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The crystral structure of CCl2= NH–CCl3+SbCl6-is reported. The compound crystallizes in the monoclinic space group P21/n with a = 11.086(11), b = 9.973(12), c = 14.478(17)Å, β = 106.69(9)°, Ζ = 4. The framework of the cation is planar, with C–N bond lengths of 1.488(7) and 1.280(5)Å. The cation and the anion have one short H ••• Cl contact of 2.313(2)Å.

H2N3+SbCl6-reacts in SO2as a solvent with SCl2to give N(SCl)2+SbCl6-. The yellow salt crys­tallizes in the monoclinic space group P21/c with a = 729.7(7), b = 1122.1(8), c = 1575.6(11) pm, and β = 99.43(6)° at 169 K with 4 formula units per unit cell. The vibrational spectra are reported.

The crystal structure of (C6H5)3CSI is reported. It is the first structure determination of an iodine sulfane. (C6H5)3CSI crystallizes in the monoclinic space group P21/c with a - 1226.4(7) pm, b = 1398.8(18) pm, c = 941.6(8) pm, β = 96.38(8)° and Z = 4. The sulfur-iodine bond length is 240.6(4) pm corresponding to the sum of the covalent radii with 237 pm. The molecules are linked via short I···S contacts of 321.0(4) pm such that a zig-zag chain is formed.

The synthesis of CF3SCl2+AsF6-is reported. The sulfonium salt is characterised by IR, Raman, 19F and 13C NMR spectroscopy. The vibrational assignment is based on a Csmodel for the cation and assisted by a normal coordinate analysis. The crystal structure has been determined from three-dimensional diffractometer data at -133 K. The structural data for the cation are: C-F = 128.8(5) pm, C-S = 197,8(3) pm, S-Cl = 195,9(1) pm and F-C-F = 111,8(3)°, Cl-S-Cl = 104,22(5)°, C-S-Cl = 99,8(1)°.

The preparation of CF3N(O)H+MF6- and CF3NH2OH+MF6- (M = As, Sb) and the crystal structure of CF3NH2OH+AsF6-are reported. CF3N(O)H+MF6-is prepared by protonation of CF3NO in the superacid system HF/MF5(M = As, Sb). With an excess of CF3NO the cation CF3NH2OH+MF6- is formed. CF3NH2OH+AsF6-crystallizes in the triclinic space group P T with a = 5.071(2), b = 8.297(3), c = 8.882(4) Å, α = 90.93(4)°, β = 95.49(4)°, γ = 102.96(4)° and Z = 2. It is formed by a redox reaction between CF3N(O)H+ and excess CF3NO.

The preparation of the stable compounds [(CH3)2SSCl]+SbF6-and [(CH3)2,SSSCl]+SbF6-from [(CH3)2SH]+SbF6- and SCl2and S2Cl2, resp., is reported.

The preparation and spectroscopic characterization of the sulfonium salts (CH3)2SSCN+AsF6-, (CH3)2SSeCN+AsF6- and (CH3)2SNCO+AsF6-is reported. The compounds are obtained via halide-pseudohalide exchange reactions with (CH3)2SBr+AsF6-and the corresponding silver pseudohalide. In addition the crystal structure of (CH3)2SSCN+AsF6-was determined. The salt crystallizes in the orthorhombic space group Pbca with a = 1048.4(9) pm, b = 1290.2(6) pm, c = 1405.1(12) pm and Z = 8.

The crystal structure of CH3C6H4S(O)2NCl2is reported. Crystals are monoclinic, space group P21/c, with a = 710.0(7), b = 1615.3(13), c = 867.2(7) pm, V = 988(2) pm3and Z = 4. The reaction with HF/SbF5yields CH3C6H4S(O)2NCl2H+SbF-6the first protonated dichloroamine salt, its vibrational -and NMR spectra are discussed

The crystal structure of SbCl4F is reported. SbCl4F crystallizes in the tetragonal space group I 4̄

The synthesis of salts of the type RnSH3-n+MF6-(R = C2H5, i-C3H7; n = 1, 2; M = As, Sb) by protonation of the corresponding thiols and sulfides in the superacid systems HF/MF5is reported. The salts have been characterized by vibrational and NMR spectroscopic methods. Isopropylsulfonium hexafluoroantimonate is the first known example of a sulfonium salt, for which a SH bond distance has been determined by a crystal structure analysis, i-C3H7SH2+SbF6-crystallizes in the monoclinic space group P21/m with a = 568.0(4), b = 801.1(6), c = 1019.7(8) pm, β = 82.63(6) °, with two formula units per unit cell.

