. The latter is linked to two hafnocene dihydride molecules by the Hf-H-Al hydrogen bridges. The Hf atom in complex 1 has a 16-electron environment.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2082–2085, October, 2004.     

Photochromic dihetarylethenes. 13. Optimization of conditions for the acylation of 2,5-dimethylthiophene with squaric acid dichloride

The conditions for acylation of 2,5-dimethylthiophene with squaric acid dichloride were optimized, and 3,4-bis(2,5-dimethylthiophen-3-yl)cyclobut-3-ene-1,2-dione was obtained in good yield. X-ray diffraction analysis demonstrated that the by-product has the structure of 1a,1b-dichloro-5-(2,5-dimethylthiophen-3-yl)-3-hydroxy-4,5a-dimethyl-1b,4a,5,5a-tetrahydro-1aH-1-thiacyclopropa[a]pentalen-2-one.