Röntgenographische Kristallstrukturbestimmung des Additionsproduktes von Fluorsulfonylisocyanat an Tetraschwefeltetranitrid (S4N4 · FSO2NCO)

X-Ray Structure Analysis of the Addition Product of Fluorosulfonylisocyanate and Tetrasulfurtetranitride (S₄N₄ · FSO₂NCO) In order to determine the structure of the addition product of tetrasulfurtetranitride with fluorosulfonylisocyanate an X-ray structure analysis was performed. The structure analysis shows a nucleophilic attack of a nitrogen atom of the S₄N₄ ring at the carbonyl carbon atom of the isocyanate forming an N? C single bond. The dipolar compound is very similar to the structures of S₄N₄ · SO₃, S₄N₄ · BF₃ and S₄N₄ · SbCl₅. The conformation of the S₄N₄ ring deviates significantly from a planar environment. The packing of the molecules int the crystal structure of the triclinic space group P1 is comparable with the arrangement of molecules in the crystal structure of S₄N₄ · SO₃.     

S4N4 und seine Derivate: Darstellung und Röntgenstrukturanalyse von CuCl2 · S4N4

Phase equilibrium in the TeO₂? Cu₂O system was determined in air at atmospheric pressure. Differential thermal analysis (DTA), X-ray powder diffraction and optical microscopy were used to identify the phase transitions. Two congruently melting compounds Te₃Cu₂O₇ and TeCu₂O₃ were obtained. They possess monoclinic and hexagonal symmetry respectively. The morphology, optical properties and indexed powder pattern up to 1.3 Å are submitted for these compounds. Experiments realized by the DTA indicated the existence of an oxidation process with beginning and rate dependent on the composition. The glass formation limits determined for 2 g and 10 g tellurite glass melts correlate with the invariant points in the system.     

Synthese und Röntgenstrukturanalyse von S4N4-Derivaten mit drei- und vierfach koordinierten Schwefelatomen

CF₃SO₂N?SCl₂ reagiert mit (CH₃)₂S[NSi(CH₃)₃]₂, (C₄H₈)S[NSi(CH₃)₃]₂ oder (C₅H₁₀)S[NSi(CH₃)₃]₂ unter Trimethylchlorsilanabspaltung zu den achtgliedrigen S₄N₄-Derivaten S₄N₄(NSO₂CF₃)₂(CH₃)₄ 3 , S₄N₄(NSO₂CF₃)₂(C₄H₈)₂ 4a und S₄N₄(NSO₂CF₃)₂(C₅H_{1 0})₂ 4b . In den achtgliedrigen SN-Ringen haben die Schwefelatome die Koordinationszahl 3 und 4. Die Röntgenstrukturanalyse von 4a ergab eine Sessel-Konformation. 4a kristallisiert orthorhombisch in der Raumgruppe Pna2₁ mit a = 17,641(4), b = 6,406(2), c = 19,130(4) Å, d_x = 1,815 g cm^?3 und Z = 4. Die mittleren S? N-Abstände betragen an den vierfach koordinierten Schwefelatomen 1,597 Å und an den Schwefelatomen mit der Koordinationszahl 3 1,650 Å. CF₃SO₂N? SCl₂ reagiert mit trimethylzinnhaltigen S? N-Verbindungen zum bekannten CF₃SO₂N[Sn(CH₃)₃]S(CH₃)NSO₂CF₃ und Dimethylzinndichlorid. Synthesis and X-Ray Structure Analysis of S₄N₄-Derivatives with Threefold and Fourfold Coordinated Sulfur Atoms CF₃SO₂N?SCl₂ reacts with (CH₃)₂S[NSi(CH₃)₃]₂, (C₄H₈)S[NSi(CH₃)₃]₂ or (C₅H₁₀S[NSi(CH₃)₂]₂ under elimination of (CH₃)₃SiCl to yield the eight-membered S₄N₄ derivatives S₄N₄?NSO₂CF₃)₂(CH₃)₄, 3 , S₄N₄(NSO₂CF₃)₂(C₄H₈)₂ 4a und S₄N₄(NSO₂CF₃)₂(C₅H_{1 0})₂ 4b . In the eight-membered SN-rings the sulfur atoms have the coordination number 3 and 4. The X-ray structure analysis of 4a revealed a chair conformation. 4a crystallizes in the orthorhombic space group Pna2₁ with a = 17.641(4), b = 6.406(2), c = 19.130(4) Å, d_x = 1.815 g cm^?3, and Z = 4. The average S? N distance was found to be 1.597 Å at fourfold coordinated sulfur atoms and 1.650 Å at sulfur with coordination number 3. CF₃SO₂N=SCl₂ reacts with trimethyl tin-containing S? N compounds to the known CF₃SO₂N[Sn(CH₃)₃]S(CH₃)NSO₂CF₃ and dimethyl tin dichloride.     

