Die Kristallstruktur des Phosphaniminato-Komplexes [TiCl3(NPPh3)•TiCl4]2 / Crystal Structure of the Phosphorane Iminato Complex [TiCl3(NPPh3)•TiCl4]2

1996 ◽  
Vol 51 (9) ◽  
pp. 1359-1362 ◽  
Author(s):  
Frank Weller ◽  
Fritjof Schmock ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Title Compound ◽  
Titanium Tetrachloride ◽  
Bond Distance ◽  
Space Group ◽  
Yellow Orange ◽  
Centrosymmetric Dimers

The title compound was prepared from Me3SiNPPh3 and an excess of titanium tetrachloride. It forms yellow-orange crystals, which were characterized by IR spectroscopy and by crystal structure determination. Space group P21/n, Z = 2; lattice dimensions at 20°C: a = 1189.2(1), b - 1718.5(1), c = 1238.1(1) pm, β = 93.363(7)°. The compound forms centrosymmetric dimers in which the titanium atoms are triply and doubly bridged by chlorine atoms to give face- and edgesharing octahedra, respectively. In the linear units [Ti]=N =PPh3 the Ti-N bond distance of 171.6(3) pm corresponds to a double bond.

Die Kristallstruktur von [Na4(OSiPh3)4(H2O)3] / The Crystal Structure of [Na4(OSiPh3)4(H2O)3]

1996 ◽  
Vol 51 (11) ◽  
pp. 1583-1586 ◽  
Author(s):  
A. Mommertza ◽  
K. Dehnickea ◽  
J. Magull
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Single Crystals ◽  
Coordination Number ◽  
Structure Determination ◽  
Title Compound ◽  
Saturated Solution ◽  
Crystal Structure Determination ◽  
Humid Atmosphere ◽  
Space Group

Colourless single crystals of the title compound are obtained from a saturated solution of NaOSiPh3 in toluene in a humid atmosphere. We have characterized [Na4(OSiPh3)H2O)3] by IR spectroscopy and by a crystal structure determination. Space group R3, Z = 6 , R = 0.056. Lattice dimensions at -70°C: a = b = 1540.3 pm, c = 2639.6 pm. The compound has the structure of a Na4O4 heterocubane which is only slighty distorted and in which one of the sodium atoms is not hydrated and shows coordination number three.

Synthesis and Crystal Structure of [Cu2(OAc)4(NCMe)2] · 2MeCN

1998 ◽  
Vol 53 (7) ◽  
pp. 774-776 ◽  
Author(s):  
Mitra Ghassemzadeh ◽  
Kioumars Aghapoor ◽  
Bernhard Neumiiller
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Structural Data ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Centrosymmetric Dimers

T etrakis-μ-acetato-bis(acetonitrile-N )-dicopper( II) bisacetonitrile (1) was syn thesized and characterized by IR spectroscopy and by an X-ray structure determination [Space group P21/n, Z = 2, lattice dimensions at - 70 °C: a = 1064.2(1), b = 1018.4(1), c = 1088.3(1) pm, β = 101.59(1)°, R1 = 0.048]. A ccording to the structural data the blue compound consists of centrosymmetric dimers [Cu2(OAc)4(NCMe)2] and noncoordinated acetonitrile molecules.

scholarly journals Kristallstruktur von (Ph3PNH2)4[Sb6O10Cl14] · 2CH3CN / Crystal Structure of (Ph3PNH2)4[Sb6O10Cl14]-2CH3CN

1994 ◽  
Vol 49 (7) ◽  
pp. 983-986 ◽  
Author(s):  
Dieter Fenske ◽  
Ralf Garbe ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Title Compound ◽  
Crystal Structure Determination ◽  
Partial Hydrolysis ◽  
Central Unit ◽  
Space Group

Abstract The title compound has been obtained by the reaction of the phosphoraneiminato complex Cl2Sb(NPPh3) with chlorine, followed by partial hydrolysis in acetonitrile. The colourless crystals were characterized by a crystal structure determination. Space group P1̅, Z = 2, structure refine­ment with 8320 observed unique reflections, R = 0.063 with I > 2σ(I). Lattice dimensions at -70 °C: a = 1245.0(6); b = 1277.7(8), c = 1623.8(9) pm, a = 77.97(2)°, β = 86.52(2)°, γ = 67.07(2)°. The compound consists of Ph3PNH2+ ions, [Sb6O10Cl14]4-ions, in which the central unit is a Sb4O6 skeleton with a double heterocubane-like arrangement with two missing corners, and of in­ cluded acetonitrile molecules without bonding interactions.