CH3S(0)C1 reacts in HF as solvent with MF5(M = As, Sb) to give products CH3S(Cl)OMF5(M = As, Sb). The new compounds are stable below 253 K and were charac­ terized by Raman and NMR spectroscopy.

The single‐crystal X‐ray structure determinations of the title complexes, cis‐di­chloro‐trans‐di­methyl‐cis‐bis(N‐methyl­pyr­rolidin‐2‐one‐O)­tin(IV), [Sn(CH3)2Cl2(C5H9NO)2], cis‐di­bromo‐trans‐di­methyl‐cis‐bis(N‐methyl­pyrrolidin‐2‐one‐O)tin­(IV), [SnBr2(CH3)2(C5H9NO)2], and cis‐di­iodo‐trans‐di­methyl‐cis‐bis(N‐methyl­pyrrolidin‐2‐one‐O)­tin(IV), [Sn(CH3)2I2(C5H9NO)2], show that those tin complexes in which coordination of the lactam ligand to SnIVis realized viaoxygen exhibit a distorted octahedral geometry.

The crystal structure of SbF5· SO2is reported. SbF5· SO2crystallizes in the monoclinic space group P21/n with a = 580.4(4) pm, b = 1047.7(5) pm, c = 1013.3(6) pm, β = 102.92(5)°, V = 600.57 · 106(6) pm3, and Z = 4. It shows five intermolecular S ··· F contacts.

An oxonium ion with hydroxymethyl and methylidene substituents is found in the salts 1-MF6 (M=As, Sb), which can be isolated from solutions of formaldehyde in superacids HF/MF5. Their formation was at first surprising, since NMR spectroscopy indicates that protonated monofluoromethanol is present in solution.

Chlorosulfonium hexachloroantimonate crystallizes in the monoclinic space group C 2/m with a = 1405.5(3) pm, b = 1055.1(2) pm , c = 882.2(2) pm, β = 110.05(3)° at 169 K with 4 formula units per unit cell. A distorted octahedral coordination around sulphur is formed by three S - C l bonds and three interionic sulphur chlorine contacts. The interionic interactions in SCl3+salts of known crystal structures are discussed.

Ein Oxonium-Ion mit einem Hydroxymethyl- und einem Methylidensubstituenten liegt in den Salzen 1-MF6 vor, die aus Lösungen von Formaldehyd in den Supersäuren HF/MF5 (M=As,Sb) isoliert werden konnten. Ihre Bildung war unerwartet, da laut NMR-Spektren in Lösung protoniertes Monofluormethanol vorliegt.

The preparation and X‐ray analysis of the title compound, [Sn2Br4(CH3)4(C5H9NO)], are described. The compound contains two Sn atoms in the asymmetric unit, that complexed by N‐methyl­pyrrolidin‐2‐one being hexacoordinated (a), the other exhibiting pentacoordination (b). The most important features are three different Sn—Br bond lengths at both Sn atoms with the following values: (a) 2.5060 (9), 2.7152 (10) and 3.7118 (10) Å; (b) 2.5084 (10), 2.5279 (9) and 3.5841 (10) Å.

The synthesis and X‐ray structure analysis of the title compound, [SnBr2(CH3)2(C4H9NO)2], are described. The crystal contains mol­ecules which are separated by normal van der Waals distances. Organotin(IV) compounds are found in a variety of structural types, in which the Sn atom can, for example, be hexacoordinated. In this case, the preferred solid‐state molecular structure of the central atom is octahedral. The degree of distortion and the configuration depend on the ligands.

The synthesis and the X‐ray structural analysis of the title compound, μ‐chloro‐1:2κ2Cl‐tri­chloro‐1κCl,2κ2Cl‐tetra­methyl‐1κ2C,2κ2C‐(N‐methyl­pyrrolidin‐2‐one)‐1κO‐ditin(IV), [Sn2Cl4(CH3)4(C5H9NO)], are described. The title compound is found to exhibit a distorted trigonal–bipyramidal geometry at both SnIVatoms. The Sn—Cl—Sn angle involving the bridging chlorine ligand is 135.56 (5)°, with the Sn—Cl bond lengths being 2.5704 (13) and 3.1159 (13) Å.

