Acetylenkomplexe von Rhenium(+ VI). Die Kristallstrukturen von [ReCl4(n-C3H7 – C= C – n-C3H7)(POCl3)] und ReCl4(THF)2 / Alkyne Complexes of Rhenium(+VI). The Crystal Structures of [ReCl4(n-C3H7 – C= C – n-C3H7)(POCl3)] and ReCl4(THF)2

1990 ◽  
Vol 45 (9) ◽  
pp. 1227-1234 ◽  
Author(s):  
Hans-Walter Swidersky ◽  
Jürgen Pebler ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Space Group ◽  
Bond Lengths ◽  
In Trans ◽  
Alkyne Complexes ◽  
In Cis ◽  
Ray Methods

The results of the magnetic susceptibility measurements of the previously reported rhenium alkyne complexes [ReCl4(PhC≡CPh)]2.2 CH2Cl2 and [ReCl4(PhC=CPh)(CH3CN)] in the temperature range of 4.2-293 K suggest d1-configurations, corresponding with oxidation state +VI for the rhenium atoms. The new alkyne complex [ReCl4(n-C3H7–C=C–n-C3H7)(POCl3)] has been prepared by the reaction of ReCl5·OPCl3 with n-C3H7-C≡C–n-C3H7 in CCl4 solution, forming dark red single crystals, which were characterized by IR spectroscopy as well as by a crystal structure determination with X-ray methods (space group P2,/c, Z = 4, 3235 observed unique reflexions, R = 0.026; lattice dimensions at –70 °C: a = 805.6(2), b = 1000.6(4), c = 2188.8(6) pm, β = 79.59(2)°). [ReCl4(n-C3H7-C=C–n-C3H7)(POCl3)] has a molecular structure with the alkyne ligand bonded side-on (bond lengths Re-C 198.4 and 198.2(5) pm). The oxygen atom of the solvating POCl3 molecule is coordinated in trans position to the ReC2 unit of the alkyne ligand (bond length Re—O = 223.7(3) pm).In THF solutions the alkyne complexes of this type undergo a slow reaction forming ReCl4(THF)2, which was also characterized by IR spectroscopy and a crystal structure determination (space group P212121, Z = 4, 2243 observed unique reflexions, R = 0.053; lattice dimensions at –70 °C: a = 773.0(14), b = 1267.1(6), c = 1398.6(7) pm). In ReCl4(THF)2 the THF molecules coordinate in cis-position (bond lengths Re–O 208 and 212(1) pm).

Die Kristallstruktur von Tris(trimethylstannyl) acetonitril / Crystal Structure of Tris(trimethylstannyl)- acetonitrile

1997 ◽  
Vol 52 (1) ◽  
pp. 145-148 ◽  
Author(s):  
Ralf Hillwig ◽  
Klaus Harms ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Single Crystals ◽  
Structure Determination ◽  
Bond Angle ◽  
Potassium Fluoride ◽  
Crystal Structure Determination ◽  
Space Group ◽  
Bond Lengths

Single crystals of (Me3Sn)3CCN were obtained by the reaction of tris(trimethylstannyl)amine with boiling acetonitrile in the presence of potassium fluoride and trimethylarsane. The compound has been characterized by IR spectroscopy and by a crystal structure determination. Space group P21/n, Z = 4; lattice dimensions at -50 °C: a = 975.4(1), b = 1316.3(2), c = 1485.3(1), β = 98.55(1)°, R = 0.029. (Me3Sn)3CCN forms monomeric molecules with a linear CCN axis (bond angle 178.7(6)°) and bond lengths of CC = 142.1(8) pm and CN = 114.5(8) pm

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.