scholarly journals Über die Reaktion von Wolframhexachlorid mit Se4N2; Kristallstruktur von PPh4[WCl5(NSeCl)] / On the Reaction of Tungsten Hexachloride with Se4N2; Crystal Structure of PPh4[WCl5(NSeCl)]

1991 ◽  
Vol 46 (12) ◽  
pp. 1625-1628 ◽  
Author(s):  
Stefan Vogler ◽  
Werner Massa ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Structure Determination ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Tetraphenylphosphonium Chloride ◽  
Tungsten Hexachloride

The reaction of tungsten hexachloride with Se4N2 leads to [WCl4(NSeCl)]2, which reacts with pyridine to form [WCl4(NSeCl)Py], and with tetraphenylphosphonium chloride to form PPh4[WCl5(NSeCl)], which was characterized by an X-ray structure determination. Space group P21, Z = 2, 1657 observed unique reflections, R = 0.074, wR = 0.061. Lattice dimensions at —80 C: a = 710.7(1), b = 2217.9(4), c = 953.6(2) pm; β = 111.93(3) . The [WCl5(NSeCl)]- ion possesses an almost linear WNSe group with bond lengths WN = 188 pm, corresponding to a double bond, and NSe = 200 pm.

Crystal structure of (Z)-Cembr-4-ene-15,19,20-triol

1977 ◽  
Vol 30 (12) ◽  
pp. 2723 ◽  
Author(s):  
EN Maslen ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Single Crystal ◽  
Least Squares ◽  
Structure Determination ◽  
Title Compound ◽  
X Ray Diffraction ◽  
Relative Configuration ◽  
Macrocyclic Ring ◽  
X Ray

The crystal structure of the title compound, CZOH3803 [compound (1) in ref.'], has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.045 for 954 'observed' reflections. Crystals are monoclinic, P2', a 9.281(2), b 17.798(6), c 6.417(1) A, B 93.81(3)", Z 2. The structure determination establishes the relative configuration of the chiral centres within the 14-membered macrocyclic ring and shows the double bond to have the unusual (Z) configuration.

scholarly journals (E)-4-[(1-Benzyl-4-benzylidene-2,5-dioxopyrrolidin-3-yl)methyl]benzaldehyde 0.25-hydrate

2012 ◽  
Vol 68 (4) ◽  
pp. o1184-o1184 ◽  
Author(s):  
Tao Yu ◽  
Yimin Hu
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Title Compound ◽  
Crystal Packing ◽  
Membered Ring ◽  
Dihedral Angles ◽  
Inversion Center ◽  
Space Group ◽  
Compound C ◽  
Centrosymmetric Dimers

The crystal structure of the title compound, C26H21NO3·0.25H2O, reveals one stereogenic centre in the molecule. Nevertheless, due to the observed centrosymmetric space group, both enantiomers are present in the crystal packing. The water molecule of crystallisation is located on a crystallographic inversion center. The molecule contains one five-membered ring (A) and three six-membered rings (benzyl ringB, benzylidene ringCand formylbenzyl ringD). All four rings are not coplanar: the dihedral angles between ringsAandB,AandC, andAandDare 70.35 (9), 33.8 (1) and 60.30 (9)°, respectively. In the crystal, pairs of weak C—H...O interactions lead to the formation of centrosymmetric dimers. Additional C—H...O interactions link the dimers into chains along [011].

N-TrimethylsilyMminotriphenylphosphoran-Kupfer(II)-chlorid, [Me3 SiNPPh3 · CuCl 2 ]2 Synthese und Kristallstruktur / N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, [Me3 SiNPPh3 · CuCl 2] 2 Synthesis and Crystal Structure

1988 ◽  
Vol 43 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Dieter Fenske ◽  
Eberhard Böhm ◽  
Kurt Dehnicke ◽  
Joachim Strähle
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Title Compound ◽  
Unit Cell ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Bond Lengths ◽  
Moisture Sensitive

