Notizen: [K(18-Krone-6)][WF5(NCl)]; Synthese und Kristallstruktur / [K(18-Crown-6)][WF5(NCl)]; Synthesis and Crystal Structure

1992 ◽  
Vol 47 (7) ◽  
pp. 1054-1056 ◽  
Author(s):  
Harald Stenger ◽  
Kurt Dehnicke ◽  
Wolfgang Hiller
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Bond Angle ◽  
Ion Pairs ◽  
Acetonitrile Solution ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ether Molecule

[K(18-crown-6)][WF5(NCl)] has been prepared as yellow crystals by the reaction of KF with WCl4(NCl) in the presence of 18-crown-6 in acetonitrile solution. The compound was characterized by its IR spectrum and by an X-ray structure determination. Space group P21/n, Z = 4, 3697 observed unique reflections, R = 0.034. Lattice dimensions at –65 °C: a = 1313.8(3), b = 851.2(1), c = 1842.7(4) pm, β = 95.304(1)°. The compound forms ion pairs, in which the pottassium ion is coordinated by the six oxygen atoms of the crown ether molecule and by two fluorine ligands of the [WF5(NCl)]- unit with K–F distances of 272.4(5) and 288.6(5) pm. The W=N–Cl group of the anion is nearly linear (bond angle 170.7(5)°) with bond lengths of WN = 172.4(7) and NCI = 162.7(7) pm.

Synthese und Kristallstruktur von [VCl2(15-Krone-5)]+[VOCl4]- / Synthesis and Crystal Structure of [VCl2(15-Crown-5)]+[VOCl4]-

1990 ◽  
Vol 45 (10) ◽  
pp. 1393-1397 ◽  
Author(s):  
Gerlinde Frenzen ◽  
Werner Massa ◽  
Thilo Ernst ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crown Ether ◽  
Single Crystals ◽  
Structure Determination ◽  
Acetonitrile Solution ◽  
Tetragonal Symmetry ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ether Molecule

[VCl2(15-crown-5)]+[VOCl4]- has been prepared by the reaction of VCl4 with 15-crown-5 in acetonitrile solution in the presence of water, forming black-brown single crystals. They were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1530 observed unique reflexions, R = 0.052. Lattice dimensions at -120°C: a = 1128.5(4), b = 1063.3(3), c = 1680(1) pm. The compound forms ions, in which the cation contains vanadium(+III), which is seven coordinate by the five oxygen atoms of the crown ether molecule and by two chlorine atoms in axial positions of a pentagonal bipyramide. The [VOCl4]- anion contains vanadium (+V) with approximately tetragonal symmetry

Synthese und Kristallstruktur von [Na-15-Krone-5][WF5(NCl)] / Synthesis and Crystal Structure of [Na-15-Crown-5][WF5(NCl)]

1989 ◽  
Vol 44 (2) ◽  
pp. 117-120 ◽  
Author(s):  
Astrid Görge ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Bond Angle ◽  
Ion Pairs ◽  
Sodium Ion ◽  
Acetonitrile Solution ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Data Space

[Na-15-crown-5][WF5(NCl)] has been prepared as yellow crystals by the reaction of NaF with WC14(NCl) in the presence of 15-crown-5 in acetonitrile solution. The compound was characterized by its IR spectrum as well as by an X-ray structure determination. Crystal data: space group P 21/n, Z = 4 (2945 observed, independent reflexions, R = 0.035). Lattice dimensions at - 65 °C: a = 827.2(8); b = 1617.3(13); c = 1372.2(10) pm; β = 99.42(5)°. The com pound forms ion pairs, in which the sodium ion is seven-coordinated by the oxygen atoms of the crown ether m olecule, and by two fluorine ligands of the [WF5(NCl)]- unit with Na -F distances of 228.3(6) and 251.3(6) pm. The W ≡ N-Cl group of the anion is nearly linear (bond angle 176.1(5)°) with bond lengths WN = 173.3(6) and NCI = 162.2(7) 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.

