Synthesen und Kristallstrukturen der Kronenether-Komplexe (18-Krone-6) · 2CH3CN, [Na-15-Krone-5][ReO4] · CH3CN und [Na-15-Krone-5]PF6 / Syntheses and Crystal Structures of the Crown Ether Complexes (18-Crown-6) · 2 CH3CN, [Na-15-Crown-5][ReO4] · CH3CN, and [Na-15-Crown-5]PF6

1989 ◽  
Vol 44 (12) ◽  
pp. 1524-1530 ◽  
Author(s):  
Frank Weller ◽  
Harald Borgholte ◽  
Harald Stenger ◽  
Stefan Vogler ◽  
Kurt Dehnicke
Keyword(s):  
Crown Ether ◽  
Sodium Fluoride ◽  
Ion Pairs ◽  
Sodium Atom ◽  
Acetonitrile Solution ◽  
Space Group ◽  
Crown Ether Complexes ◽  
Water Space ◽  
Ether Molecule ◽  
Oxygen Atoms

Single crystals of (18-crown-6) · 2 CH3CN were obtained by cooling a solution of 18-crown-6 in acetonitrile to 4 °C. Space group P21/n, Z = 2, 629 observed independent reflexions, R = 0.062. Lattice dimensions at 19°C: a = 911.7(1), b = 852.0(1), c = 1370.0(2) pm; β = 104.61(1)°. The compound forms a molecular structure with approximate D3d symmetry of the crown ether molecule, and C—H ··· O interactions of the acetonitrile molecules with the crown ether, the Η···Ο distances being 243, 253, and 267 pm, respectively.[Na-15-crown-5][ReO4] · CH3CN is formed as a by-product of the reaction of ReNCl4 with sodium fluoride in acetonitrile in the presence of 15-crown-5 and traces of water. Space group Ρ 1̄ , Ζ = 2, 3107 observed independent reflexions, R = 0.045. Lattice dimensions at 19°C: a = 823.4(1), b = 1078.8(1), c = 1204.0(1) pm; α = 112.40(1)°, β = 94.35(1)°, γ = 104.63(1)°. The compound forms ion pairs, in which the sodium atom is sixfold coordinated by the five oxygen atoms of the crown ether molecule, as well as by one oxygen atom of the ReO4- ion, which is only slightly distorted. The bond length Na—OReO3 is 237.8(8) pm, the bond angle NaORe is 164.3(5)°.[Na-15-crown-5]PF6 is formed in the reaction of [ReCl3(NSCl)2 · POC13] with sodium fluoride in acetonitrile solution in the presence of 15-crown-5. Space group Pna21, Ζ = 4, 1130 observed independent reflexions, R = 0.123. The high R value is due to disorder of the skeletal atoms of the crown ether molecule. The compound forms ion pairs, in which the sodium atom is sevenfold coordinated by the five oxygen atoms of the crown ether molecule, as well as by two fluorine atoms of the PF6- ion with Na—F bond lengths of 240(2), and 246(2) pm, respectively.

Synthesen und Kristallstrukturen der Kronenether-Komplexe [Li3(12-Krone-4)3O2CCH3] [Cd(Se4)2], {[K(18-Krone-6)]2[Hg(Se4)2]}2 und [Na(15-Krone-5)]NO3 / Syntheses and Crystal Structures of the Crown Ether Complexes [Li3(12-Crown-4)33O2CCH3][Cd(Se4)2], {[K(18-Crown-6)]2[Hg(Se4)2]}2, and [Na(15-Crown-5)]NO3

1989 ◽  
Vol 44 (4) ◽  
pp. 444-454 ◽  
Author(s):  
Gertrud Kräuter ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Crown Ether ◽  
Ion Pairs ◽  
Sodium Atom ◽  
Ethanolic Solution ◽  
Lithium Ions ◽  
Space Group ◽  
Crown Ether Complexes ◽  
Structure Determinations ◽  
Centrosymmetric Dimers ◽  
Oxygen Atoms

