Trithiooxalat als variabler Brückenligand – Kristall- und Molekülstruktur von μ-Trithiooxalato-bis[bis(triphenylphosphan)kupfer(I)]

Trithiooxalate as Varying Bridging Ligand – Crystal and Molecular Structure of μ-Trithiooxalato-bis[bis(triphenylphosphane)copper(I)] Due to its design, trithiooxalat (trto) as a multidentate, chalcogen-rich ligand allows different coordination possibilities. In contrast to the corresponding dinuclear silver complex [(Ph₃P)₂Ag]₂(trto), which is side-on(S,S′)/end-on(S′,S″) coordinated, the title complex is exclusively side-on (S,S′ and S″,O) coordinated involving the oxygen donor atom. [(Ph₃P)₂Cu]₂(trto) crystallizes in the triclinic space group P1 (No. 2) with a = 10.195(2), b = 13.090(3), c = 13.450(3) Å, α = 116.10(2)º, β = 90.10(2)º, γ = 101.49(2)º, and Z = 1. The bridging ligand with its nonsymmetrical donor atom set is disordered around the centre of symmetry (inversion centre).     

Antimykotisch wirksame Imidazolyl-alkene: Synthese und Röntgenstrukturanalyse von Omoconazol

Antimycotic Imidazolyl-alkenes: Synthesis and X-Ray Crystal Structure of Omoconazol The synthesis of omoconazol 4 from 2′,4′-dichloro-α-(1H-imidazol-1-yl)propiophenon ( 5 ) and 1-bromo-2-(4-chlorophenoxy)ethane ( 6 ) is described. Omoconazol, C₂₀H₁₇Cl₃N₂O₂, crystallises in the monoclinic space group P2₁/n, a = 14.329, b = 8.703, c = 16.791 Å, β = 105.75°. The crystal structure showed that omoconazol has the (Z)-configuration, in accordance with previous NMR results.     

Synthese und Röntgenstruktur von 3-Hydroxy-N-methyl-hasubanan

Synthesis and X-ray data of 3-hydroxy-N-methyl-hasubanan A new simple way to synthesis 3-hydroxy-N-methyl-hasubanan ( 1c ) is described and a single crystal X-ray structure analysis is presented.     

Synthese und Röntgenstrukturanalyse des Additionsproduktes von Schwefeltrioxid an Tetraschwefeltetranitrid (S4N4· SO3)

Synthesis and X-ray Structure Analysis of the Addition Compound of Sulfurtrioxide and Tetrasulfurtetranitride (S₄N₄· SO₃) S₄N₄ · SO₃ was obtained by reaction of S₄N₄ with SO₃ in CH₂Cl₂ and by solvent free reaction of S₄N₄ with Fluorosulfonic acid anhydride. The structure of the adduct could be determined by single crystal X-ray structure analysis. The “cage” of the S₄N₄ is analogous to the structure of S₄N₄ · SbCl₅ reconvoluted into a deformated saddle conformation with nearly C_s-symmetry. The S? N bond lengths in the S₄N₄ ring vary from 1.51 to 1.69 Å. The C_s-symmetry is significantly disturbed by the position of the SO₃ group. In the crystal structure with monoclinic unit cell of space group P2₁/n the molecules are packed into columns, which are arranged pseudohexagonally.     

Synthese und Röntgenstrukturanalyse von Tris(diethyldithiocarbamato) dimethylphenylphosphantechnetium(III), einem Technetium-Komplex mit der Koordinationszahl 7

Preparation and Crystal and Molecular Structure of Tris(diethyldithiocarbamato)dimethylphenylphosphinetechnetium (III) The title compound Tc(S₂CNEt₂)₃(Me₂PhP) I has been prepared by the reaction of TcCl₃(Me₂PhP)₃ with NaS₂CNEt₂. The crystal structure of I has been determined by single-crystal X-ray diffraction methods at room temperature. Crystals are rhombic, space group P2₁2₁2₁, with a = 8.708(1), b = 12.012(1), c = 29.626(3) Å and Z = 4. The compound consists of discrete I molecules. The technetium atom has a seven-coordinated environment which is best described as a distorted pentagonal bipyramid. The Tc—P distance (2.330(3) Å) is remarkably short compared with other technetium complexes with mono-dentate phosphine ligands.     