Cu6Br6(NPMe3)4, ein gemischt-valenter Kupfercluster / Cu6Br6(NPMe3)4, a Mixed-Valent Cluster of Copper

1994 ◽  
Vol 49 (7) ◽  
pp. 987-990 ◽  
Author(s):  
Rolf Meyer zu Köcker ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Bromine Atom ◽  
Unit Cell ◽  
Crystal Structure Determination ◽  
Space Group ◽  
Bond Lengths ◽  
Cluster Molecule

Abstract Cu6Br6(NPMe3)4 has been prepared as a by-product from the reaction of CuBr with Me3SiNPMe3 in a CH2Cl2 suspension. The dark red-violet crystals, which contain three molecules CH2Cl2 per unit cell, have been characterized by a crystal structure determination. Cu6Br6(NPMe3)4 · 3 CH2Cl2: Space group P1̅, Z = 2, lattice dimensions at -95 °C: a = 1165.2(4), b = 1168.9(4), c = 1842.9(6) pm, a = 75.61(3)°, β = 84.15(3)°, γ = 61.08(2)°, 6918 observed unique reflections, R = 0.066. In the cluster molecule Cu6Br6(NPMe3)4 the copper atoms form a nearly ideal octahedron with Cu-Cu bond lengths of 268.8 pm in average. Each of the Cu atoms is con­nected with a terminal bromine atom. Four planes of the octahedron are capped by μ3-nitrogen atoms of the (NPMe3)- groups.

Über die Reduktion von Alkinkomplexen des Molybdäns und Wolframs in hohen Oxidationsstufen. Die Kristallstruktur von MoCl3(THF)3 / On the Reduction of Alkyne Complexes of Molybdenum and Tungsten in High Oxidation States. The Crystal Structure of MoCl3(THF)3

1989 ◽  
Vol 44 (10) ◽  
pp. 1161-1166 ◽  
Author(s):  
Peter Hofacker ◽  
Claus Friebel ◽  
Kurt Dehnicke ◽  
Petra Bäuml ◽  
Wolfgang Hiller ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Oxidation States ◽  
Epr Spectra ◽  
Space Group ◽  
X Ray ◽  
High Oxidation ◽  
Oxygen Sensitive ◽  
Alkyne Complexes ◽  
Ray Methods

The reduction of the tungsten alkyne complexes [WCl4(RC≡CR)]2 (R = Ph, SiMe3) with cobaltocen in THF solutions leads to the complexes [CoCp2]2[WCl4(RC≡CR)]2 (R = Ph (1); R = SiMe3 (2)), as green, oxygen sensitive crystalline powders. Reduction of [WCl4(Me3SiC=CSiMe3)]2 and of [MoCl4(PhC=CPh)]2 with sodium naphthalide in THF solutions in the presence of 15-crown-5 gives [Na-15-crown-5]3[W2Cl9], and MoCl3(THF)3, respectively. All compounds have been characterized by IR spectroscopy, and 1 and 2, in addition, by their EPR spectra. The crystal structure of MoCl3(THF)3 was determined by X-ray methods. Space group P21/c, Z = 4, 2642 observed unique reflexions, R = 0.050. Lattice dimensions at 20 °C: a = 888.4(2), b = 1281.5(3), c = 1535.2(3) pm, β = 92.17(2)°. The compound forms monomeric octahedral molecules with a meridional arrangement of the ligands.

Synthese und Kristallstrukturen der Wolfram(VI)-Alkinkomplexe [WCl4(Ph - C≡C - I)(THF)] und [WCl4(Ph-C≡C-Te-C4H9)(THF)] / Synthesis and Crystal Structures of the Tungsten(VI) Alkyne Complexes [WCl4(Ph-C≡C-I)(THF)] and [WCl4(Ph-C≡C-Te-C4H9)(THF)]

1993 ◽  
Vol 48 (8) ◽  
pp. 1105-1111 ◽  
Author(s):  
Michael Plate ◽  
Peter Hofacker ◽  
Werner Massa ◽  
Birgit Schwarz ◽  
Bernhard Neumüller ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Oxygen Atom ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Trans Position ◽  
Space Group ◽  
Structure Determinations ◽  
In Trans ◽  
Alkyne Complexes