[Li3(12-crown-4)3O2CCH3][Cd(Se4)2] has been prepared by the reaction of [Li(12-crown-4)]2Se6 with Cd(C2CCH3)2 in ethanolic solution. The corresponding polyselenide complex of mercury is formed by the reaction of [K(18-crown-6)]2Se6 with Hg(O2CCH3)2 in the same solvent. Both com pounds form dark red crystals, which were characterized by single crystal X-ray structure determinations. The only product to be isolated from the reaction of Bi(NO3)3·5H2O with [Na( 15-crown-5)]2Se6 in ethanolic solution was [Na(15-crown-5)]NO3, whose structure has also been determined. [Li3(12-crown-4)3O2CCH3][Cd(Se4)2]: space group Pbca, Z = 8. 1404 observed independent reflexions. R = 0.097. Lattice dimensions (19 °C): a = 1981.5(6). b = 1400.3( 1), c = 3268.9(9) pm. The compound forms a dicationic ensemble, in which three lithium ions coordinate with the oxygen atoms of the acetate ion. In the anions the cadmium atom is coordinated tetrahedrally by four selenium atoms of two Se42- units.{[K (18-crown-6)]2[Hg(Se4)2]}2: space group P 1, Z = 1. 3210 observed independent reflexions, r = 0.055. Lattice dimensions (19 °C): a = 1057.4(2). b = 1130.6(2), c = 2000.1(2) pm. α = 88.52(1)°, β = 85.86(1)°, γ = 66.22(1)°. The com pound has a complex ionic structure, in which the formula units form centrosymmetric dimers through K-O contacts between two cations. In addition there are K···Se contacts with the spiro-bicyclic anions, which - together with 6 K-O bonds within the crowns - lead to the coordination number of 8 for the remaining potassium ions.[Na(15-crown-5)]NO3: space group P212121, Z = 4. 1211 observed independent reflexions. R = 0.052. Lattice dimensions (20 °C): a = 912.9(2). b = 989.6(1). c = 1658.3(3) pm. The compound forms ion pairs, in which the sodium atom coordinates with the five oxygen atoms oi the crown ether, as well as with two oxygen atoms of the nitrate ion with Na -O bond lengths of 240 and 247 pm.

Synthese und Kristallstrukturen der ionischen Kronenetherkomplexe [TiCl3(15-Krone-5)(CH3CN)][SbCl6) und [VCI(OH)(18-Krone-6)(CH3CN)2][SbCl6] · ½(18-Krone-6 · CH3CN) / Synthesis and Crystal Structures of the Ionic Crown Ether Complexes [TiCl3(15-Crown-5)(CH3CN)][SbCl6) und [VCI(OH)(18-Crown-6)(CH3CN)2][SbCl6] · ½(18-Crown-6 · CH3CN)

1993 ◽  
Vol 48 (2) ◽  
pp. 149-155 ◽  
Author(s):  
Michael Plate ◽  
Gerlinde Frenzen ◽  
Kurt Dehnicke
Keyword(s):  
Crown Ether ◽  
Chlorine Atom ◽  
Titanium Atom ◽  
Hydroxyl Group ◽  
Acetonitrile Solution ◽  
Antimony Pentachloride ◽  
Space Group ◽  
Structure Determinations ◽  
Ether Molecule ◽  
Oxygen Atoms

AbstractThe title compounds were prepared by the reaction of titanium tetrachloride with 15-crown-5 and antimony pentachloride, and by the reaction of vanadium trichloride with 18-crown-6 and antimony pentachloride in the presence of traces of water in acetonitrile solution, respectively. The complexes were characterized by IR spectroscopy and by X-ray structure determinations.[TiCl3(15-crown-5)(CH3CN)][SbCl6]: Space group Pnma, Z = 4, 1355 observed unique reflections, R = 0.035. Lattice dimensions at -80 °C: a = 1987(1), b = 1742.2(6), c = 111.0(2) pm. The compound consists of SbCl6- anions and cations [TiCl3(15-crown-5)(CH3CN)]+, in which the titanium atom is coordinated octahedrally by three chlorine atoms in facial arrangement, by the nitrogen atom of the acetonitrile molecule, and by two oxygen atoms of the crown ether molecule.[VCl(OH)(18-crown-6 )(CH3CN)2][SbCl6] · ½(18-crown-6 · CH3CN); Space group P 1̄, 3936 observed unique reflections, R = 0.714. Lattice dimensions at -80 °C: a = 1194.2(6), b = 1349.8(6), c = 1365.5(6) pm, α = 93.55(4)°, β = 111.23(4)°, γ = 93.15(4)°. The compound consists of SbCl6- anions, included 18-crown-6 and acetonitrile molecules, and cations [VCl(OH)(18-crown-6)(CH3CN)2]+, in which the vanadium atom is octahedrally coordinated by two nitrogen atoms of the acetonitrile molecules in trans positions, by a chlorine atom and a hydroxyl group in cis position, and by two oxygen atoms of the crown ether molecule. One of the acetonitrile molecules forms weak hydrogen bridges with two oxygen atoms of the included crown ether molecule as well as with one chlorine atom of the SbCl6- ion.

