Natrium-tetraethylammonium-tetrasulfid, Na+NEt4+S42−. Synthese und Kristallstruktur / Sodium Tetraethylammonium Tetrasulfide, Na+NEt4+S42−. Synthesis and Crystal Structure

1992 ◽  
Vol 47 (6) ◽  
pp. 819-822 ◽  
Author(s):  
Irina Sens ◽  
Alfred Dirk Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Equimolar Solution

NaNEt4S4 was obtained from an equimolar solution of Na2S4 and NEt4Cl in ethanol. Its crystal structure was determined by X-ray diffraction with 4175 observed unique reflexions, R = 0.044. Crystal data: a = 713.4(4), b = 1744.5(9), c = 1204.0(5) pm, β = 105.8(3)°, space group P21/n, Ζ = 4. In the structure, chains consisting of Na+ and S42− ions run in the a direction, every Na+ being coordinated by four terminal S atoms of S42− ions (two terminal, one chelating). The chains are separated by the NEt4+ ions.

scholarly journals Synthese und Kristallstruktur von [Na(15-Krone-5)]2S6 / Synthesis and Crystal Structure of [Na(15-crown-5)]2S6

1992 ◽  
Vol 47 (8) ◽  
pp. 1063-1066 ◽  
Author(s):  
Alfred-Dirk Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Ether Molecule

[Na(15-crown-5)]2S6 was obtained from Na2S4 und 15-crown-5 in acetonitrile. Its crystal structure was determined by X-ray diffraction with 2968 observed reflexions, R = 0.119. Crystal data: a = 861.4(9), b = 1006(1), c = 2097(1) pm, α = 89.7(1), β = 100.20(8), γ = 114.6(1)°, Ζ = 2, space group Ρ 1̄. The chain-like S62- ion has transoid conformations, each of its terminal atoms is in contact with one Na+ ion which in turn is coordinated with one crown ether molecule.

Synthese und Kristallstruktur von [N(PPh3)2][VCl3(N3S2)]·C7H8 / Synthesis and Crystal Structure of [N(PPh3)2][VCl3(N3S2)]·C7H8

1987 ◽  
Vol 42 (4) ◽  
pp. 410-414 ◽  
Author(s):  
Aida El-Kholi ◽  
Ruth Christophersen ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Subsequent Treatment ◽  
Vanadium Atom ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

Abstract [N(PPh3)2][VCl3(N3S2)]·C7H8 is formed by the reaction of VCl2 (N3S2) with excess PPh3 in CH2C12 and subsequent treatment of the reaction mixture with toluene, as well as by the reaction of VCl2(N3S2) with [N(PPh3)2]Cl in CH2Cl2 in the presence of toluene. The compound forms red crystals, which have been characterized by IR spectroscopy. The crystal structure was determined by X-ray diffraction (1433 observed, independent reflexions, R = 0.070). Crystal data: mono-clinic, space group Cc, Z = 4, a = 994.1, b = 2148.0, c = 2055.2 pm, β = 90.03°. The compound consists of [N(PPh3)2]⊕ cations and [VCl3(N3S2)]⊖ anions, in which the vanadium atom is five-coordinated by threee chlorine atoms and two nitrogen atoms, and is part of a planar VN3S2 ring.

Tetraphenylphosphonium-hexachloroarsenat, PPh4[AsCl6]; Synthese und Kristallstruktur / Tetraphenylphosphonium Hexachloroarsenate, PPh4[AsCl6]; Synthesis and Crystal Structure

1990 ◽  
Vol 45 (7) ◽  
pp. 927-930 ◽  
Author(s):  
Joachim Bebendorf ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Rotation Axes

When ozone is passed through a solution of (PPh4)2[As2Cl8] in dichloromethane at –40 °C, first an instable red compound forms, then intense yellow PPh4[AsCl6] is obtained. The latter can also be obtained by introducing chlorine instead of ozone. The crystal structure of PPh4[AsCl6] was determined by X-ray diffraction (844 observed unique reflexions, R = 5,9%). Crystal data: tetragonal, space group P4/n, a = 1305.6(3), c = 752.2(4) pm, Z = 2. The structure is isotypic with that for other PPh4[MCl6] compounds, the octahedral AsCl6- ions being situated on fourfold rotation axes and showing a well-known positional disorder in that they are somewhat tilted against the symmetry axes due to packing strain.

