scholarly journals Die Kristallstrukturen der Dysprosium-Komplexe [DyCl3(DME)2] und [DyCl2(THF)5]+[DyCl4(THF)2]- / Crystal Structures of the Dysprosium Complexes [DyCl3(DME)2] and [DyCl2(THF)5]+[DyCl4(THF)2]-

1996 ◽  
Vol 51 (4) ◽  
pp. 531-535 ◽  
Author(s):  
Stefan Anfang ◽  
Kurt Dehnicke ◽  
Jörg Magull
Keyword(s):  
Molecular Structure ◽  
Crystal Structures ◽  
Chlorine Atom ◽  
Octahedral Geometry ◽  
Space Group ◽  
Structure Determinations ◽  
Bipyramidal Structure ◽  
Chloride Ligands ◽  
Oxygen Atoms

Abstract [DyCl3(DME)2] (DME = 1,2-dimethoxyethane) has been prepared from the known tetrahy-drofuran complex [Dy2Cl6(THF)7] in boiling DME. Both complexes were characterized by structure determinations. [DyCl3(DME)2]: Space group P21/c, Z = 4, lattice dimensions at -70 °C: a = 1141.9(6), b = 884.2(4), c = 1558.3(6) pm, β = 104.83(4)°. The complex has a molecular structure with a distorted pentagonal bipyramidal geometry in which the oxygen atoms of the chelating DME molecules and one chlorine atom occupy the pentagonal plane. [DyCl2(THF)5]+[DyCl4(THF)2]-: Space group C2/c, Z = 4, lattice dimensions at -70 °C: a -1241.4(9), b = 1139.4(6), c = 2735.1(19) pm, β = 91.19(4)°. The complex contains a seven-coordinate cation with axial chloride ligands in a pentagonal bipyramidal structure and a six-coordinate anion with a trans octahedral geometry.

Die Reaktionen von Wolframhexachlorid mit überschüssigem 2,2-Dimethylpropylidinphosphan; die Kristallstrukturen von WCl5P2(C5H9)3, WCl4P5(C5H9)5 und [C3(C4H9)3]+[WCl5(C4H9C≡CC4H9)]- / The Reactions of Tungsten Hexachloride with Excess 2,2-Dimethylpropylidynephosphane; the Crystal Structures of WCl5P2(C5H9)3, WCl4P5(C5H9)5, and [C3(C4H9)3]+[WCl5(C4H9C=CC4H9)]⁻

1991 ◽  
Vol 46 (4) ◽  
pp. 519-529 ◽  
Author(s):  
Frank Weller ◽  
Irene Pauls ◽  
Kurt Dehnicke ◽  
Gerd Becker
Keyword(s):  
Molecular Structure ◽  
Crystal Structures ◽  
Phosphorus Atom ◽  
Type Structure ◽  
Tungsten Atom ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Tungsten Hexachloride

The reaction of tungsten hexachloride with excess 2,2-dimethylpropylidynephosphane, C4H9—C≡P, leads to the tungsten phosphaalkyne clusters WCl5P2(C5H9)3 and WCl4P5(C5H9)5, as well as to the tris(t-butyl)cyclopropenium pentachloro tungsten alkyne complex [C3(C4H9)3]+[WCl5(C4H9C≡CC4H9)]-. All complexes were characterized by X-ray structure determinations.WCl5P2(C5H9)3: Space group P2,/n, Z = 8,4653 observed unique reflexions, R = 0.033. Lattice dimensions at 20 °C: a = 1577.8(2), b = 1661.3(1), c = 1869.8(2) pm, β = 110.64(1)°. The compound has a molecular structure, in which the tungsten atom is surrounded by three chlorine atoms, three carbon atoms with W—C distances of 182, 230, and 231 pm, and by one phosphorus atom with W—P = 246 pm.WCl4P5(C5H9)5: Space group P21/c, Z = 4, 3517 observed unique reflexions, R = 0.043. Lattice dimensions at 20 °C: a = 1770.0(2), b = 1032.9(2), c = 1876.0(3) pm, β = 102.86(1)°. The complex has a molecular structure, in which the tungsten atom is surrounded by two chlorine atoms, two carbon atoms with W—C distances of 189 and 215 pm, as well as by four phosphorus atoms with W — P distances of 242, 250, 264, and 268 pm.[C3(C4H9)3]+[WCl5(C4H9C=CC4H9)] : Space group P21/c, Ζ = 4, 3284 observed unique reflexions, R = 0.052. Lattice dimensions at 20 °C: a = 941.5(3), b = 1762.2(6), c = 1903.5(7) pm, β = 92.27(3)°. The compound consists of tris(t-butyl)cyclopropenium ions, and anions [WCl5(C4H9C=CC4H9)]⁻, in which the bis(t-butyl)alkyne ligand is coordinated side-on, corresponding to a cyclopropene type structure with W—C distances of 198 pm.