Synthese und Röntgenstrukturanalyse von Bis(2,2,6,6-tetramethylpiperidin-1-oxidato-O,N)-molybdän(VI)-dioxid

Synthesis and X-Ray Structure Analysis of Bis(2,2,6,6-tetramethylpiperidine-1-oxidato-O,N)molybdenum (VI) Dioxide The title compound ( 1 ) was synthesized by a photoreaction of the 2,2,6,6-tetramethylpiperidin-1-oxyl [TMPO] radical with Mo(CO)₆ and characterized by an X-ray structure analysis as (TMPO)₂MoO₂ complex. In the coordinatively unsaturated 16 electron compound of mm2 symmetry the Mo^VI is coordinated nearly tetrahedrally by the four ligands, the TMPO^? ligands being O,N coordinated. The Mo? O, Mo? N, and Mo?O distances are 1.972(3), 2.198(3), and 1.711(2) Å respectively; the N? O distances are 1.436(4) Å. The stereochemistry of the Mo coordination is the same as in other (R₂NO)₂MoO₂ complexes.     

Synthese,schwingungsspektroskopische Charakterisierung und Einkristallröntgenstrukturanalyse von Tetramethylammoniumcyanat [N(CH3)4]OCN

Synthesis, Vibrational Analysis, and Single Crystal Structure of Tetramethylammoniumcyanate [N(CH₃)₄]OCN By ionic exchange pure tetramethylammoniumcyanate [N(CH₃)₄]OCN was synthesized for the first time. Single crystals were investigated on a 4-circle-diffractometer. Structure solution and refinement was done in Pmn2₁. The structure may be derived from the CsCl-type with linear, non-symmetric cyanate-anions and tetrahedral, slightly distorted tetramethylammonium-cations. Vibrational spectra confirm the distortion of the cation which can be caused by weak O … H(C)-interactions.     

Synthese und Kristallstrukturen der Phosphanimin-Komplexe [Cu(μ-HNPEt3)]4(O3S–CF3)4 und [Pt2Me6(μ-I)2(μ-HNPMe3)]

Synthesis and Crystal Structures of the Phosphaneimine Complexes [Cu(μ-HNPEt₃)]₄(O₃S–CF₃)₄ and [Pt₂Me₆(μ-I)₂(μ-HNPMe₃)] The title compounds have been prepared by the reaction of copper(I)triflate with [NiBr(NPEt₃)]₄ in CH₂Cl₂ suspension in the presence of water, and by the reaction of [PtMe₃I]₄ with Me₃SiNPMe₃ in boiling toluene in the presence of cesium fluoride, respectively. According to the crystal structure determinations the cation of the copper complex forms tetrameric units [Cu(HNPEt₃)]₄⁴⁺ with S₄ symmetry with Cu–N bond lengths of 191.6 and 192.1 pm. In the platinum complex the platinum atoms are linked by two μ-I bridging atoms as well as by the μ-N atom of the HNPMe₃ ligand with Pt–N bond lengths of 228.1 and 229.5 pm.     

Synthese,Struktur und magnetische Eigenschaften von [CrCl(μ-Cl)(TMEDA)]2

Synthesis, Structure, and Magnetic Properties of [CrCl(-μCl)(TMEDA)]₂ The title complex [CrCl(μ-Cl)(TMEDA)]₂ ( 1 ) is obtained in an equimolar reaction of CrCl₂(THF) with TMEDA in high yield. 1 crystallises in the monoclinic space group P2₁/c with a = 843.2(2), b = 1 109.(2), c = 1 147.4(3) pm, β = 102.99(2)° and Z = 2. The molecular structure of 1 contains two, slightly distorted quadratic pyramidal CrL₅-subunits, which are linked via two unsymmetrical Cl-bridges. The μ-Cl-functions take the apical position of one and a basal position of the second CrL₅-unit, wherein the apical Cr–Cl bond (277.6(1) pm) is destinctly longer than the basal Cr–Cl bond (240.6(1) pm). The terminal Cr–Cl bond is still shorter (237.5(1) pm). The Cr…Cr distance is far beyond any bonding interaction. This is confirmed by means of magnetic susceptibility measurements, which show four unpaired electrons per Cr centre; however, a small antiferromagnetic coupling of J/k = ?7.3 K can be calculated. This coupling is suggested to be originated by a 90°-σ-superexchange via the asymmetric μ-Cl functions.