scholarly journals Dimethylantimonazid: Synthese, Spektren und Kristallstruktur Dimethylbismutazid: Synthese und Kristallstruktur Trimethylbleiazid: Verfeinerung der Kristallstruktur / Dimethyl Antimony Azide: Preparation, Spectra and Crystal Structure Dimethyl Bismut Azide: Synthesis and Crystal Structure Trimethyl Lead Azide: Refinem ent of the Crystal Structure

1985 ◽  
Vol 40 (10) ◽  
pp. 1320-1326 ◽  
Author(s):  
Joachim Müller ◽  
Ulrich Müller ◽  
Almuth Loss ◽  
Jörg Lorberth ◽  
Harald Donath ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Lone Pair ◽  
Lead Azide ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal

Reaction of Me2SbBr or Et2SbBr with AgN3 in ether affords Me2SbN3 and Et:SbN3. respectively. Me2SbN3 can also be obtained from Me2SbNMe2 and HN3 in ether. Me2BiN3 from Me2BiN(SiMe3)3 and HN3 in ether. Me2SbN3 and Et2SbN3 dissolve as monomers in benzene; 1H, 13C, iaN and 15N NMR spectra of the solutions are reported. IR and Raman spectra of solid Me2SbN3 and Et2SbN, as well as the mass spectrum of Me2SbN3 are assigned. The crystal structures of Me2SbN3 and Me2BiN3 were determined by X-ray diffraction data collected at -67 °C (888 and 439 reflexions, R = 0.024 and 0.076. respectively). Both compounds are isotypic, space group Pnma. Z = 4. Crystal data: Me2SbN3, a = 843.6. b = 919.3, c = 744.1 pm: Me2BiN3, a - 870.8. b = 911.3, c = 738.4 pm. In the crystals, the metal atoms are linked via the aN atoms of the azido groups to form endless zig-zag chains. Whereas the Bi -N distances are equal. Sb-N bonds alternate with two different lengths (232 and 243 pm). Including the lone pair of electrons, the metal coordination can be described as distorted trigonal bipyramidal, with nitrogen atoms occupying the apical positions. With new X-ray diffraction data collected at -100 °C, the crystal structure of Me3PbN3 was refined (1692 reflexions, R = 0.036). Crystal data: a = 656.3, c = 1377 pm. space group P3221, Z = 3. It consists of endless metal-nitrogen chains of helical symmetry. the Pb atoms having trigonal bipyramidal coordination.

Synthese und Kristallstruktur von [K(18-Krone-6)]2S6 · 2 CH3CN / Synthesis and Crystal Structure of [K(18-Crown-6)]2S6• 2CH3CN

1992 ◽  
Vol 47 (12) ◽  
pp. 1673-1676 ◽  
Author(s):  
Alfred-Dirk Bacher ◽  
Ulrich Müller ◽  
Karin Ruhlandt-Senge
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Crystalline Compound ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Ether Molecule

[K(18-crown-6)]2S6•2CH3CN was obtained from K2S5 and 18-crown-6 in acetonitrile. The crystalline compound easily loses the incorporated acetonitrile. Its crystal structure was determined by X-ray diffraction with 3095 reflexions, R = 0.058. Crystal data: a = 1621.4(8), b = 812.1(3), c = 3271(2) pm, β = 90.75(4)°, space group C2/c, Ζ = 4. The chain-like S62- ion has transoid conformations. Each of its terminal atoms is coordinated to one K+ ion, which in turn is surrounded by one crown ether molecule.

scholarly journals Zur Darstellung und Kristallstruktur von β-NbO2 / Synthesis and Crystal Structure of β-NbO2

1982 ◽  
Vol 37 (11) ◽  
pp. 1361-1368 ◽  
Author(s):  
H.-J. Schweizer ◽  
Reginald Gruehn
Keyword(s):  
Crystal Structure ◽  
Long Range ◽  
Chemical Transport ◽  
Range Order ◽  
Long Range Order ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