[WCl4(Ph-C≡C-I)(THF)] has been prepared by the reaction of trans-[WCl4(SEt2)2] with Ph - C≡C - I in THF solution, whereas [WCl4(Ph-C≡C-Te-nC4H9)(THF)] has been synthesized by the reaction of Ph-C≡C-Te-nC4H9 with tungsten hexacloride in the presence of C2Cl4 and THF. Both complexes were characterized by IR spectroscopy and by crystal structure determinations.[WCl4(Ph-C≡C-I)(THF)]: Space group P21/c, Z = 4, 2617 observed unique reflections, R = 0.064. Lattice dimensions at –70°C: a = 1518.2(3), b = 714.5(1), c = 1540.0(3) pm, β = 90.09(3)°.[WCl4(Ph-C≡C-Te–nC4H9)(THF)]. Space group P1̄, Z = 2, 3911 observed unique reflections, R = 0.067. Lattice dimensions at 20°C: a = 844.0(3), b = 974.6(4), c = 1002.4(3) pm, α = 76.00(4), β= 105.14(1), γ = 82.03(3)°.Both complexes have molecular structures, in which the tungsten atoms are seven-coordi-nate by four chlorine ligands, by the two alkyne carbon atoms, and in trans position to the latter by the oxygen atom of the THF molecule. The WC bond lengths are 198 and 200(1) in the telluro complex and 206 and 196(1) pm in the iodine derivative.

Notizen: Kristallstruktur von [MoCl2(NSN) · 2 THF]2; einem Metallaheterocyclus mit der NSN4--Einheit / Crystal Structure of [MoCl2(NSN) · 2 THF]2; a Metallaheterocycle with the NSN4- Unit

1989 ◽  
Vol 44 (10) ◽  
pp. 1325-1328 ◽  
Author(s):  
Klaus Hösler ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Bond Angle ◽  
Membered Ring ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

The chlorothionitrene complex [Cl4Mo(NSCl)]2 reacts with N,N,N′-tris(trimethylsilyl)benzamidine in THF solution to form the heterocyclic complex [MoCl2(NSN) · 2 THF]2, which contains the [NSN]4-unit. The compound is characterized by IR spectroscopy and by an X-ray structure determination (Space group P2,/c, Z = 2, 1504 observed unique reflexions, R = 0.044. Lattice dimensions at 19°C: a = 1176.0(1), b = 1108.6(4), c = 1227.3(3) pm, β = 118.25(1)°). The compound forms centrosymmetric molecules [(THF)2Cl2Mo(NSN)2MoCl2(THF)2], in which the molybdenum atoms are members of a nearly planar Mo(NSN)2Mo eight-membered ring with bond lengths MoN 180.2 and 175.2 pm; NS 157.5 and 160.6 pm; the bond angle NSN is 108.3°, corresponding to a NSN4- unit.

scholarly journals Synthese und Kristallstruktur von 2-Trimethylsilyl-1,3-bistrimethylsilylimino-1,3-dihydro-isoindol sowie die Kristallstruktur von Hexakis(trimethylsilyl)-1,4-benzdiamidin / Synthesis and Crystal Structure of 2-Trimethylsilyl-1,3-bis-trimethylsilylimino-1,3-dihydro-isoindole and the Crystal Structure of Hexakis(trimethylsilyl)-1,4-benzdiamidine

1989 ◽  
Vol 44 (5) ◽  
pp. 548-552 ◽  
Author(s):  
Frank Weller ◽  
Fritjof Schmock ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Bond Lengths

