Crystallization and Structure of {(H52C44O4-3)[Li+6(NH3)2](3-O4C44H52)}, an Edge-Shared Li+6 Double Tetrahedron between Calix[4]arenetrianion Half-Shells: Another Self-Organized and Lipophilically-Wrapped Polyion Aggregate

Abstract

The first two examples!a of novel lipophilically-wrapped polyion aggregates,2 in which a cluster of cations and anions provides thermodynamical stability and a kinetically persistent impenetrable hydrocarbon skin, have both been discovered serendipitously: the (octahedron + prismane) polyhedron (1) crystallized after addition of ra-butyllithium to the solution obtained from dissolving barium metal in ferf-butyl alcohol (1), and the hexameric sodium imido diphosphonate was prepared by reacting the tetraphenoxydiphosphonate inline with NaH in benzene (2): {[Ba2%Li+3O£-2]11+(-OC(CH3)3)"(0C4Ha)3}(2) {(H5C60)24(0PNP0Na+S6}

Polymetallated 4‐tert‐Butylcalix[4]arene Complexes of Sodium and Potassium Stabilized by Crown Ethers: Syntheses, Structures and Activation of Carbon Dioxide

“…A number of other alkali metal complexes with monoanionic and dianionic calixarenes are also known 11−13. Recently, Harrowfield described partially deprotonated thiacalixarene complexes of the Li−Cs series,14 and in 1995 Bock et al published the molecular structure of [Li 3 (calix[4]arene‐3H)(NH 3 )] 2 the first alkali metal complex of a multiply deprotonated calix[4]arene 15…”

cis-Aconitic Acid at 150K

“…The crystal structure of dipotassium cis-aconitate (Glusker, Orehowsky, Casciato & Carrell, 1972) has been determined in order to obtain information about a possible mechanism for this conversion. Our report, which is part of a project on the study of the formation of lipophilically wrapped polyion aggregates (Bock, John, N~ither & Havlas, 1995;Bock, Dienelt, Schrdel & Havlas, 1995), shows that the conformation of the dianion in the dipotassium salt and that in the crystal structure of the acid, (I), are similar.…”

Lithium calix[4]arenes: structural studies and use in the ring opening polymerization of cyclic esters

“…Of the number of synthetic routes to lithiated calixarenes outlined above, 9–14 we chose as our entry point the use of LiO t Bu. Reaction of LiO t Bu (5 equiv.)…”

“… 7 Over the last decade or so, a number of routes to lithiated calix[4]arenes and their thia-bridged analogues have been developed. The early work on calix[ n ]arenes involved the use of 7 Li NMR spectroscopy, 8 whilst for p-tert -butylcalix[4]arene (L 4 H 4 ), early structural work involved the use of lithium amide, 9 whilst Davidson et al employed n BuLi in the presence of either wet or dried hexamethylphosphoramide (hmpa) and isolated Li 4 L 4 ·LiOH·4hmpa or [Li 4 L 4 ·2hmpa] 2 , respectively. 10 Floriani et al also employed n BuLi in the presence of naphthalene to prepare lithiated calix[4]arenes.…”