NMR, PGSE Diffusion, and X-ray Diffraction Studies of Lithium and Potassium Salts Derived from Diphenylphosphino(o-cyanophenyl)aniline and Their Crown Ether Complexes

2005 ◽  
Vol 44 (21) ◽  
pp. 7616-7623 ◽  
Author(s):  
Ignacio Fernández ◽  
Frank Breher ◽  
Paul S. Pregosin ◽  
Zhaofu Fei ◽  
Paul J. Dyson
Keyword(s):  
Crown Ether ◽  
X Ray Diffraction ◽  
Potassium Salts ◽  
X Ray ◽  
Crown Ether Complexes

scholarly journals A structural study of alkaline earth metal complexes with hybrid disila-crown ethers

2017 ◽  
Vol 46 (27) ◽  
pp. 8727-8735 ◽  
Author(s):  
Fabian Dankert ◽  
Kirsten Reuter ◽  
Carsten Donsbach ◽  
Carsten von Hänisch
Keyword(s):  
Crown Ether ◽  
Dft Calculations ◽  
Crown Ethers ◽  
Alkaline Earth ◽  
Earth Metal ◽  
Alkaline Earth Metal ◽  
Complex Stability ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crown Ether Complexes

A series of disila-crown ether complexes have been characterized by single crystal X-ray diffraction. The complex stability of different systems were studied by DFT calculations and proton NMR experiments.

Darstellung von 1,3,5-Trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinanen; Einkristall-Röntgenstrukturanalyse eines Platin(II)-Komplexes/Preparation of 1,3,5-Trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinanes; Single Crystal X-Ray Diffraction Study of a Platinum(II)-Complex

1992 ◽  
Vol 47 (4) ◽  
pp. 517-525 ◽  
Author(s):  
Thomas G. Meyer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crown Ether ◽  
Single Crystal ◽  
Diffraction Study ◽  
Planar Geometry ◽  
Boat Conformation ◽  
Staudinger Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Synthesis ◽  
Square Planar

A new synthesis for 2-chloro-1,3,5-trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinane (1) is described. Chlorine-fluorine exchange in 1 by means of sodium fluoride in acetonitrile in the presence of catalytic amounts of a crown ether furnished 2-fluoro-1,3,5-trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinane (2). The synthesis of the bromine and iodine analogues, 3 and 4, by metathesis of 1 with the appropriate trimethylsilyl halides, Me3SiBr and Me3SiI, respectively, is also described. The syntheses of an iron(0)tetracarbonyl complex (5) and of a dichloroplatinum( II) complex (6) are reported. A single crystal X-ray diffraction study was conducted on 6. [P21/c, a = 1161.3(3), b = 1423.2(3), c = 1247.7(3) pm, β = 109.42(2)°, R = 0.028], There are deviations from ideal square planar geometry at platinum. The heterocycles display a flattened boat conformation. A Staudinger reaction of 1 with Me3SiN3 led to the formation of a substituted cyclotriphosphazene.

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.

Unexpected Structural Diversity in Alkali Metal Azide-Crown Ether Complexes: Syntheses, X-ray Structures, and Quantum-Chemical Calculations

2006 ◽  
Vol 12 (9) ◽  
pp. 2620-2629 ◽  
Author(s):  
Michael D. Brown ◽  
John M. Dyke ◽  
Francesco Ferrante ◽  
William Levason ◽  
J. Steven Ogden ◽  
...  
Keyword(s):  
Crown Ether ◽  
Alkali Metal ◽  
Quantum Chemical Calculations ◽  
Quantum Chemical ◽  
Structural Diversity ◽  
X Ray ◽  
Metal Azide ◽  
Crown Ether Complexes

Synthesis and Crystal Structure of a Caesium Hydrogen Benzoylcyanoximate Complex with 18-Crown-6: Cs(18-Crown-6){H(L)2}

1997 ◽  
Vol 52 (8) ◽  
pp. 901-905 ◽  
Author(s):  
Vera V Ponomareva ◽  
Victor V Skopenko ◽  
Konstantin V Domasevitch ◽  
Joachim Sieler ◽  
Thomas Gelbrich
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Crown Ether ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
The Mean ◽  
Cyano Groups ◽  
Oxygen Atoms

Abstract The caesium hydrogen benzoylcyanoximate (L-) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [monoclinic, space group P21/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Å, β = 90.13(1)°, V = 3434.3(9) Å, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of Cs(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}-, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O - - - O ca. 2.456(5)Å]. The caesium atom deviates by 1.492(3) Å from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical “sunrise coordination” [Cs-O (ether) 3.040(9)-3.312(7) Å]. The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (Cs-O ca. 3.040(9), 3.312(7) Å; Cs-N ca. 3.469(5), 3.679(6) Å). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism.