Spektroskopische Untersuchung des [FCl2V(15N3S2)]--Ions; Kristallstruktur von [Na-Benzo-15-Krone-5][FCl2V(N3S2)] / Spectroscopic Investigation of the Ion [FCl2V(15N3S2)]-; Crystal Structure of [Na-Benzo-15-Crown-5][FCl2V(N3S2)]

1989 ◽  
Vol 44 (11) ◽  
pp. 1385-1392 ◽  
Author(s):  
Dieter Rehder ◽  
Dieter Fenske ◽  
Gerhard Baum ◽  
Harald Borgholte ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Fluorine Atom ◽  
Nmr Spectra ◽  
Ion Pairs ◽  
Sodium Atom ◽  
Space Group ◽  
Trigonal Bipyramidal ◽  
R Value ◽  
Ether Molecule

[Na-15-crown-5][FX2V(N3S2)] (X = Cl, Br) and [Na-benzo-15-crown-5][FCl2V(N3S2)] have been prepared by reactions of X2V(N3S2) with sodium fluoride in acetonitrile suspensions in the presence of 15-crown-5 and benzo-15-crown-5, respectively. The 15N-labeled complex [Na-15-crown-5]-[FCl2V(15N3S2)] was also prepared and characterized by 15N, 19F, and 51V NMR spectra, as well as by IR spectroscopy.Whereas the crystal structure of [Na-15-crown-5][FCl2V(N3S2)], owing to disorder of the crown ether molecule, could be refined only to an R-value of 0.16 (space group C2/m, Z = 4, a = 1995.4(11); b = 1016.2(6); c = 1047.2(8) pm; β = 100.83(4)° at —65 °C), the crystal structure of the corresponding [Na-benzo-15-crown-5][FCl2V(N3S2)] was determined without complications. Space group P2,/c, Z = 4, 5565 observed independent reflexions, R = 0.036. Lattice dimensions at 20 °C: a = 1198.9(6); b = 970.3(5); c = 1918.2(10) pm; β = 93.74(3)°. The compound forms ion pairs, in which the sodium atom is seven-coordinated by the oxygen atoms of the crown ether molecule, the fluorine atom and one chlorine atom of the trigonal-bipyramidal [FCl2V(N3S2)]- unit. The vanadium atom is part of a planar VN3S2 ring; fluorine and two nitrogen atoms of the cyclothiazeno ring occupy the equatorial positions.

Ionische Kronenetherkomplexe von Thallium(I), Blei(II) und Indium(III). Die Kristallstrukturen von [T1(12-Krone-4)2] [SbC6], [Pb(15-Krone-5)2] [SbCl6]2 • [SbCl3(15-Krone-5)] und [In(12-Krone-4)2] [SbCl6]3· 3 CH3CN / Ionic Crown Ether Complexes of Thallium(I), Lead(II), and Indium(III). Crystal Structures of [T1(12-Crown-4)2][SbCl6], [Pb(15-Crown-5)2] [SbCl6]2 • [SbCl3(15-Crown-5)], and [In(12-Crown-4)2] [SbCl6]3 · 3 CH3CN

1993 ◽  
Vol 48 (10) ◽  
pp. 1331-1340 ◽  
Author(s):  
Henning von Arnim ◽  
Kurt Dehnicke ◽  
Klaus Maczek ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Lone Pair ◽  
Acetonitrile Solution ◽  
Lead Ion ◽  
Space Group ◽  
Crown Ether Complexes ◽  
Structure Determinations ◽  
Lead Complex ◽  
Oxygen Atoms