Synthese und Röntgenstrukturanalyse des 8π-Elektronenringsystems S4N4O2Sn2(CH3)6 und des magnetische Verhalten von S4N4O2 und S8N8O4

Synthesis and X-Ray Structure Analysis of the 8π-Electron-Ring-System S₄N₄O₂Sn₂(CH₃)₆ and the Magnetic Properties of S₄N₄O₂ and S₈N₈O₄ S₄N₄O₂ reacts with N[Sn(CH₃)₃]₃ in a molar ratio of 1:1 to an eight-membered trimethyltin-substituted 8π-electron skeleton, S₄N₄O₂Sn₂(CH₃)₆. In contrast to known 6π-electronsystems this compound has tin atoms which are tetracoordinated. This was demonstrated on the basis of an x-ray analysis. S₄N₄O₂Sn₂(CH₃)₆ · 1/2 C₆H₆ crystallizes in the space group P2₁/c with a = 1396.0(4), b = 1190.3(4), c = 1256.7(3) pm, and β = 103.46(2)°. It was shown that the ability of coordination at the tin atom depends on the electron density. The magnetic properties of S₄N₄O₂ and S₈N₈O₄ were investigated by the Faraday method. The high diamagnetism in these ring compounds is caused by the π-electrons.     

Einkristallzüchtung und Röntgenstrukturanalyse von CoSO4 · Pyrazin · 6 H2O (I) und (CoSO4)2 · Pyrazin · 12 H2O (II)

Crystal Growth and Structure of CoSO₄ · Pyrazine · 6 H₂O (I) and (CoSO₄)₂ · Pyrazine · 12 H₂O (II) Single crystals of μ-pyrazino-bis[pentaquacobalt(II)]-sulfate-dihydrate CoSO₄(pz) · 6 H₂O and Tetraqua-μ-pyrazino-cobalt(II)sulfate-dihydrate (CoSO₄)₂(pz) · 12 H₂O were grown by using gel methods and investigated by X-ray analysis. CoSO₄(pz) · 6 H₂O (I) shows monoclinic symmetry, space group C2/c; a = 1006.4(4) pm, b = 1026.9(4) pm, c = 1261.5(2) pm; β = 104.01(4)°; Z = 4. (CoSO₄)₂(pz) · 12 H₂O (II) shows orthorhombic symmetry, space group Pbam; a = 1262.3(4) pm, b = 1231.3(4) pm, c = 684.1(2) pm; Z = 2. CoSO₄ and Pyrazine crystallize in a polymeric (I) as well as in a dimeric (II) compound. In the polymeric compound the molecules are bonded by pyrazine to form alternating linear chains. The dimer is a dinuclear complex with a bridging pyrazine molecule.     

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 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 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.     

Die Röntgenstrukturanalyse des Triformamids und des Tris(dichlormethyl)amins

X-Ray Structure Determinations of Triformamide and Tris(dichlormethyl)amine Triformamide, N(CHO)₃ ( I ) and Tris(dichlormethyl)amine, N(CHCl₂)₃ ( II ), both crystallize in the hexagonale space group P6₃/m with 2 formula units per cell. The molecular symmetry is C_3h in both cases, that means I is totally planar, II consists of a planar NC₃H₃ skeleton. The structure was refined to an R-value of 0,031 ( I ) and 0,028 ( II ), respectively.     

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 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.     

Röntgenographische und spektroskopische Untersuchungen an Ba2Ni(N3)6· 3H2O

Preparation and X-Ray Examination of Ba₂Ni(N₃)₆ · 3 H₂O Ba₂Ni(N₃)₆ · 3 H₂O has been prepared by the reaction of an aqueous solution of Ba(N₃)₂ with basic nickel azide. The crystals are green, the lattice constants are: a = 7.09 Å, b = 7.09 Å, c = 16.30 Å, α = 74.58°, β = 105.42°, γ = 97.10°, N = 2. Optical spectra point to an octahedral microsymmetry of the azide ions around nickel.     

