scholarly journals Synthese und Kristallstruktur von [WCl3(N 3S2)(Pyridin)] / Synthesis and Crystal Structure of [WCl3(N3S2)(Pyridine)]

1986 ◽  
Vol 41 (6) ◽  
pp. 796 ◽  
Author(s):  
Heribert Wadle ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crystal Data ◽  
Pyridine Ligand ◽  
Tungsten Atom ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
In Trans ◽  
Moisture Sensitive

[WCl3(N3S2)(pyridine)] was obtained by the reaction of a mixture of S5N5[WCl4(N3S2)] and S4N3[WCl4(N3S2)] with pyridine in dichloromethane. It forms brown, moisture-sensitive crystal plates and was characterized by its IR spectrum and an X-ray crystal structure determination (1404 ob­served reflexions. R = 0.052). Crystal data: ortho­rhombic, space group Pbca. Z = 8, a = 708.3, b = 1275.4, c = 2628.6 pm. The tungsten atom has a distorted octahedral coordination and is part of a planar WN3S2 ring with WN bond lengths of 176 and 186 pm. The pyridine ligand (W−N 232 pm) is in trans position to the shorter WN bond.

Synthese und Kristallstruktur von VBr2(N3S2)(Pyridin)2/ Synthesis and Crystal Structure of VBr2(N3S2)(pyridine)2

1986 ◽  
Vol 41 (7) ◽  
pp. 831-833 ◽  
Author(s):  
Wolfgang Willing ◽  
Ruth Christophersen ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Chloro Complex ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
Moisture Sensitive

AbstractVBr2(N3S2)(pyridine)2 is obtained in form of brown-black, moisture sensitive crystals by the reaction of the corresponding chloro complex with trim ethylbrom osilane. The com pound is characterized by its IR spectrum and an X-ray crystal structure determination (1322 observed reflexions, R = 0.077). Crystal data: monoclinic, space group Aba2, Z = 4, a = 1100.3, b = 1480.0, c = 983.3 pm. A molecular structure with a distorted octahedral coordination for the vanadium atoms was found: there are two short VN bonds o f 178 pm with two N atoms o f the planar N3S2 chelate, two long (228 pm) VN(pyridine) bonds trans to the former VN bonds and two bromo ligands.

Synthese und Kristallstruktur des Dichloroselenonitren-Komplexes (PPh4)2[WCl5(NSeCl2)] / Synthesis and Crystal Structure of the Dichloro-selenonitrene Complex (PPh4)2[WCl5(NSeCl2)]

1992 ◽  
Vol 47 (3) ◽  
pp. 301-304 ◽  
Author(s):  
Stefan Vogler ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Structure Determination ◽  
Selenium Atom ◽  
Tungsten Atom ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Octahedral

The title compound has been prepared by the reaction o f [WCl4(NSeCl)]2 with PPh4Cl in CH2Cl2 solution. It forms red crystals, which were characterized by an X-ray structure determination. Space group P21/c, Z = 4, 3856 observed unique reflections, R = 0.073. Lattice dimensions at 25 °C: a = 2266.0(5), b = 1121.0(2), c = 2013.0(4) pm, β = 109.66(3)°. The structure consists o f PPh4+ ions and anions [WCl5(NSeCl2)]2-, in which the tungsten atom is surrounded in a distorted octahedral way by five chlorine atoms and by the nitrogen atom of the (NSeCl2)3- ligand. The W = N = SeCl2 group is characterized by WN and SeN double bonds; the selenium atom has a pseudo trigonal-bipyramidal coordination with the N atom and two lone pairs in equatorial and the chlorine atoms in axial positions.

[Na-15-Krone-5][MoF2Cl2(N3S2)]; Synthese und Kristallstruktur / [Na-15-Crown-5][MoF2Cl2(N3S2)]; Synthesis and Crystal Structure

1988 ◽  
Vol 43 (10) ◽  
pp. 1235-1239 ◽  
Author(s):  
Karin Völp ◽  
Gerhard Baum ◽  
Werner Massa ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ion Pairs ◽  
Sodium Atom ◽  
Acetonitrile Solution ◽  
Trans Position ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
In Trans ◽  
Ether Molecule

The cyclothiazeno complex [Na-15-crown-5][MoF2Cl2(N3S2)] has been prepared by the reaction of sodium fluoride with [MoCl3(N3S2)]2 in acetonitrile solution in the presence of [15-crown-5]. The compound was characterized by its IR spectrum as well as by an X-ray structure determination (3560 observed independent reflexions, R = 0.039). Crystal data: monoclinic, P21/n, Z = 4; a = 1044.8(2); b = 1513.7(2); c = 1363.8(3) pm; β = 104.33(2)°. The structure consists of ion pairs, in which the sodium atom is seven-coordinated by the oxygen atoms of the crown ether molecule and by the two fluorine ligands of the [MoF2Cl2(N3S2)]- unit. The molybdenum atom is a member of the planar MoN3S2 ring; the fluorine atoms are coordinated in trans position to the nitrogen atoms of the cyclothiazeno ring.

