Darstellung und Kristallstruktur des Bis(diisobutylammonium)-heptasulfids [H2N(i-C4H9)2]2S7 / Synthesis and Crystal Structure of Bis(diisobutylammonium)-heptasulfide [H2N(i-C4H9)2]2S7

1993 ◽  
Vol 48 (12) ◽  
pp. 1732-1736 ◽  
Author(s):  
C. Müller ◽  
P. Böttcher

The reaction of diisobutylamine, H2S, and sulfur in a mixture of dimethylformamide, formamide, and ethanol yields orange crystals of bis(diisobutylammonium)-heptasulfide. The compound crystallizes in the centrosymmetric orthorhombic space group Pbca, the lattice constants are a = 11.234(4), b = 17.875(7), c = 27.009(10) Å. The S72-chain does not have the common helical all-trans-conformation, but a mixed conformation trans-cis-trans (sequence of the signs of torsion angles + + - - and - - + +).

1994 ◽  
Vol 49 (4) ◽  
pp. 489-493 ◽  
Author(s):  
C. Müller ◽  
P. Böttcher

The reaction of trimethylamine, H2S, and sulfur in ethanol yields orange crystals of bis(trimethylammonium) hexasulfide. The com pound crystallizes in the centrosymmetric monoclinic space group P 2/c. The lattice constants are a = 10.310(7), b = 5.752(2), c = 13.348(10) Å, β = 98.41(6)°. The S26-chain has a helical all-trans-conformation (sequence of the signs of torsion angles +++ and --- ).


1993 ◽  
Vol 48 (1) ◽  
pp. 90-92 ◽  
Author(s):  
C. Müller ◽  
P. Böttcher

The reaction of dicyclohexylamine and sulphur (molar ratio 2:7) with H2S in a mixture of dimethylformamide and formamide yields red crystals of bis(dicyclohexylammonium)heptasulfide. The compound crystallizes in the centrosymmetric space group P21,/c, the lattice constants are a = 9.787(2) Å, b = 18.972(4) Å, c = 17.118(3) Å, β = 96,12(2)°. The S72- chain has not the common helical all-trans-conformation, but a mixed conformation trans-cis-trans (sequence of the signs of torsion angles ++ - - and - - ++).


1988 ◽  
Vol 43 (1) ◽  
pp. 21-24 ◽  
Author(s):  
A. Schliephake ◽  
H. Falius ◽  
H. Buchkremer-Hermanns ◽  
P. Böttcher

Abstract The preparation and crystal structure of the first octasulfide is described. The reaction of triethylamine, sulfur and dihydrogen sulfide in a solution of formamide yields orange-red crystals of bis(triethylammonium)octasulfide. The crystals are orthorhombic, space group Pbcn. with 4 molecules per unit cell. The cell constants are a = 23.709(4) Å. b = 13.276(4) Å. c = 7.388(2) Å. The chains of sulfur, S82-, do not show the common helical all-trans conformation, but a mixed sequence with the signs of the dihedral angles (++−++ and −−+−−).


1991 ◽  
Vol 46 (5) ◽  
pp. 699-702 ◽  
Author(s):  
Rolf Buschmann ◽  
Hans-Uwe Schuster

A new compound LiCo6P4 could be synthesized, it crystallizes in the hexagonal space group P6̅m2 with the lattice constants a = 658.4(3) pm, c = 333.8(2) pm, c/a = 0.507. The structure shows close relations to the Fe2P- or Zr2Fe12P7-type structures.


1991 ◽  
Vol 46 (1) ◽  
pp. 84-96 ◽  
Author(s):  
Norbert Niederprüm ◽  
Roland Boese ◽  
Günter Schmid

Using a miniature zone melting device with focused infrared light it was possible to grow crystals of bis(dimethylamino)methylborane (1) and bis(monomethylamino)methylborane (2) at temperatures o f 182 K and 177 K, respectively. The crystal structure and the X - X difference electron density have been determined at temperatures o f 120 K (1) and 115 K (2).1 crystallizes in the orthorhombic space group Pbca with a = 758.87(7), b = 1559.74(12) and c = 1296.73(12) pm. The mean B - N distance is 143.1(3) pm.2 crystallizes in the monoclinic space group P21/c with a = 775.06(6), b = 1533.94(17), c = 1011.06(10) pm and β = 102.669(7)° with intermolecular N ··· H hydrogen bridges. The mean B - N distance is 141.5(2) pm.It is shown that the variation of torsion angles at small angles has more influence on bond lengths than the same or a greater variation at large angles and that it is necessary to pay more attention to the torsion angles ( C - B - N - C ) rather than to the interplanar angles (plane N ,B,N - plane N ,C,C ).


1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.


1982 ◽  
Vol 37 (11) ◽  
pp. 1361-1368 ◽  
Author(s):  
H.-J. Schweizer ◽  
Reginald Gruehn

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.


1988 ◽  
Vol 41 (7) ◽  
pp. 1127 ◽  
Author(s):  
SF Colmanet ◽  
MF Mackay

The reaction of sodium 1,2-dicyanoethenedithiolate [( mnt )Na2] with (NH4)2 [TcBr6] in ethanol yields crystals of (AsPh4)2 [ Tc ( mnt )3] (1) after precipitation with AsPh4Cl. The crystal structure of (1) has been determined by X-ray diffraction. Crystals are orthorhombic, space group Pbcn , a 20.256(1), b 15.513(1), c 18.274(1)Ǻ, Z 4. Refinement on 2910 diffractometer data measured with Cu Kα radiation converged at R 0.056. The structure consists of [ Tc ( mnt )3]2- anions and (AsPh4)+ cations . The technetium(IV) atom is coordinated to six sulfur atoms to give a distorted octahedron.


1989 ◽  
Vol 44 (5) ◽  
pp. 615-618 ◽  
Author(s):  
Evamarie Hey ◽  
S. Bruce Wild ◽  
Simon G. Bott ◽  
Jerry L. Atwood

The unit cell of (R*,R*)-(±)-[(η5-C5H5){1.2-C6H4(PMePh)2}Fe(PCl3)]Cl · 2 MeCN is orthorhombic, space group Pccn, with a = 1531.2(3). b = 2202.7(20). c = 1874.6(16) pm, and Z = 8. The salt crystallizes as a racemic compound with four pairs of asymmetric cations of opposite helicity and associated anions and solvent molecules in each unit cell.


1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke

[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.


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