[Na-15-Krone-5]2[ZrF2Cl4] und (PPh4)2[ZrCl6] · 2 CH2Cl2; Synthesen, IR-Spektren und Kristallstrukturen / [Na-15-Crown-5]2[ZrF2Cl4] and (PPh4)2[ZrCl6] · 2 CH2Cl2; Syntheses, IR Spectra, and Crystal Structures

1989 ◽  
Vol 44 (10) ◽  
pp. 1155-1160 ◽  
Author(s):  
Eva Hartmann ◽  
Kurt Dehnicke ◽  
Dieter Fenske ◽  
Helmut Goesmann ◽  
Gerhard Baum
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Ir Spectra ◽  
Crystal Structures ◽  
Chlorine Atom ◽  
Sodium Fluoride ◽  
Sodium Ions ◽  
Ionic Structure ◽  
Space Group ◽  
Structure Determinations

[Na-15-crown-5]2[ZrF2Cl4] has been prepared by the reaction of the amidinato complex [Ph—C(NSiMe3)2ZrCl3]2 with sodium fluoride in acetonitrile suspension, as well as by the reaction of ZrCl4 in acetonitrile, both in the presence of 15-crown-5. On an analogous route (PPh4)2[ZrCl6] · 2 CH2Cl2 has been prepared by the reaction of [Ph—C(NSiMe3)2ZrCl3]2 with PPh4Cl in CH2Cl2 solution, as well as by the reaction of ZrCl4 with PPh4Cl in CH2Cl2. The compounds are characterized by their IR spectra and by crystal structure determinations.[Na-15-crown-5]2[ZrF2Cl4]: Space group Ρ21/a, Z = 4, 6589 observed independent reflexions, R = 0.069. Lattice dimensions at 20°C: a = 1705.0(9), b = 1092.4(6), c = 1906.5(10) pm, β = 113.14(3)°. [Na-15-crown-5]2[ZrF2Cl4] forms ion triples, in which both sodium ions are sevencoordinate by five oxygen atoms of the crown ether molecules, as well as by a fluorine and a chlorine atom of the cis-[ZrF2Cl4]2- unit.(PPh4)2[ZrCl6] · 2 CH2Cl2: Space group P1̄, Z = 1, 4831 observed independent reflexions, R = 0.041. Lattice dimensions at 20°C: a = 1030.1(5), b = 1124.8(6), c = 1245.6(6) pm, α = 70.81(3), β = 80.61(4), γ = 80.39(4)°. The compound has an ionic structure with ZrCl62- ions of symmetry Ci.

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.

Synthese, FIR-Spektren und Kristallstrukturen der Pentaselenide K2Se5 und [Na(15-Krone-5)]2Se5 / Syntheses, FIR Spectra, and Crystal Structures of the Pentaselenides K2Se5 and [Na(15-crown-5)]2Se5

1992 ◽  
Vol 47 (2) ◽  
pp. 205-210 ◽  
Author(s):  
Volker Müller ◽  
Gerlinde Frenzen ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crown Ether ◽  
Crystal Structures ◽  
Type Structure ◽  
Sodium Ions ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
R Value ◽  
Fir Spectra ◽  
Oxygen Atoms

K2Se5 has been prepared by crystallization from a potassium polyselenide solution in DMF. In a similar way [Na(15-crown-5)]2Se5 can be prepared by crystallization from a sodium polyselenide solution in DMF in the presence of 15-crown-5. Both compounds were characterized by FIR spectroscopy as well as by X-ray structure determinations. K2Se5: Space group P 212121, Z = 4, 1659 observed independent reflections, R = 0.061. Lattice dimensions at - 90 °C; a = 671.5(5), b = 694.9(5), c = 1776.4(9) pm. The compound crystallizes with the K2S5 type structure. [Na(15-crown-5)]2Se5: Space group P 1̄, Z = 2, 3026 observed indenpendent reflections, R = 0.140. Lattice dimensions at -100 °C: a = 853.7(5), b = 1042.8(10), c = 2011.0(10) pm; α = 88.95(5)°, β = 79.42(5)°, γ = 66.15(5)°. The compound forms an ion triple, in which the sodium ions are coordinated by the five oxygen atoms of the crown ether molecules as well as by the terminal selenium atoms of the pentaselenide chain. The rather high R value is a result of the disordered crown ether molecules.