Abstract The title compound has been prepared by the reaction of N-trimethylsilyl-iminotriphenylphos-phorane with copper(II) chloride in boiling CCl4 /C2H5OH, and forms moisture sensitive crystals, which are green in transmittance and black in reflexion. [Me3SiNPPh3 · CuCl2 ] 2 was characterized by its IR spectrum as well as by a crystal structure determination (4197 observed, independent reflexions, R = 0.049). The lattice dimensions are at 20 °C: a = 1102.7. b = 1407.3. c = 1560.2 pm; β = 94.27°; space group P21/n with two formula units in the unit cell. The complex consists of centrosymmetric, dimeric molecules with a planar Cu2 Cl2 ring (Cu-CI bond lengths 229 and 231 pm). A terminally bonded CI atom (Cu-CI = 221 pm) and the N atom of the Me3SiNPPh3 ligand (Cu-N = 198.5 pm) complete the coordination number four of the nearly planar surroundings of the Cu atoms.

Die Kristallstruktur von [Na(12-Krone-4)2+]2Se82- · (Se6, Se7) / The Crystal Structure of [Na(12-Crown-4)2+]2Se82- · (Se6, Se7)

1991 ◽  
Vol 46 (10) ◽  
pp. 1287-1292 ◽  
Author(s):  
Rüdiger Staffel ◽  
Ulrich Müller ◽  
Andreas Ahle ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Title Compound ◽  
Crystal Structure Determination ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure

The title compound was prepared from sodium polyselenide and 12-crown-4 in DMF solution in the presence of cerium(III)chloride in the form of black needles. The crystal structure determination by X-ray diffraction shows a partially disordered structure, in which the anionic units Se82- · Se7 and Se82- · Se6 are present in the ratio 0.72/0.28. These units are associated to layers parallel to (100); the layers alternate with pseudohexagonal layers of [Na(12-crown-4)2]+ ions. Space group P1̅, Z = 2, 3903 observed unique reflections, R = 0.114, wR= 0.084. Lattice dimensions at -65°C: a = 1247.9(3), b = 1367.8(8), c = 1660(1) pm, α = 94.65(5), β = 98.94(3), γ = 91.10(3)°.

Notizen: Synthese und Kristallstruktur von [OsCl4(CH3CN)2] · 1/2 CH3CN / Synthesis and Crystal Structure of [OsCl4(CH3CN)2] · 1/2CH3CN

1990 ◽  
Vol 45 (8) ◽  
pp. 1210-1212 ◽  
Author(s):  
Dieter Fenske ◽  
Gerhard Baum ◽  
Hans-Walter Swidersky ◽  
Kurt Dehnicke
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Room Temperature ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Slow Reaction ◽  
Moisture Sensitive

[OsCl4(CH3CN)2] · 1/2CH3CN has been prepared by the reaction of OsCl5 with acetonitrile in a slow reaction at room temperature, forming red, moisture sensitive crystals. The compound was characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1281 observed unique reflexions, R = 0.031. Lattice dimensions at 20 °C: a = 1032.5(5), b = 1356.0(7), c = 975.9(5) pm. The complex has a molecular structure, in which the osmium atom is octahedrally coordinated by four chlorine atoms and by two N-atoms of the ciscoordinated acetonitrile molecules. The included CH3CN molecules are disordered in two positions.

Notizen: Kristallstruktur von 1,1-Dichlor-3,5-diphenyl-4-H-1,2,4,6-λ4-selenatriazin, SeCl2C2N3H(C6H5)2 / Crystal Structure of 1,1-Dichloro-3,5-diphenyl-4-H-1,2,4,6-λ4-selenatriazine, SeCl2C2N3H(C6H5)2

1989 ◽  
Vol 44 (7) ◽  
pp. 857-859 ◽  
Author(s):  
Dieter Fenske ◽  
Christina Ergezinger ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Title Compound ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

The title compound has been prepared as a byproduct of the reaction of Se2Cl2 with Ν,Ν,N′-Tris(trimethylsilyl)benzamidine in CH2Cl2 solution. [SeCl2(HNC2N2Ph2)]2 was characterized by an X-ray structure determination. Space group P21/n, Z = 2, 2979 observed independent reflexions, R = 0.032. Lattice dimensions (-65 °C): a = 1050.1(4), b = 1018.9(4), c = 1402.1(6) pm; β = 99.78(3)°. The compound forms centrosymmetric dimeric molecules with SeCl2Se bridges (bond lengths 241.6(1) and 339.3(1) pm), the selenium atoms being members of nearly planar [xxx] selenatriazine rings with Se—N bond lengths of 182.2(2) and 181.5(2) pm.

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