By using chemical transport reactions with various transporting agents (HgCl2, NbCl5, Nb3O7Cl) a slightly substoiehiometric NbO2-phase, β-NbO2, was obtained from samples with O/Nb ∼ 1.5 (source; T > 1373 K) and with deposition temperatures > 1273 K (sink). The rango of composition of β-NbO2 was found to exist from NbO1.990 to NbO1.998.The structure of the tetragonal, column-shaped black crystals was determined by X-ray diffraction. It crystallizes tetragonally in the space group I41 with lattice constants a = 9.693(3) Å, c = 5.985(1) Å and Z = 10 formula units.The crystal structure of β-NbO2 is shown to be a deformed rutile type. As in α-NbO2 the Nb-atoms are grouped in pairs. However, both oxides are different with respect to their long-range order.

Brom- und Chlorthionitrenkomplexe des Rheniums. Die Kristallstruktur von (PPh4)2 [ReBr4(NS)(NSBr)]·CH2Br2 Bromo- and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh4)2[ReBr4(NS)(NSBr)]·CH2Br2

1986 ◽  
Vol 41 (7) ◽  
pp. 825-830 ◽  
Author(s):  
Hans-Günter Hauck ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Ring Cleavage ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Pyridine Complex ◽  
Subsequent Addition

AbstractThe thionitrosyl-halothionitrene com pounds (PPh4)2[ReX4(NS)(NSX)]·2 CH2X2, X = Cl or Br, are obtained by nucleophilic ring cleavage of the Re(N2S2) rings of complexes [ReX4(N2S2)]⊖ with PPh4X in CH2X2. (AsPh4)2[ReCl4(NS)(NSCl)] · CH2Cl2 can also be obtained by the reaction of [ReCl4(NSCl)(POCl3)] with S(NSiMe3)2 and subsequent addition of AsPh4Cl. The pyridine complex [ReBr2(NS)(NSBr)(NC5H5)2] · CH2Br2 forms by bromination of the corresponding chloro compound with Me3SiBr. The IR spectra are reported. The crystal structure of (PPh4)2[ReBr4(NS)(NSBr)] · CH2Br2 was determ ined by X-ray diffraction (4158 independent observed reflexions, R = 0.059). Crystal data: a = 1039.7, b - 1232.5, c - 2158.4 pm, α = 81.59, β = 87.05, γ = 77.06°, Z = 2, space group P1̄. The compound consists of PPh4⊕ ions, CH2Br2 molecules, and anions [ReBr4(NS)(NSBr)]2⊖ in which the rhenium atoms are coordinated by four bromine atoms, one thionitrosyl and one brom othionitrene group. The latter have cis arrangement and ReN bond lengths of 186 pm. W hereas the thionitrosyl group is nearly linear, the R = N = SBr group has an ReNS angle of 165°.

[ η6-C6Me6Fe- η5-C5H5]2Fe2Cl6 · 2 CH2Cl2: Bildung und Kristallstruktur / [η6-C6Me6Fe-η5-C5H5]2Fe2Cl6· 2CH2Cl2: Formation and Crystal Structure

1992 ◽  
Vol 47 (8) ◽  
pp. 1075-1078 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Ir Spectrum ◽  
Title Compound ◽  
The Novel ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

When hexymethylbenzene-cyclopentadienyl-iron reacts with ozone in dichloromethane, the title compound is one of the products. Its crystal structure was determined by X-ray diffraction (R = 0.145 for 1412 unique reflexions). Crystal data: a = 1815.1(8), b = 1314.8(5), c = 1823.0(8) pm, space group Pbca, Z = 8. The sandwich-like [η6-C6Me6Fe-η5-C5H5]+ ions exhibit large thermal motions, and the CH2C12 molecules are disordered in two orientations. The novel [Fe2Cl6]2- ion has the structure of two tetrahedra sharing an edge. Its IR spectrum is reported.

Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur / Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure

1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
The Other ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Lattice Constants ◽  
Bond Lengths

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides

Sign in / Sign up

Export Citation Format

Share Document