The title compound, C 22 H 22 OS [systematic name: 4-(1,3,3-trimethyl-2,3-dihydro-1 H -4-thiaphenanthren-1-yl)phenol], crystallizes unsolvated from nitromethane as colourless prisms (m.p. 425–427 K) in the polar monoclinic space group Ia with Z ′ = 2 (molecules A and B ). Both independent molecules possess a very similar proximal conformation, this referring to the juxtaposition of the 4-hydroxyphenyl substituent with respect to the syn -related methyl group. In the crystal, molecule A is linked to molecule B by an O—H...O hydrogen bond. In turn, molecule B exhibits a weak O—H...π interaction with the phenolic group of molecule A related by a -glide symmetry. Together, these lead to [100] chains.

The title resorcinol forms true clathrates analogous to those formed by Dianin’s compound itself; the ethyl acetate clathrate has space group R3, with a = 27.222(3), c = 10.727(2) å, and Z = 18 (host). One of the diol host’s OH groups participates in a hydrogen-bonded [OH] 6 unit, whilst the other forms an 0H...0 (ether) hydrogen bond to an adjacent hexameric unit stacked (infinitely) along the c axis. In contrast to Dianin’s compound, sublimation in vacuo does not give the stable “empty” cage form, but leads to spontaneous resolution, the unsolvated crystal being orthorhombic, space group P2 1 2 1 2 1 with a = 9.9031(15), b = 10.599(3), c= 13.501(4) Å, and Z = 4. Molecules are now linked head- to- tail by OH...0 (ether) hydrogen bonds to form infinite chains translationally propagated along a. Two such adjacent, parallel chains, related by a 2 1 screw axis along a, form a pair consolidated by intemwlecular hydrogen bonds of OH...O(H) type, involving both hydroxyl groups of the diol.

In its stoichiometric 1:1 clathrate with acetone, studied by X-ray diffraction at 123 K, the title host molecule possesses a unique abbbabbb conformation with six side-chain units anti-parallel to the other two; the guest acetone's conformation exhibits non-crystallographic C-2 symmetry, and the observed lowering in symmetry from C-2v in the vapour is accompanied by a significant opening of the guest's C-C-C angle, in accord with a key theoretical prediction in the literature (J. Chem. Phys., 1993, 98, 2754).

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.

In its molecular crystal the title compound, C74H54S10, has an anti conformation about the central C—C bond. The molecule is centrosymmetric and exhibits regular alternation of the phenylthio side-chain units above and below the mean plane of the 14 C atoms of the diphenylethane skeleton. In contrast, the ethylene link unit has a syn relationship with respect to the phenyl groups of the phenylthio substituents in the ortho positions.

The title compound, C 11 H 16 N 2 O 4 S, shows significant rotation of the NEt 2 and NO 2 groups from the benzene plane, which reduces the steric compression of these ortho substituents. The methyl groups of the NEt 2 substituent adopt a syn arrangement, unlike the anti arrangement in N,N-diethyl-2,4-dinitroaniline

The resolution of electron microscopy may be extended by combining the phase information in microscope images with electron diffraction intensities. A general method for obtaining structural reconstructions at a resolution greater than that of the phase information is demonstrated for crystals of perchlorocoronene. By using entropy maximization methods combined with likelihood ranking, the resolution is extended from 0.32 nm in the microscope images to 0.1 nm in the reconstruction from phase and intensity data.

The title compounds (1 and 3, respectively) were studied by X-ray crystal structure analysis. Both are trigonal space group R3BAR, with lattice parameters a = 27.718(6), c = 8.161(2) angstrom, Z = 3 and a = 31.267(7), c = 6.560(2), Z = 18, respectively. The dodecamethyl compound 1 is isomorphous with its parent hexakis(4-benzylphenoxy)benzene (2), a known host. However, 'collapse' along the c-axial direction has occurred such that the appreciable clathrate cavity of 2 has been replaced by only a very small residual void for 1. Phenol 3 does not pack in discrete [OH]6 hydrogen-bonded hexamers; instead, molecules are assembled in infinite chains, linked by OH ... O hydrogen bonds of length 2.735(3) angstrom, which are propagated along threefold screw axes. A variable-temperature CPMAS NMR study of side-chain aryl group rotation in 1 gives a value DELTAG(not equal) of 14.0 +/- 0.7 kcal mol-1 (at 42-degrees-C) for the (crystallographically unique) para-disubstituted ring, a similar 14 kcal mol-1 free energy barrier being found hindering rotation of this ring, and of the outer phenyl ring of 1, at 9-degrees-C.

The title compound1 crystallizes as colorless polyhedra in the monoclinic polar space groupCc, witha=8.107(2),b=21.577(3),c=9.542(2)Å,β=103.58(2)°, by contrast with its thioether precursor3, crystals of which have the trigonal space groupR¯3. The structure comprises infinite chains of molecules linked head-to-tail by S=O⋯HO hydrogen bonds of length 2.723(2)Å, with H⋯O contact 1.97(4)Å and O-H⋯O 177(3)°; H⋯Ô=S 146(1)°.