scholarly journals Kristallstrukturen der Tetrachloroniccolate (PPh4)2[NiCl4] und [Na-15-Krone-5]2[NiCl4] / Crystal Structures of the Tetrachloroniccolates (PPh4)2[NiCl4] and [Na- 15-Crown-5]2[NiCl4]

1990 ◽  
Vol 45 (7) ◽  
pp. 995-999 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Ulrich Müller
Keyword(s):  
Crown Ether ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Sodium Ions ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Cl Atoms

The title compounds were obtained from NiS + PPh4Cl + HCl in dichloromethane, from NiCl2 and PPh4Cl and from NiCl2 + Na2S + 15-crown-5 in acetonitrile or CH2Cl2, respectively. Their crystal structures were determined by X-ray diffraction. (PPh4)2[NiCl4]: monoclinic, space group C 2/c, Z = 4, a = 1094.9(3), b = 1946.1(4), c = 2033.5(5) pm, β = 91.48(3)°; R = 0.07 for 2895 unique observed reflexions. [Na-15-crown-5]2[NiCl4]: triclinic, space group P1̄, Z = 2, a = 987.6(1), b = 998.0(1), c = 1779.9(2) pm, α = 104.17(1), β = 95.43(1), γ = 109.95(1)°; R = 0.090 for 4155 unique observed reflexions. In both cases, the [NiCl4]2- ions have distorted tetrahedral structures. With PPh4+ as the cation the distortion corresponds to a twisted tetrahedron which fulfils the point symmetry D2, the deviation from a flattened D2d-tetrahedron being small. In (PPh4)2[NiCl4] cations and anions alternate in layers parallel to (001). In [Na-15-crown-5]2[NiCl4] two of the Cl atoms of the anion are coordinated to sodium ions; one of the crown ether molecules shows positional disorder.

Structure of Tl(18-crown-6){Cl3CC(O)N P(O)(OCH3)2}: Coordination of the Ionic Multidentate Weakens the Interaction of the Metal Atom with the Crown Ether

1999 ◽  
Vol 54 (4) ◽  
pp. 451-455 ◽  
Author(s):  
Victor A. Trush ◽  
Konstantin V. Domasevitch ◽  
Vladimir M. Amirkhanov ◽  
Joachim Sieler
Keyword(s):  
Ir Spectroscopy ◽  
Crown Ether ◽  
Metal Atom ◽  
Central Atom ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
The Mean ◽  
Oxygen Atoms

The thallium(I) dimethyl-N-trichloroacetylamidophosphate complex with a 18-crown-6 of the composition Tl(18-crown-6){L} (L = {Cl3CC(O)NP(O)(OCH3)2} -) has been prepared and characterized by means of IR spectroscopy and X-ray diffraction (orthorhombic, space group P212121 with a = 8.660( 1), b = 11.557(2), c =26.296(3) Å, Z = 4, V = 2631.8(6) Å3; R1 = 0.0285 and wR2 = 0.0558 for 4314 unique reflections). It was shown that (L-) is coordinated to the central atom in a bidentate manner via oxygen atoms of phosphoryl [Tl-O(l) 2.678(4) Å] and carbonyl groups [Tl-O(2) 3.012(6) Å.The Tl( 18-crown-6)+ moiety adopts a typical “sunrise” coordination with the metal atom laying 1.134(2) Å above the mean plane of the oxygen atoms of the macrocycle. This deviation is the highest value of the structurally examined Tl( 18- crown-6 )+ complexes. The Tl-O (etheric) separations are in the range 2.913(4) - 3.198(5) Å (av. 3.030(6) Å).

Crown Ether Complexes of Sulfonium Salts—The X-Ray Crystal Structures of[PhCOCH2SMe2·[18]Crown-6]n[PF6]n and[(PhCOCHPhSMe2)2·[18]Crown-6][PF6]2

1984 ◽  
Vol 23 (12) ◽  
pp. 977-979 ◽  
Author(s):  
Billy L. Allwood ◽  
John Crosby ◽  
David A. Pears ◽  
J. Fraser Stoddart ◽  
David J. Williams
Keyword(s):  
Crown Ether ◽  
Crystal Structures ◽  
Sulfonium Salts ◽  
X Ray ◽  
Crown Ether Complexes
Sign in / Sign up

Export Citation Format

Share Document