Synthese und Kristallstruktur von [Na-15-Krone-5][MoF5 (NCl)]

1988 ◽  
Vol 43 (9) ◽  
pp. 1125-1129 ◽  
Author(s):  
Dieter Fenske ◽  
Karin Völp ◽  
Kurt Dehnicke
Keyword(s):  
Crown Ether ◽  
Nmr Spectra ◽  
Bond Angle ◽  
Ion Pairs ◽  
Sodium Ion ◽  
Acetonitrile Solution ◽  
Crystal Data ◽  
X Ray ◽  
Data Space ◽  
Ether Molecule

Abstract [Na-15-Crown-5][MoF5(NCl)] has been prepared as yellow crystals by the reaction of NaF with MoF4(NCl) in the presence of 15-crown-5 in acetonitrile solution. The compound was charac­terized by its IR and 19F NMR spectra as well as by an X-ray structure determination. Crystal data: space group P21/n, Z = 4 (3736 observed, independent reflexions, R = 0.034). Lattice dimensions at -70 °C: a = 823.5(4). b = 1612.2(9), c = 1383.4(8), β = 99.35(3)°. The compound forms ion pairs, in which the sodium ion is seven-coordinated by the oxygen atoms of the crown ether molecule and by two fluorine ligands of the [MoF5(NCl)]- unit with Na-F distances of 228.3 and 249.6 pm. The Mo=N-Cl group of the anion is nearly linear (bond angle 175.8°) with bond lengths MoN = 172.9 and NCl = 161.8 pm.

[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.

[Na-15-Krone-5] [ReF2Cl2(NO)2]; Synthese, IR-Spektrum und Kristallstruktur / [Na-15-Crown-5][ReF2Cl2(NO)2]; Synthesis, IR Spectrum, and Crystal Structure

1989 ◽  
Vol 44 (11) ◽  
pp. 1393-1396 ◽  
Author(s):  
Stefan Vogler ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crown Ether ◽  
Ir Spectrum ◽  
Ion Pairs ◽  
Sodium Ion ◽  
X Ray ◽  
Moisture Sensitive ◽  
In Cis ◽  
Ether Molecule

[Na-15-crown-5][ReF2Cl2(NO)2] has been prepared by the reaction of ReCl3(NO)2 with sodium fluoride in acetonitrile suspension in the presence of 15-crown-5. It forms green, slightly moisture sensitive crystals, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/c, Z = 4, 4821 observed unique reflexions, R = 0.040. Lattice dimensions at —60 °C: a = 1024.6(7), b = 801.4(4), c = 2386.6(12) pm; β = 99.90(4)°. The compound forms ion pairs via two Na—F contacts with bond lengths of 239.8 and 233.4 pm. Thus the sodium ion is seven-coordinate by the five oxygen atoms of the crown ether molecule and by two fluorine ligands of the [ReF2Cl2(NO)2]- unit. The nitrosyl groups of the anion are in transposition to the fluorine atoms and in cis-position to one another (symmetry C2v).

scholarly journals Notizen: Synthese und Kristallstruktur von [Co(15-Krone-5)(CH3CN)2]CoCl4 · CH3CN / Synthesis and Crystal Structure of [Co( 15-Crown-5)(CH3CN)2]CoCl4 · CH3CN

1990 ◽  
Vol 45 (4) ◽  
pp. 563-566 ◽  
Author(s):  
Werner Massa ◽  
Thilo Ernst ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Structure Determination ◽  
Title Compound ◽  
Complex Ions ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Ether Molecule ◽  
Oxygen Atoms

The title compound has been prepared by the reaction of 15-crown-5 with a solution of CoCl2 in acetonitrile. It forms blue crystals, which were characterized by an X-ray structure determination. Space group Pca 21, Z = 4, 2883 observed unique reflexions, R = 0.032. Lattice dimensions at –80 °C: a = 1420.9(3), b = 1017.2(2), c = 1775.0(3) pm. The lattice contains the complex ions [Co(15-crown-5)(CH3CN)2]2+ and CoCl42-, and interstitial CH3CN molecules. In the cation CoII is seven-coordinate by the five oxygen atoms of the crown ether molecule and by two nitrogen atoms of the acetonitrile molecules in axial positions of a pentagonal bipyramide.

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 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 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.

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