Synthese und Kristallstruktur des cyclischen Hydrazido-Komplexes {Fe2Cl4[(NSiMe3)(CPh)]2N2} / Synthesis and Crystal Structure of the Cyclic Hydrazido Complex {Fe2Cl4[(NSiMe3)(CPh)]2N2}

1989 ◽  
Vol 44 (4) ◽  
pp. 495-498 ◽  
Author(s):  
Wolfgang Hiller ◽  
Eva Hartmann ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Title Compound ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Data Space ◽  
Moisture Sensitive

The title compound has been prepared by the reaction of FeCl3 with N, N, N′-tris(trimethylsilyl) benzamidine in CH2Cl2 solution as dark red, moisture-sensitive crystals. The complex was characterized by its IR spectrum as well as by an X-ray structure determination.Crystal data: space group P21/n, Z = 2 (1178 observed independent reflexions, R = 0.089). Lattice dimensions (20 °C): a = 1240.2(2), b = 645.7(3), c = 1779.7(3) pm, β = 91.31(2)°. The compound forms centrosymmetric molecules, in which the iron atoms are members of two fused planar heterocycles with the NN group as the com m on edge. The NN bond length (142.5(9) pm) is very close to the NN bond length of hydrazine.

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.

Dichlorcyclopropenon als stabiler Komplexligand. Die Kristallstruktur von [NbOCl3·OC3Cl2]4 / Dichlorocyclopropenone as Stable Complex Ligand. The Crystal Structure of [NbOCl3·OC3Cl2]4

1988 ◽  
Vol 43 (7) ◽  
pp. 795-800
Author(s):  
Ute Patt-Siebel ◽  
Helmut Thullen ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Partial Hydrolysis ◽  
Stable Complex ◽  
Crystal Data ◽  
X Ray ◽  
Data Space ◽  
In Trans ◽  
Moisture Sensitive ◽  
Hydrolysis Of ◽  
Complex Ligand

The reaction of tetrachlorocyclopropene with NbOCl3 yields NbCl5·OC3Cl2 (1); 1 is also formed by partial hydrolysis of C3Cl3+NbCl6- (2), which is prepared from C3Cl4 and NbCl5. [NbOCl3·OC3Cl2]4 (3) was obtained by hydrolysis of 1 in form of pale-yellow, moisture sensitive, non-explosive crystals, and characterized by its IR spectrum and an X-ray crystal structure determination (1871 independent observed reflexions, R = 0.048). Crystal data: space group P1̄. Z = 2. a = 993.7(4), b = 1090.5(5). c = 1097.4(3) pm, α = 69.51(3), β = 70.47(3), γ = 66.51(4)° (at -17 °C). 3 consists of centrosymmetrical tetramers; the four Nb atoms form a square and are linked via almost linear oxo groups with alternating short and long NbO bonds with mean bond lengths of 175 and 208 pm. In trans position of each of the short NbO bonds a dichlorocyclopropenone molecule is attached via its oxygen atom with an NbO distance of 223 pm.

S5N5[SnCl5(CH3CN)]; Synthese, IR-Spektrum, 119Sn-Mößbauer-Spektrum und Kristallstruktur / S5N5[SnCl5(CH3CN)]; Synthesis, IR Spectrum , Mössbauer Spectrum and Crystal Structure

1986 ◽  
Vol 41 (10) ◽  
pp. 1191-1195 ◽  
Author(s):  
Ute Patt-Siebel ◽  
Somluck Ruangsuttinarupap ◽  
Ulrich Müller ◽  
Jürgen Pebler ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Bond Angle ◽  
Mossbauer Spectrum ◽  
Monoclinic Space Group ◽  
Mössbauer Spectrum ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral

S5N5[SnCl5(CH3CN)] is prepared by the reaction of SnCl2 with trithiazyl chloride in acetonitrile suspension. The compound is characterized by its IR spectrum, the 119Sn Mössbauer spectrum and by an X-ray crystal structure determination (1851 observed, independent reflexions, R = 0.024). S5N5[SnCl5(CH3CN)] crystallizes in the monoclinic space group P21/n with Z = 4 and the lattice dimensions a = 758.8; b = 1574.6; c = 1429.1 pm; β = 97.65°. The compound consists of planar S5N5® cations with the azulene-like structure, and anions [SnCl5(CH3CN)]e in which the tin atom has a distorted octahedral coordination. The bond angle Sn-N ≡ C (168°) is surprisingly small.