Crystal and molecular structure of di-o-anisylketone

1985 ◽  
Vol 63 (12) ◽  
pp. 3374-3377 ◽  
Author(s):  
C. Faerman ◽  
S. C. Nyburg ◽  
G. Punte ◽  
B. E. Rivero ◽  
A. A. Vitale ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Compound C ◽  
Twist Conformation ◽  
Oxygen Atoms

The crystal and molecular structure of the title compound, C15H14O3, is described. Crystals are monoclinic, space group P21/n, a = 9.893(5), b = 10.719(5), c = 12.136(3) Å, β = 90.56(3)°. The molecule has a twist conformation and interactions between oxygen atoms of the methoxyl groups are thought to play some part in this.

μ2-Halogenokomplexe von N-Bromsuccinimid und N-Bromphthalimid. Die Kristallstrukturen von PPh4[X(N-Bromsuccinimid)2] und von PPh4[X(N-Bromphthalimid)2] mit X = CI und Br / μ2-Halogeno Complexes of N-Bromosuccinimide and N-Bromophthalimide. The Crystal Structures of PPh4 [X(N-Bromosuccinimide)2] and PPh4 [X(N-Brom ophthalimide)2] with X = Cl and Br

1994 ◽  
Vol 49 (5) ◽  
pp. 593-601 ◽  
Author(s):  
Mitra Ghassemzadeh ◽  
Klaus Harms ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crystal Structures ◽  
Yellow Crystal ◽  
Halide Ions ◽  
Space Group ◽  
Bond Angles ◽  
Structure Solution ◽  
Structure Determinations ◽  
Acetonitrile Solutions

The μ2-halogeno complexes PPh4[X(N-bromosuccinimide)2] and PPh4[X(N-bromophthali- mide)2] with X = Cl and Br have been prepared by reactions of N-bromosuccinimide and N-bromophthalimide, respectively, with the corresponding tetraphenylphosphonium halides PPh4X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determinations. PPh4[Cl(N-Bromosuccinimide)2] (1): Space group P21/n, Z = 4, structure solution with 2516 observed unique reflections, R = 0.040. Lattice dimensions at -25 °C: a = 1775.9(1), b = 764.3(1), c = 2341.7(2) pm, β = 101.84(1)°. PPh4[Br(N-Bromosuccinimide)2] (2): Space group P21/n, Z = 4, structure solution with 5620 observed unique reflections, R = 0.061. Lattice dimensions at 20 °C: a = 1776.9(9), b = 762.2(3), c = 2331(1) pm, β = 103.02(3)°. PPh4[Cl(N-Bromophthalimide)2] (3): Space group P1̅, Z = 4, structure solution with 3812 observed unique reflections, R = 0.039. Lattice dimensions at -50 °C: a = 918.5(2), b = 1115.0(3), c = 2584.4(5) pm, α = 88.22(3)°, β = 83.20(3)°, γ = 85.10(3)°. PPh4[Br(N-Bromophthalimide)2] (4): Space group P1̅, Z = 2, structure solution with 3413 observed unique reflections, R = 0.044. Lattice dimensions at -50 °C: a = 1120.2(2), b = 1308.6(3), c = 1343.2(3) pm, α = 105.10(3)°, β = 104.16(3)°, γ = 92.99(3)°. The structures of 1-4 consist of PPh4+ ions, anions [X(N-bromosuccinimide)2]- and [X(N-bromophthalimide)2]-, respectively, in which the halide ions X- are coordinated by the bromine atoms of N-bromosuccinimide and N-bromophthalimide molecules, respectively. The bond angles Br···X···Br are 86.48(5)° for 1, 85.1(1)° for 2, 102.31(6)° and 93.61(6)° for 3, and 91.86(4)° for 4. The bond angles N-Br···X are nearly linear.

Kristallstrukturen der iodierten closo-Hexaborate trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P)2[B6H2I4] · 2 CH3CN und (CH2Py2)[B6HI5]/Crystal Structures of the Iodized closo-Hexaborates trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P )2[B6H2I4] · 2 CH3CN and (CH2Py2)[B6HI5]

1998 ◽  
Vol 53 (2) ◽  
pp. 206-210 ◽  
Author(s):  
D. Sonnak ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