2-Trimethylsilyl-1,3-bis-trimethylsilylimino-1,3-dihydro-isoindole, C8H4N3(SiMe3)3 (2), has been prepared by the reaction of 1,2-benzodinitrile with LiN(SiMe3)2, followed by treatment with ClSiMe3. 2 forms yellow crystals, which were characterized by a crystal structure determination, as was the known hexakis(trimethylsilyl)-1,4-benzdiamidine, {[(SiMe3)2N](SiMe3N)C-C6H4-C(NSiMe3)[N(SiMe3)2]}) (1).1: space group P1, Z = 1̄,2520 observed independent reflexions, R = 0.052. Lattice dimensions (19°C): a = 662.7(1); b = 1088.3(1); c = 1417.4(2) pm; α = 76.60(1)°; β = 87.33(1)°; γ = 73.90(1)°. 1 forms monomeric centrosymmetric molecules with the amidino groups in 1,4-position of the C6H4 ring. The CN distances are 127.1(3) and 141.3(3) pm, respectively, corresponding to C=N̅-SiMe3 and C-N̅(SiMe3)2 moieties.2: space group P212121, Z = 4, 1960 observed independent reflexions, R = 0.058. Lattice dimensions (20°C): a = 643.0(1); b = 1477.4(1); c = 2414.4(2) pm. 2 forms monomeric molecules with a planar isoindole skeleton with different Si-N-bond lengths of the SiMe3 groups in 2-position (180.2(5) pm) and in 1,3-positions (171.4(5); 170.9(9) pm).

Synthese und Kristallstruktur von [TeCl2(NPMe3)2]2/ Synthesis and Crystal Structure of [TeCl2(NPMe3)2]2

1995 ◽  
Vol 50 (4) ◽  
pp. 573-576 ◽  
Author(s):  
Hella Folkerts ◽  
Kurt Dehnicke ◽  
Jörg Magull
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Acetonitrile Solution ◽  
Trans Position ◽  
Synthesis And Crystal Structure ◽  
Bond Lengths ◽  
Structure Solution ◽  
In Trans ◽  
Moisture Sensitive

[TeCl2(NPMe3)2]2 has been prepared by the reaction of TeCl4 with Me3SiNPMe3 in acetonitrile solution. Tlie compound forms white moisture sensitive crystals which have been characterized by IR spectroscopy and by a crystal structure determination. Space group P21/c, Z = 2, structure solution with 3510 independent reflections, R = 0.029. Lattice dimensions at - 70 °C; a = 1206.0(9); b = 1054.7(7); c = 1156.0(6) pm; β = 99.27(5)°. [TeCl2(NPMe3)2]2 forms centrosymmetric molecules via TeCl2Te bridges with bond lengths Te-Cl of 267.2 and 366.9 pm, the longer one being in trans-position to one of the terminally bounded (NPMe3-) groups. The TeN bond lengths of 190.1 and 192.6 pm are unusually short.

[Mn(n-Bu)(NPEt3)]4, eine manganorganische Verbindung mit Heterocuban -Struktur [Mn(n-Bu)(NPEt3)]4, an Organomanganese Compound with Heterocubane Structure

1996 ◽  
Vol 51 (3) ◽  
pp. 433-436 ◽  
Author(s):  
Hans-Joachim Mai ◽  
Bernhard Neumüller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Group 14 ◽  
Space Group ◽  
Structure Solution ◽  
Moisture Sensitive

[Mn (n- Bu)(NPEt3)]4 has been prepared by the reaction of [MnBr(NPEt3)]4 with n-butyllithium in boiling pentane. The pyrophoric compound forms red, moisture sensitive crystals, which were characterized by IR spectroscopy and by a crystal structure determination (tetragonal, space group 141/a, Z = 4, structure solution with 699 observed unique reflections, R = 0.054. Lattice dimensions at -50 °C:a = b = 2177.4(3) pm, c = 1147.1(2) pm). [Mn (n-Bu)(NPEt3)]4 forms a nearly perfect Mn4N4 hetero cubane framework with μ3-N bridges of the NPEt3- groups and σ-bonded n-butyl groups with Mn - C distances of 216.8 pm. The n-butyl groups and two of the ethyl groups are disordered.

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.

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