AbstractChlorination of coronene (I) gives perchlorocoronene (II) which is substituted with the sodium arenethiolates (III), producing the dodecakis‐(arylthio)coronenes (IV).

C 8 H 10 O 2 S cristallise dans P2 1 /n avec a=11,256, b=5,951 et c=13,099 A, β=114,44 o , Z=4; affinement jusqu'a R=0,063. Confirmation de l'attribution structurale anterieure

ChemInformVolume 19, Issue 28 Isocyclic Compounds ChemInform Abstract: New and Unexpected Reactivity of Saturated Fluorocarbons. D. D. MACNICOL, D. D. MACNICOL Dep. Chem., Univ., Glasgow G12 8QQ, U. K.Search for more papers by this authorC. D. ROBERTSON, C. D. ROBERTSON Dep. Chem., Univ., Glasgow G12 8QQ, U. K.Search for more papers by this author D. D. MACNICOL, D. D. MACNICOL Dep. Chem., Univ., Glasgow G12 8QQ, U. K.Search for more papers by this authorC. D. ROBERTSON, C. D. ROBERTSON Dep. Chem., Univ., Glasgow G12 8QQ, U. K.Search for more papers by this author First published: July 12, 1988 https://doi.org/10.1002/chin.198828120AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat No abstract is available for this article. Volume19, Issue28July 12, 1988 RelatedInformation

In contrast top-hydroxyphenyl-2,2,4-trimethylchroman, Dianin's compound (1), or itsthia analogue2, the title seleno-ether has been found to form two crystallographically distinct types of clathrate. In the first-discovered form, the α-modification of as yet undefined structure, the rhombohedral unit cell (R\(\bar 3\), a = 57.42(1) Å, c = 10.817(1) Å, [from EtOH]) has approximately four times the volume of that found in the clathrates of1 or2 and contains 72 host molecules. Recrystallisation of the selena-host fromn-hexane, however, produces another type of rhombohedral crystal: theβ-modification has space group R\(\bar 3\), witha=28.225(2)Å,c=10.859(1)Å, and 18 host molecules in the unit cell. A detailed X-ray study of this latter inclusion compound (host-guest ratio 6:1) has established its true clathrate nature; the disorderedn-hexane guest, showing electron density consistent with an extended planar zig-zag conformation, is found threading the hour glass-shaped cavity's central constriction.

The title hexaphenol (1), a direct analogue of the β-hydroquinone hexameric unit, has been prepared by six-fold demethylation of hexakis (p-methoxyphenyloxy)benzene (2) with BBr3. Host1 forms a trigonal adduct, space groupR3,a=22.088(3),c=12.232(3) Å, containing 6 molecules of pyridine per host molecule: a detailed X-ray study of this inclusion compound reveals a true clathrate structure, the closed cages of which accommodate a small, non-stoichiometric amount of water.

Consideration of the shape and hydrogen bonding pattern of anentire guest unit, in the known 2:1:2 complex of 2′-hydroxy-2,4,4,7,4′-pentamethylflavan (1) with 1,4-dioxan and water, has indicated a structurally compatible guest,trans-1,4-bis(hydroxymethyl)cyclohexane (3b) which is selectively clathrated from a mixture with itscis isomer (3a). The new complex is triclinic, space group,P\(\bar 1\), witha=8.137(1),b=9.106(1),c=14.552(2) Å, α=93.56(1), β=94.08(1), γ=98.62(1)°, and two host and one guest molecule in the unit cell. A novel hydrogen bonded host-guest arrangement has also been found for host (1), involving ethanol and piperazine [triclinic, space groupP\(\bar 1\), witha=8.438(1),b=10.252(1),c=14.052(1) Å, α=71.28(1), β=89.72(1), γ=83.88(1)δ]; while for the 1:1 ether adduct of (1) the triclinic unit cell, space groupP\(\bar 1\), is approximately doubled in volume [a=8.309(2),b=10.546(3),c=26.664(6) Å, α=102.10(2), β=100.48(2), γ=81.04(2)°], there now being two crystallographically independent host-guest units involving ϕOH·OEt2 hydrogen bonds of length 2.71(1) Å and 2.77(1)Å. In the 2:1 complex of the isomeric host 2′-hydroxy-2,4,4,6,5′-pentamethylfavan (2) withN, N′-dimethylpiperazine (5) [triclinic space groupP\(\bar 1\), witha=7.411(1),b=10.143(3),c=15.109(3)Å, α=98.73(2), β=88.30(1), γ=109.72(2)°] the centrosymmetric chair-shaped guest molecule is clamped by two axially oriented ϕOH...N hydrogen bonds of length 2.759(3)Å.

Bei der Chlorierung von Triphenylen (Ia) erhält man anstelle der Perchlorverbindung (Ib) über diskutierte Zwischenstufen ein Umlagerungsprodukt (II) neben dem Perchlor‐o‐terphenyl (III).