The ionic crown ether complexes [Tl(12-crown-4)2][SbCl6] (1) and [In(12-crown-4)2][SbCl6]3·3 CH3CN (3) have been prepared by reaction of T1C1 and InCl3, respectively, with SbCl5 in the presence of 12-crown-4 in acetonitrile solution. The lead complex [Pb(15-crown-5)2][SbCl6]2· [SbCl3(15-crown-5)] (2) has been obtained from the reaction of Pb(CH3)2Cl2 with SbCl5 in the presence of 15-crown-5 in acetonitrile solution. 1-3 were characterized by crystal structure determinations.[Tl(12-crown-4)2][SbCl6] (1): Space group C2/c, Z = 4, 2306 observed unique reflections, R = 0.051. Lattice dimensions at -70°C: a = 2360.9(5), b = 1189.6(2), c = 1080.4(3) pm, β = 111.14(2)°. 1 contains cations [Tl(12-crown-4)2]+, in which the Tl+ ion is coordinated sandwichlike by the eight oxygen atoms of the two crown ether molecules. The lone pair at the thallium ion shows steric activity.[Pb(15-crown-5)2][SbCl6]2·[SbCl3(15-crown-5)] (2): Space group Pna2(1), Z = 4, 4631 observed unique reflections, R = 0.048. Lattice dimensions at -70°C: a = 2972.5(3), b = 1481.9(5), c = 1305.5(1) pm. 2 consists of [Pb(15-crown-5)2]2+ ions, in which the lead ion is coordinated sandwich-like by the ten oxygen atoms of the two crown ether molecules without steric activity of the lone pair of Pb2+, of SbCl6- ions, and of molecules [SbCl3(15-crown-5)], which are already known.[In(12-crown-4)2][SbCl6]3·3CH3CN (3): Space group P1̅, Z = 2, 5530 observed unique reflections, R = 0.059. Lattice dimensions at -70°C: a = 1041.8(8), b = 1052(1), c = 1543(2) pm, α = 103.62(9)°, β=108.68(8)°, γ = 99.48(8)°. 3 consists of [In(12-crown-4)2]3+ ions, SbCl6- anions, and crystal CH3CN molecules. The In3+ ion is coordinated sandwich-like by the eight oxygen atoms of the two crown ether molecules, which are disordered in two positions

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.

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.

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.

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

Stabilisierung des reaktiven Methylcarbonat-Ions im Kronenether- Komplex [Cs(18-Krone-6)(CH3CO3)] und dessen Hydrolyseprodukt / Stabilization of the Reactive Methylcarbonate Ion in the Crown Ether Complex [Cs(18-crown-6)(CH3CO3)], and its Hydrolysis Product

2008 ◽  
Vol 63 (9) ◽  
pp. 1101-1106
Author(s):  
Adelė Jonušaite ◽  
Arnold Adam
Keyword(s):  
Crown Ether ◽  
Hydrolysis Product ◽  
Starting Material ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
Space Group ◽  
Methyl Carbonate ◽  
Hydrolysis Of ◽  
Ether Complex ◽  
Oxygen Atoms

[Cs(18-crown-6)(CH3CO3)] (1) has been obtained by the reaction of CsOCH3 with 18-crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane) in methanol in a CO2 atmosphere. The compound crystallizes in the monoclinic space group P21/n (no. 14) with a = 12.141(3), b = 8.610(1), c = 17.985(4) Å , β = 91.17(2)° and V = 1879.6(7) Å3. Cs is tenfold coordinated by six oxygen atoms of the crown ether and four oxygen atoms of two methyl carbonate anions which act as bidentate ligands. The slow hydrolysis of the methylcarbonate results in the hydrogencarbonate complex {Cs2(18-crown- 6)2 · [H2(CO3)2] · H2O · CH3OH} (2), the basic structural constitution of the starting material being retained. This new compound crystallizes in the monoclinic space group P21/c with a = 8.657 (7), b = 22.601 (2), c = 19.619 (15) Å, β = 92.09 (6)° and V = 3836.5 (6) Å3.

Sign in / Sign up

Export Citation Format

Share Document