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.

Anionische Komplexe [Mo2(O2CPh)4X2]2⊖ mit X = N3, Cl, Br. Die Kristallstruktur von (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 / Anionic Complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, Cl, Br. The Crystal Structure of (PPh4)2[Mo2(O2C-Ph)4Cl2] · 2CH2Cl2

1985 ◽  
Vol 40 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Kay Jansen ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Diffraction Data ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Anionic Complexes

The syntheses and IR spectra of the complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, CI, Br and the counter ion PPh4⊕ are reported. The azido and the bromo complexes are obtained from a solution of [Mo2(O2CPh)4] with PPh4N3 in pyridine or by reaction with PPh4Br in CH2Br2, respectively. When (PPh4)2[Mo2(O2CPh)4(N3)2] is dissolved in CH2Cl2, nitrogen is evolved and the complex with X = CI is obtained. The crystal structure of (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 was determined from X-ray diffraction data (5676 observed independent reflexions, R = 0.042). It crystallizes in the monoclinic space group P21/n with four formula units per unit cell; the lattice constants are a = 1549, b = 1400, c = 1648 pm, β = 94.6°. The centrosymmetric [Mo2(O2CPh)4Cl2]2⊖ ion has a rather short Mo-Mo bond of 213 pm, whereas the MoCl bonds are very long (288 pm)

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.

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

Synthesis and Crystal Structure of K6Mo10O33

2007 ◽  
Vol 62 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Nachiappan Arumugam ◽  
Eva-Maria Peters ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
Molybdenum Oxide ◽  
Solid State Reaction ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

A new potassium molybdenum oxide, K6Mo10O33, was synthesized by solid state reaction from the appropriate quantities of pre-dried MoO3 and K2MoO4, fired at around 650 °C for 2 d. The structure has been solved by using single crystal X-ray diffraction. The compound adopts the space group P1, with the lattice constants a = 7.7100(5), b = 11.9659(8), c = 17.1321(12) A° , α = 86.42 (10), β = 77.18(10), γ = 74.14(10)°. The structure is built up of infinite chains of edge-sharing MoO6 octahedra and groups of four MoO6 octahedra forming Mo4O17 units. These sub-units are connected together by common vertices.

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.

Cyclo-thiazenokomplexe von Molybdän und Wolfram. Die Kristallstruktur von AsPh4[WCl4(N3S2)] / Cyclo-thiazeno Complexes of Molybdenum and Tungsten. The Crystal Structure of AsPh4[WCl4(N3S2)]

1984 ◽  
Vol 39 (12) ◽  
pp. 1680-1685 ◽  
Author(s):  
Ulrich Kynast ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Moist Air ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lattice Constants ◽  
Bond Lengths ◽  
Distorted Octahedral

The dark brown cyclo-thiazeno com plexes [MoCl3(N3S2)]2 and [WCl3(N3S2)]2 are obtained by quantitative reactions of MoNCl3 with (NSCl)3 and of WOCl4 or WSCl4 with excess (NSCl)3, respectively. They are diamagnetic, thermally stable up to 200 °C, and only slightly sensitive towards moist air, but react explosively with aqueous bases. According to the IR spectra [MoCl3(N3S2)]2 is dimerized via chloro bridges whereas the tungsten com pound is associated via the γ-nitrogen atoms of the cyclo-thiazeno ligand. By reaction with [AsPh4]Cl or [PPh4]Cl in CH2Cl2, the compounds EPh4[MCl4(N3S2)] are obtained (E = P, As; M = Mo, W). The crystal structure of AsPh4[WCl4(N3S2)] was determined from X-ray diffraction data (1845 observed reflexions, R = 0.045). It crystallizes in the monoclinic space group P21/c with four formula units per unit cell. The lattice constants are a = 1352.4, b = 968.4, c = 2393.8 pm and β = 115.1°. The com pound is built up from AsPh4⊕ cations and [WCl4(N3S2)]⊖ anions in which the W atoms are coordinated in a distorted octahedral fashion by four Cl and two N atoms of the N3S2 ligand. The WN bond lengths (182 and 188 pm) correspond to douple bonds. The WN3S2 ring is planar and has SN bond lengths between 154 and 161 pm.

scholarly journals High-pressure synthesis and crystal structure of the mixed-cation borate Ga4In4B15O33(OH)3

2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
High Temperature ◽  
Diffraction Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Mixed Cation ◽  
High Pressure High Temperature ◽  
Pressure Synthesis

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.

Single-crystal investigation of Ce5AgxGe4−x (x = 0.1−1.08) with Sm5Ge4 type

2020 ◽  
Vol 75 (8) ◽  
pp. 765-768
Author(s):  
Bohdana Belan ◽  
Dorota Kowalska ◽  
Mariya Dzevenko ◽  
Mykola Manyako ◽  
Roman Gladyshevskii
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Binary Compound ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

AbstractThe crystal structure of the phase Ce5AgxGe4−x (x = 0.1−1.08) has been determined using single-crystal X-ray diffraction data for Ce5Ag0.1Ge3.9. This phase is isotypic with Sm5Ge4: space group Pnma (No. 62), Pearson code oP36, Z = 4, a = 7.9632(2), b = 15.2693(5), c = 8.0803(2) Å; R1 = 0.0261, wR2 = 0.0460, 1428 F2 values and 48 variables. The two crystallographic positions 8d and 4c show Ge/Ag mixing, leading to a slight increase in the lattice parameters as compared to those of the pure binary compound Ce5Ge4.

Synthesis and crystal structure of (Ag,Pd)22Se6

2013 ◽  
Vol 28 (1) ◽  
pp. 13-17 ◽  
Author(s):  
F. Laufek ◽  
A. Vymazalová ◽  
D.A. Chareev ◽  
A.V. Kristavchuk ◽  
J. Drahokoupil ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Glass Tube ◽  
Structure Type ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
Silica Glass Tube

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.

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