Synthese und Einkristallröntgenstrukturanalyse von Bromdi(isopropenyl)bismutan

Synthesis and Single Crystal X‐Ray Structure Analysis of Bromodi(isopropenyl)bismuthane Tri(isopropenyl)bismuthane ( 1 ) reacts with bromine to form bromodi(isopropenyl)bismuthane ( 2 ) and dibromo(isopropenyl)bismuthane ( 3 ). The single crystal X‐ray structure determination of 2 (monoclinic, P 2₁/c; a = 1058.6(3), b = 1127.0(3), c = 1561.3(4) pm, and β = 109.26(2)°; Z = 8 molecules; d_c = 2.803 g/cm³; R = 0.059) shows two crystallographically independent molecules which are connected by Bi–Br…Bi bridges (Bi–Br 282.3(2) and 284.7(2); Br…Bi 302.9(2) and 303.6(2) pm) forming helical chains directed along the b‐axis of the unit cell. Every turn of the helix (360°) consists of four molecules and corresponds to the length of the b‐axis (1127.0(3) pm).     

Synthese,Struktur und Phasenumwandlung von Te4[AsF6]2·SO2

Synthesis, Crystal Structure, and Solid State Phase Transition of Te₄[AsF₆]₂·SO₂ The oxidation of tellurium with AsF₅ in liquid SO₂ yields Te₄²⁺[AsF₆^—]₂ which can be crystallized from the solution in form of dark red crystals as the SO₂ solvate. The crystals are very sensitive against air and easily lose SO₂, so handling under SO₂ atmosphere or cooling is required. The crystal structure was determined at ambient temperature, at 153 K, and at 98 K. Above 127 K Te₄[AsF₆]₂·SO₂ crystallizes orthorhombic (Pnma, a = 899.2(1), b = 978.79(6), c = 1871.61(1) pm, V = 1647.13(2)·10⁶pm³ at 297 K, Z = 4). The structure consists of square‐planar Te₄²⁺ ions (Te‐Te 266 pm), octahedral [AsF₆]^— ions and of SO₂ molecules which coordinate the Te₄ rings with their O atoms in bridging positions over the edges of the square. At room temperature one of the two crystallographically independent [AsF₆]^— ions shows rotational disorder which on cooling to 153 K is not completely resolved. At 127 K Te₄[AsF₆]₂·SO₂ undergoes a solid state phase transition into a monoclinic structure (P112₁/a, a = 866.17(8), b = 983.93(5), c = 1869.10(6) pm, γ = 96.36(2)°, V = 1554, 2(2)·10⁶ pm³ at 98 K, Z = 4). All [AsF₆]^— ions are ordered in the low temperature form. Despite a direct supergroup‐subgroup relationship exists between the space groups, the phase transition is of first order with discontinuous changes in the lattice parameters. The phase transition is accompanied by crystal twinning. The main difference between the two structures lies in the different coordination of the Te₄²⁺ ion by O and F atoms of neighbored SO₂ and [AsF₆]^— molecules.     

AsPh4[W2Cl4(N3S2)3] · CCl4; Synthese und Kristallstruktur

AsPh₄[W₂Cl₄(N₃S₂)₃] · CCl₄; Synthesis and Crystal Structure The title compound was obtained in form of black crystals along with other products by the reaction of H₂S and AsPh₄[WCl₄(N₃S₂)] in dichloromethane and subsequent addition of CCl₄. Its crystal structure was determined by X-ray diffraction (3036 observed reflexions, R = 0.051). Crystal data: triclinic, space group P¯1, Z = 2, a = 1369, b = 1398, c = 1441 pm, α = 64.8, β = 68.02 and γ = 58.1°. The compound consists of AsPh₄^⊕ ions, CCl₄ molecules and [W₂Cl₄(N₃S₂)₃]^? ions. In the latter, one tungsten atom is member of one planar WN₃S₂ ring while the second tungsten atom belongs to two such rings forming a nearly planar S₂N₃WN₃S₂ unit. Two nitrogen atoms of this unit are linked to the other tungsten atom forming a WN₂W ring. Two chloro ligands at each tungsten atom complete the coordination sphere to coordination numbers of six.