Monique Perrin

Synthesis, X-ray crystal structure and complexation properties towards metal ions of new thiacalix[4]arenes

Abstract p-tert-Butyl-tetrakis[(methylcarbonyl)methoxy]tetrathiacalix[4]arene and p-tert-butyl-tetrakis[(benzoyl)methoxy]tetrathiacalix[4]arene were prepared and their conformation was established by X-ray crystallography. p-tert-Butyl-tetrakis[(diethylamide)methoxy]tetrathiacalix[4]arene was also synthesized. The ability of these three macrocycles to bind metal ions was investigated via a solvent extraction study.

Synthesis of new 1,2,4-oxadiazolidin-3-ones by cycloaddition of 2-alkyl-3-aryloxaziridines with chlorosulfonylisocyanate

Abstract 2-Alkyl-4-chlorosulfonyl-5-aryl-1,2,4-oxadiazolidin-3-ones 5 were prepared via cycloaddition of 2-alkyl-3-aryloxaziridines 3 with chlorosulfonylisocyanate. The structure of 5 was proved by a crystal X-ray analysis. Hydrolysis of 5 in the presence of triethylamine afforded 2-alkyl-5-aryl-1,2,4-oxadiazolidin-3-ones 6 .

Bis-ferrocene derivatives of bridged calix[4]arenes: syntheis, X-ray crystal structure and electrochemical properties

The reaction of chlorocarbonylferrocene (2) with bridged calix[4]arene macrocyclic compounds, in which two opposite para-positions are connected by an additional aliphatic chain where n = 5 (1a) or n = 8 (1b) respectively, gave the corresponding new redox-active bis-ferrocene derivatives of bridged calix[4]arenes, 3a and 3b. An X-ray diffraction study of 3a shows that the caliz[4]arene has a cone conformation in which the two ferrocene substituents are located on the phenolic units connected to each other by the aliphatic chain bridge. Cyclic voltammetric and coulometric studies in dichloromethane reveal that 3a and 3b undergo reversible two electron oxidations at + 0.90 V (versus SCE), suggesting that the two respective ferrocene moieties are oxidised in one step. Proton NMR complexation studies (CD3CN) showed neither 3a or 3b form solution host-guest complexes with t-butylamine and benzylamine.

Study of calixarenes-dyes. Structure of p-tetrakis(phenylazo)calix[4]arene

Abstract The first crystal structure of a calixarene-dye, that of p-tetrakis-(phenylazo)calix[4]arene, is presented in this work. Recrystallization of this purified substance in N,N-dimethylformamide afforded crystals suitable for X-ray diffraction. The compound crystallizes in the triclinic space groupe P1 with a = 14.477(3), b = 15.699(3), c = 11.251(5) A, x = 95.29(3), β = 89.94(3), γ = 112.35(2)°, and Dc = 1.290g/cm3 for Z = 2. Refinement based on 6932 observed reflections afforded a final R value of 0.089. These calixarene-N,N-dimethyl-formamide 1:1 crystals have a high density for a compound constituted only of hydrogen, oxygen and nitrogen atoms. This is due to the penetration of a benzylazo group of a calixarene molecule in the cavity of a neighbouring calixarene molecule. A hydrogen bond is established between the oxygen atom of the N,N-dimethylformamide and an oxygen atom of the calixarene; CH3…π interactions also exist between an aromatic nucleus of the phenylazo group and N,N-dimethylformamide...

A New Organic Solid State Reaction: Hydrogenation of Phenols

Abstract During the past fifteen years there has been a number of detailed studies devoted to the chemistry of organic molecular solids and made by a number of groups involving chemists and crystallographers. These workers were interested in the reactions of the organic solids subjected either to a physical agent like light or heat or to a chemical one which can be a solid, a liquid or a gas.1

Crystal structure of the 1 : 4 complex between 18-crown-6 and a polyfunctional guest: 2-hydroxymethyl-4-(1,1,3,3-tetramethylbutyl)phenol

AbstractSingle crystal X-ray analysis of the 1 : 4 complex between 18-crown-6 and 2-hydroxymethyl-4-(1,1,3,3-tetramethylbutyl)phenol is reported. Crystals of the complex are triclinic

Structure of 5,17-dimethyl-11,23-dioctylcalix(4) arene

P\bar 1

The molecular structure of 3(5)-methyl-4,5(3)-trimethylenepyrazole hydrochloride and its13C and15N NMR spectroscopy

witha = 11.929 (2),b = 18.655(2),c = 8.313(1)Å,α = 93.14(1),β = 94.02(1),γ = 100.89(1)o, andDc = 1.111 g cm−3 forZ = 1. TheR index is 0.057 for 5935 reflections measured at 293 K. The complex lies on a center of symmetry, the macroring has the Ci symmetry (g+g+aag−aag−ag−g−aag+aag+a). The CH2-OH group at theortho position to the phenolic OH lies near the benzene ring plane; this conformation differs from the one found for uncomplexed phenol-alcohol molecules. The packing is characterized by layers of hydrogen bonded entities parallel toac; alongb the layers are stabilized by van der Waals interactions.