scholarly journals (AsPh4)4[CrCl4(μ-N2S2)]4 · 8 CH2Cl2; Synthese, IR-Spektrum und Kristallstruktur / (AsPh4)4[CrCl4(μ-N2S2)]4 · 8 CH2Cl2; Synthesis, IR Spectrum and Crystal Structure

1985 ◽  
Vol 40 (10) ◽  
pp. 1314-1319 ◽  
Author(s):  
Heribert Wadle ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Major Product ◽  
X Ray ◽  
Lattice Constants ◽  
Chromium Hexacarbonyl ◽  
Distorted Octahedral Coordination ◽  
Chromium Vi ◽  
Distorted Octahedral ◽  
Tetraphenylarsonium Chloride ◽  
Crystal Structural

Trithiazylchloride, (NSCl)3, reacts with metallic chromium, with chromium hexacarbonyl, with CrCl3·3 thf, as well as with chromium(VI) oxide to form mixtures, in which S4N3⊕ [CrCl4(N2S2)]⊖ can be identified as the major product. This compound reacts with tetraphenylarsonium chloride in dichloromethane to form the title compound, which we have characterized by IR spectroscopy and an X-ray crystal structural analysis. (AsPh4)4[CrCl4(N2S2)]4·8 CH2Cl2 crystallizes monoclinically in the space group C2/c with four formula units per unit cell and with the following lattice constants at -100 °C: a = 2146, b = 2033, c = 3137 pm; β = 96.0° (9918 independent observed reflexions, R = 0.064). The compound consists of AsPh4⊕ ions, tetrameric anions [CrCl4(N2S2)]44⊖ and included CH2Cl2 molecules. The chromium atoms of the anions occupy the corners of a nearly ideal square; they are connected via the N-atoms of planar N2S2-rings, which are oriented perpendicularly to the Cr4-plane. The chromium atoms complete their distorted octahedral coordination with four terminal chlorine atoms, the axial ones of which form short Cl···S-contacts of average 310 pm to the S-atoms of the N2S2-rings.

Multianvil High-Pressure Synthesis And Crystal Structure Of β-YbBO3

2001 ◽  
Vol 56 (8) ◽  
pp. 697-703 ◽  
Author(s):  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Title Compound ◽  
Variable Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Oxygen Coordination ◽  
Distorted Octahedral ◽  
Pressure Synthesis ◽  
Octahedral Oxygen

β-Ytterbium borate (β-YbBO3) was synthesized under high-pressure in a Walker-type multianvil apparatus at 2.2 GPa and 1400 °C. The title-compound crystallizes in the trigonal calcite structure, space group R3̄̄c. Single crystal X-ray data yielded a = 492.1(2), c = 1630.5(9) pm, wR2 = 0.0344 for 165 F2 values and 11 variable parameters. Within the trigonal planar BO3 groups the B-O distance is 137.8(4) pm. The ytterbium atoms have a slightly distorted octahedral oxygen coordination (Yb-O: 224.4(2) pm)

Synthese, IR-Spektrum und Kristallstruktur des Amidinatokomplexes [Na(15-Krone-5)][Ph—C(NSiMe3)2SnCl3F] / Synthesis, IR Spectrum, and Crystal Structure of the Amidinato Complex [Na(15-Crown-5)][Ph — C(NSiMe3)2SnCl3F]

1989 ◽  
Vol 44 (8) ◽  
pp. 889-892 ◽  
Author(s):  
John David Kildea ◽  
Wolfgang Hiller ◽  
Beatrice Borgsen ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Ion Pairs ◽  
Acetonitrile Solution ◽  
Trans Position ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Moisture Sensitive

The title compound [Na(15-crown-5)][C6H5–C(NSiMe3)2SnCl3F] is synthesized by the reaction of sodium fluoride with Ph—C(NSiMe3)2SnCl3 in acetonitrile solution in the presence of 15-crown-5 as white, moisture-sensitive crystals. The complex is characterized by its IR spectrum as well as by an X-ray structure determination. Space group P212121 Z = 4, 4897 observed independent reflexions, R = 0.094. Lattice dimensions at 20°C: a = 1065.7(2), b = 1431.0(2), c = 2325.6(3) pm. The compound forms ion pairs with a bent Sn–F–Na bridge (bonding angle 119.0(5)°) and distances Sn–F of 196(1) and Na–F of 232(1) pm. The tin atom is in a distorted octahedral environment defined by the two N atoms of the symmetrically coordinated amidinato ligand, by three chlorine atoms, and by the fluorine ligand; the latter is in a trans-position relative to one of the nitrogen atoms.

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