Abstract X-ray structure determinations have been performed on single crystals of trans-(Ph4P)2-[B6H4I2] (1) (triclinic, space group P1̄, a = 9.9680(12), b = 10.9690(11), c = 11.0470(14) Å,α = 88.167(9), β = 80.466(12), γ = 68.839(11)°, Z = 1), mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2 (2)(triclinic, space group P1̄, a = 11.8694(11), b = 15.1699(13), c = 17.051(2) Å, α = 75.118(9), β = 71.953(10), γ = 69.331(8)°, Z = 2), trans-(Ph4P )2[B6H2I4] · 2 CH3CN (3) (monoclinic, space group P21/n, a = 14.9665(10), b = 7.6783(10), c = 23.385(3) Å, β = 95.78(9)°, Z = 2), and (CH2Py2)[B6HI5] (4) (orthorhombic, space group Pnma, a = 13.660(2), b = 11.8711(13), c = 13.839(2) Å, Z = 4). The B6 octahedra are compressed in the direction of the B-I bonds, resulting in shortened diagonal B ··· B distances with average values of the groups I-B ··· B-I = 2.37 and I-B ··· B-H = 2.43 Å as compared with H-B ··· B-H = 2.49 Å.

Crystal and Molecular Structure of Difluorochlorine(III)-hexafluoroarsenate(V), ClF2AsF6

1971 ◽  
Vol 49 (15) ◽  
pp. 2539-2543 ◽  
Author(s):  
H. Lynton ◽  
J. Passmore
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Chlorine Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Arsenic Atom ◽  
Space Group

Crystals of difluorochlorine(III)hexafluoroarsenate(V), ClF2AsF6, are monoclinic, space group A2/a, a = 10.676(9), b = 7.673(7), c = 8.064(7) Å, β = 113.40(5)°. The structure was refined by three dimensional least squares methods to R = 0.045 for 185 independent observed reflections. The chlorine atom has two nearest fluorine neighbors at 1.541(14) Å, with a F—Cl—F angle of 103.17(0.70)°, and two longer fluorine bonds at 2.339(14) Å. All five atoms lie in a plane. The arsenic atom is octahedrally coordinated to six fluorine atoms and is connected to two ClF2+ groups via trans fluorine bridges.

Crystal Structures of the Selenate Alums CsM[SeO4]2.12H2O (M = Al, Cr, Fe, Rh or In)

1990 ◽  
Vol 43 (2) ◽  
pp. 393 ◽  
Author(s):  
RS Armstrong ◽  
JK Beattie ◽  
SP Best ◽  
GP Braithwaite ◽  
P Delfavero ◽  
...  
Keyword(s):  
Bond Length ◽  
Crystal Structures ◽  
Structural Class ◽  
Cubic Crystals ◽  
Space Group ◽  
Structure Determinations

Structure determinations ofthe alums CsM[SeO4]2.12H2O have been carried out for M =aluminium(III), chromium(III), iron(III), rhodium(III) and indium(III). Structures of the cubic crystals, space group Pa3, were determined at 295(1) K. For Al, Cr, Fe, Rh and In, respectively, crystals with a = 12.544(3), 12.575(3), 12.615(5), 12.532(7) and 12.694(6)Ǻ gave 568, 561, 556, 566 and 269 independent reflections which refined to R = 0.040, 0.041, 0.051, 0.031 and 0.027. The compounds belong to the α alum structural class, in contrast to the caesium sulfate alums of aluminium, chromium, iron and indium, which have the β alum structure. This difference between the α and β alum structures does not affect the MIII-O bond length.

Crystal and Molecular Structure of 1,11-bis(Tropolone)-3,6,9-trioxaundecane · RbI

1980 ◽  
Vol 35 (12) ◽  
pp. 1533-1537 ◽  
Author(s):  
K. K. Chacko ◽  
W. Saenger
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Type Structure ◽  
The Other ◽  
Space Group ◽  
X Ray ◽  
Circular Structure ◽  
Cell Dimensions ◽  
Oxygen Atoms

Abstract The complex between the polyether ligand 1,11-bis(tropolone)-3,6,9-trioxaundecane and RbI crystallizes in space group P21/c with cell dimensions a = 11.383(4), b = 14.493(5), c = 16.122(6) Å and β = 111.02(5)° with Z = 4. The structure was solved on the basis of 3734 X-ray reflections measured on a diffractometer with CuKα-radiation and refined to an R of 0.101. The polyether wraps around the Rb+ in a circular structure. One of the tropolone rings is elevated in order to avoid collision. Rb+ is located 1.224(6) Å above the plane formed by five oxygen atoms of the ligand, it is coordinated to I -(3.666(2)Å) and to all oxygens. The Rb+ ··· O distances of the least electronegative “ester oxygens”, 3.14(1) Å and 3.18(1) Å are significantly longer compared to the other Rb+···O distances in the range 2.81(1) Å to 3.08(1) Å. The conformation about the C-C and C-O bonds of the ligand are gauche and trans as generally found in such molecules. The two tropolone seven-membered rings are slightly non-planar and display an envelope-type structure.

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