Cyclothiazeno-Vanadiumdibromid, VBr2(N3S2) / Cyclo-Thiazeno Vanadium Dibromide, VBr2(N3S2)

1985 ◽  
Vol 40 (11) ◽  
pp. 1457-1462 ◽  
Author(s):  
Jürgen Hanich ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

VBr2(N3S2) was synthesized by reaction of VCl2(N3S2) with Me3SiBr. It reacts with PPh4Br in dibromomethane solution to form (PPh4)2[VBr3(N3S2)]2. The compounds were characterized by their IR and 51V NMR spectra. The crystal structure of VBr2(N3S2) was determined by X-ray diffraction (2060 reflexions. R = 0.114). Crystal data: triclinic, space group P1̄, a = 586.4, b = 794.2, c = 744.6 pm. α - 89.25, β - 108.58, γ = 99.67°. Z = 2. The vanadium atoms form planar, six-membered rings wjith the N3S2 groups, with short VN distances (172 and 185 pm). Bromine- bridged dimers are associated via V−N links to form chains in a similar way as in some tetrahalides. The structure is similar to that of VCl2(N3S2), but the chains are rotated by 17° along their axes.

Tetraphenylphosphonium-ikosioctabromooctaantimonat(III), (PPh4)4Sb8Br28 / Tetraphenylphosphonium Ikosioctabromooctaantimonate(III), (PPh4)4Sb8Br28

1996 ◽  
Vol 51 (9) ◽  
pp. 1245-1247 ◽  
Author(s):  
Wolfgang Fachbereich Biologie-Chemie, Univer ◽  
Ulrich Fachbereich Biologie-Chemie, Univer
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Closest Packing ◽  
Distorted Octahedral

The title compound was obtained by the reaction of PPh4Br, Sb2Se3, and bromine in dichloromethane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1249.1(2), b = 1307.8(2), c = 2152.3(4) pm, α = 102.93(2), β = 100.83(2), γ = 100.42(2)°, Z = 2, triclinic, space group P1̄. (PPh4)4Sb8Br28 is isotypic with (PPh4)4Sb8I28. The Sb8Br284- ion can be taken as the association product of eight SbBr3 molecules with four Br− ions. Each Sb atom has a distorted octahedral coordination with three shorter (252 to 274 pm) and three longer (300 to 353 pm) Sb-Br bonds. The octahedra share common edges in two parallel rows of four octahedra each. The arrangement of the 28 bromine atoms corresponds to a section of a closest packing of spheres.

Preparation and Crystal Structure of New 1,3-Diaza-λ5,λ5-diphosphetidines

1986 ◽  
Vol 41 (10) ◽  
pp. 1201-1205 ◽  
Author(s):  
Ch. Donath ◽  
M. Meisel ◽  
K .-H . Jost ◽  
K. K. Palkina ◽  
S. I. Maksimova ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Methyl Ester ◽  
Single Crystal ◽  
Fractional Crystallization ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Benzyl Amine

Abstract Reaction of py · PS2Cl (py = pyridine) with benzyl amine in the presence of NEt3 yields triethyl-ammonium 1,3-dibenzyl-2,4-dithioxo-1,3-diaza-2λ5,4λ5-diphosphetidine-2,4-dithiolate which reacts with MeI to give the corresponding methyl ester. By fractional crystallization from cyclohexane three modifications of the methyl ester were obtained (two trans-(A and A') and one cis-modification (B)). The crystal structure of these modifications have been determined by single crystal X-ray diffraction. Crystal data: A: triclinic, space group P1̄ , Z = 2, a = 7.100(3), b = 10.088(6), c = 17.785(6) Å , α = 99.18(4)°, β = 93.75(5)°, γ = 106.96(4)°, A': monoclinic, P21/c, Z = 2, a = 7.933(3), b = 13.689(3), c = 9.917(4) Å, β = 111.98(3)°; B: orthorhombic, P cab, Z = 8, a = 12.962(6), b = 16.581(6), c = 19.475(7).

Bildung von Arsensäure aus [As2Cl8]2Ionen und Ozon. Die Kristallstruktur von PPh4Cl · H3AsO4 / Formation of Arsenic Acid from [As2Cl8]2- Ions and Ozone. Crystal Structure of PPh4Cl · H3AsO4

1992 ◽  
Vol 47 (12) ◽  
pp. 1677-1680 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Alfred-Dirk Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
X Ray Diffraction ◽  
Arsenic Acid ◽  
Subsequent Reaction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Reaction of ozone with (PPh4)2[As2Cl8] in CH2C12 at low temperatures yields a red compound, possibly an ozonide. Upon evaporation of the solvent at –78 °C the ozone is released again. At -40 °C or above a subsequent reaction yields PPh4[AsCl6], PPh4Cl · H3AsO4, and other products. The crystal structure of PPh4Cl · H3AsO3 was determined by X-ray diffraction (4253 observed reflexions, R = 0.031). It is triclinic, space group P1̅, and consists of H3AsO4 molecules joined to dimer units via H bridges and associated via O–H · · · Cl- bridges to strands. The packing of the PPh4+ ions is discussed. Products of the reaction of (PPh4)2[Sb2Cl8] with ozone in CH2C12 are PPh4[SbCl6] and (PPh4)2[SbOCl4]2 · 2 CH2Cl2.

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

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.