The title compound, di‐μ‐chloro‐bis{[(2,3,4‐η)‐ethyl 6,6‐di­methyl‐5‐oxohept‐2‐enoato]­palladium(II)}, [Pd2Cl2(C11­H17­O3)2], is a binuclear chloro‐bridged palladium allyl complex that was obtained serendipitously From the reaction of 6,6‐di­methyl‐2‐hepten‐4‐ynoate with Na2PdCl4in water‐containing alcohol. The allyl group is substituted with an ester and a tert‐butyl­carboxy group. The dimeric mol­ecules link viaC—H⃛O contacts into a two‐dimensional network parallel to the bcplane.

The title compound, di­bromo­di­methyl(N‐methyl­pyrrolidin‐2‐one‐O)­tin(IV), [SnBr2(CH3)2(C5H9NO)], exhibits pentacoordination of the Sn atom, with long and short Sn—Br bonds [2.6737 (4) and 2.5256 (4) Å, respectively]. The distorted trigonal–bipyramidal coordination polyhedron has two methyl groups and one Br atom in the equatorial plane, the second Br atom and the N‐methyl­pyrrolidinone (NMP) ligand occupying the apical positions.

Esterification of a single diastereomer of 2‐(4‐methylene­cyclohex‐2‐enyl)propanol, (II), with (1R,4S)‐(+)‐camphanic acid [(1R,4S)‐4,7,7‐trimethyl‐3‐oxo‐2‐oxabicyclo[2.2.1]heptane‐1‐carboxylic acid] leads to the crystalline title compound, C20H28O4. The relative configuration of the camphanate was determined by X‐ray diffraction analysis. The outcome clarifies the relative and absolute stereochemistry of the naturally occurring bisabolane sesquiterpenes β‐turmerone and β‐sesquiphellandrene, since we have converted (II) into both natural products viaa stereospecific route.

Stereoselective hydroboration of (−)‐isopulegol and subsequent fractional crystallization furnishes the title compound, C10H20O2. The relative configuration of the stereogenic centres has been assigned by means of X‐ray diffraction analysis since the monoterpenediol is employed as a versatile chiral building block in stereospecific natural product synthesis.

Catalytic enantioselective cycloaddition of azomethine ylides (II) to methylene oxindoles (I) gives pyrrolidinyl‐spirooxindoles after acylation with high diastereoselectivity in most cases with exception of ortho‐substituted azomethine ylides.

ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 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.

The synthesis and crystal structure analysis viaX‐ray diffraction of the title compound, C20H24O4, (I), are described. The title compound is an androstadione bearing a diene in the Aand Brings [Krause & Thorand (1999). Inorg. Chim. Acta, 296, 1–11]. The diene conjugates with the carbonyl group. Intermolecular H⃛O contacts (2.53 and 2.64 Å; C—H⃛O angles 161 and 158°) indicate hydrogen bonds.

The title compound, C12H16O4, (I), was prepared by oxidation of (5S*,6R*)‐1,7‐di­oxa­di­spiro­[4.0.4.4]­tetra­decane‐2,8‐diol us­ing silver(I) carbonate and posesses a cisconfiguration of the two five‐membered‐ring lactones fused spiro to the six‐membered carbocycle, which has a chair conformation. It represents an exceptional structure for bis‐tetra­hydro­furan units, which are interesting building blocks in natural products. The synthesis, spectroscopic data and X‐ray structural analysis are described. The crystal contains discrete mol­ecules separated by normal van der Waals distances.

The synthesis, spectroscopic data and X‐ray structural analysis of the title compound, C26H35NO2S, (I), are described. The crystal contains discrete mol­ecules separated by normal van der Waals distances. The benzene­sulfon­amide derivative of the corresponding amine allows the assigment of its relative configuration. The secondary amine has been synthesized viaa sequential multi‐step hydro­formyl­ation procedure according to Eilbracht et al.[Chem. Rev.(1999), 99, 3329–3365].).

The crystal structure of the title compound, C10H20O2, was published [Körner et al.(2000). Acta Cryst. C56, 74–75] with an erroneous position for an hydroxy H atom. This has now been corrected and leads to a more sensible hydrogen‐bonding scheme.

ChemInform 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.

ChemInform 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.

The title compound, C16H26O2, (I), prepared by oxidation of (1R*,11R*)‐12‐hydroxy­bi­cyclo­[9.4.1]­hexa­decan‐16‐one using pyridinium dichromate, has a transconfiguration of the two fused rings and represents an interesting precursor for the synthesis of macrocyclic structures.

The title compound, C23H19N2O3P, was prepared by the reaction of ethynyldi­phenyl­phosphine oxide with phenyl isocyanate, triethyl­amine and nitoethane in benzene. The molecular structure is stabilized by an intramolecular N—H⋯O hydrogen bond.