Crystal structure and thermal expansion of hexakis(phenylthio)benzene and its CBr4 clathrate

1995 ◽  
Vol 73 (4) ◽  
pp. 513-521 ◽  
Author(s):  
Darek Michalski ◽  
Mary Anne White ◽  
Pradip K. Bakshi ◽  
T. Stanley Cameron ◽  
Ian Swainson
Keyword(s):  
Crystal Structure ◽  
Thermal Expansion ◽  
Neutron Powder Diffraction ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Temperature Range ◽  
Thermal Expansion Coefficients ◽  
Expansion Coefficients

The crystal structures of hexakis(phenylthio)benzene (HPTB) and its CBr4 clathrate have been determined by single crystal X-ray diffraction data collected at T = 18 °C and refined to final Rw of 0.036 and 0.047, respectively. Pure HPTB is triclinic, space group [Formula: see text] (No. 2), with a = 9.589(2) Å, b = 10.256(1) Å, c = 10.645(2) Å, α = 68.42(1)°, β = 76.92(2)°, γ = 65.52(1)°, and Z = 1. The CBr4 clathrate of HPTB is rhombohedral, space group [Formula: see text] (No. 148), with a = 14.327(4) Å, b = 20.666(8) Å, and Z = 3. The host–guest mole ratio of HPTB–CBr4 is 1:2. Neutron powder diffraction was carried out on powders of both compounds in the temperature range 25 K < T < 295 K. Thermal expansion coefficients were determined for HPTB and HPTB–CBr4 over this temperature range. Keywords: thermal expansion, crystal structure, clathrate.

Cyclo-thiazenokomplexe von Vanadium(V) Die Kristallstruktur von (AsPh4)2[V(N3)3(N3S2)]2 · CH2Cl2 / Cyclo-thiazeno Complexes of Vanadium(V) The Crystal Structure of (AsPh4)2[V(N3)3(N3S2)]2 · CH2Cl2

1984 ◽  
Vol 39 (12) ◽  
pp. 1686-1695 ◽  
Author(s):  
Jürgen Hanich ◽  
Magda Krestel ◽  
Ulrich Müller ◽  
Kurt Dehnicke ◽  
Dieter Rehder
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Nmr Spectra ◽  
Formula Unit ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Nmr Data ◽  
Donor Acceptor

An improved synthesis for [VCl2(N3S2)]∞, was found in the reaction of VOCl3 with (NSCl)3; when the reaction is performed in H2CCl2 and (NSCl)3 is used in excess, the thiazyl-solvate [VCl2(N3S2) · NSCl]2 is obtained. [VCl2(N3S2)] reacts with AsPh4Cl to form (AsPh4)2[VCl3(N 3S2)]2; this reacts with AgN3 in CH2Cl2 suspension to yield (AsPh4)2[V (N3)3(N3S2)]2 · CH2Cl2. The compounds were characterized by their IR and 51V NMR spectra. The latter are compared with new 51V NMR data for [VO2Cl2]⊖ and [VOCl4]⊖ ; a decrease of 51V shielding in the order [VO2Cl2]⊖ > [VOCl4]⊖ > [VX3(N3S2)]22⊖ (X - N3 > Cl) is found, which is interpreted in terms of increasing polarizability of the ligands and of ring contributions to the extreme deshielding observed with the thiazenovanadates.The crystal structure of (AsPh4)2[V(N3)3(N3S2)]2 · CH2Cl2 was determined from X-ray diffraction data (1496 observed reflexions, R = 0.058). It crystallizes in the triclinic space group P 1̄ with one formula unit per unit cell and with the lattice constants a - 1087, b = 1317, c = 1350 pm, α = 58.8, β = 85.9, γ = 68.0°. The structure consists of AsPh4⊕ ions, CH2Cl2 molecules and centrosymmetric [V(N3)3(N3S2)]22⊖ anions. In the latter. N3S2 ligands are bonded to the V atoms in a chelate manner with short V = N bonds (189 and 172 pm) forming planar VN3S2 rings. The dimerization is accomplished by V -N donor-acceptor interactions (224 pm) involving one N atom of each VN3S2 ring. The vanadium coordination number of 6 is com pleted by three azido groups with V -N bond distances of 200 to 204 pm.

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.

The Structure of the Tetranuclear Cubane-Like Nickel(II) Xanthate Alkoxide [Ni(C2H5OCS2)-(C5H4NCH2O)]4 as Its Acetone Solvate, an Example of a Non-Reversible Inclusion Compound

1986 ◽  
Vol 39 (7) ◽  
pp. 1035 ◽  
Author(s):  
K Bizilj ◽  
SG Hardin ◽  
BF Hoskins ◽  
PJ Oliver ◽  
ERT Tiekink ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Inclusion Compound ◽  
Mixed Ligand ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Oxygen Atoms

The crystal structure of the acetone solvate of a mixed ligand tetranuclear nickel(II) complex involving the pyridine-2-methoxide ( pym ) and 0-ethylxanthate (exa) anions has been determined by X-ray diffraction methods. Crystals of [Ni (exa)( pym )]4.Me2CO are triclinic, space group Pī , a 13.825(2), b 15.606(3), c 12.288(2)Ǻ, α 101.16(2), β 101.38(1), γ 85.80(1)°, with Z 2; R and Rw were 0.056 and 0.057 respectively for 4,771 unique reflections for which I ≥ 3σ(I). The structure consists of tetranuclear cubane -like clusters with four nickel and four oxygen atoms arranged at alternate corners of a distorted cube. The discrete molecules of occluded acetone are located in cavities defined by the [Ni( exa )( pym )]4 units.

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