Synthese und Kristallstruktur des Phosphaniminatokomplexes [MoCl4(NPPh3)(Pyridin)] · CH2Cl2/ Synthesis and Crystal Structure of the Phosphaneiminato Complex [MoCl4(NPPh3)(pyridine)] · CH2Cl2

1987 ◽  
Vol 42 (8) ◽  
pp. 947-950 ◽  
Author(s):  
Karin Völp ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Pyridine Molecule ◽  
Trans Position ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Bond Lengths ◽  
Cell Dimensions ◽  
In Trans ◽  
Moisture Sensitive

Abstract[MoCl4(NPPh3)(pyridine)] · CH2Cl2 is formed by the reaction of the cyclothiazeno complex [MoCl3(N3S2) · (pyridine)] with triphenylphosphane in CH2Cl2 solution. It forms red, moisture sensitive needles. [MoCl4(NPPh3)(C5H5N)] · CH2Cl2 crystallizes monoclinically in the space group P21/n with four formula units per unit cell (1934 independent observed reflexions. R = 0.057). The cell dimensions are a = 1165, b = 1473, c = 1696 pm; β = 107.82°. The Mo atom is coordinated by four chlorine atoms, by the N atom of the (NPPh3-) ligand, and in trans-position to it by the N atom of the pyridine molecule. The Mo= N = PPh3 group has a nearly linear MoNP axis (176.6°) with bond lengths of MoN = 172 pm and PN = 165 pm.

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.

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.

scholarly journals ReNF4 · ReF5(NCl), ein Nitrido-Nitrenokomplex von Rhenium(VII)/ ReNF4 · ReF5(NCl), a Nitrido Nitrene Complex of Rhenium (VII)

1984 ◽  
Vol 39 (8) ◽  
pp. 1114-1117 ◽  
Author(s):  
Willi Kafitz ◽  
Kurt Dehnicke ◽  
Eberhard Schweda ◽  
Joachim Strähle
Keyword(s):  
Ir Spectrum ◽  
Fluorine Atom ◽  
Structural Investigation ◽  
Unit Cell ◽  
Trans Position ◽  
X Ray ◽  
Bond Lengths ◽  
Direct Fluorination ◽  
Cell Dimensions ◽  
In Trans

AbstractReNF4 · ReF5(NCl) is prepared by direct fluorination of ReNCl4 with fluorine between 80 °C and 130 °C. The red crystals are extremely sensitive to moisture. The complex is characterized by the IR spectrum and by an X-ray structural investigation. ReNF4 · ReF5(NCl) crystallizes orthorhombically in the space group Pnma with 4 formula units per unit cell and with the cell dimensions a = 1440, b = 848, c = 776 pm (419 observed, independent reflexions, R = 13.9%). The complex consists of the molecules ReNF4 and ReF5(NCl), which are linked by a linear asymmetric fluorine bridge. The bridging fluorine atom is in trans-position to the nitrido ligand Re -F - 228 pm) and to the nitreno ligand (Re -F = 159 pm and Re= N - Cl 164 pm) correspond to triple 188 pm). The Re ≡ N bond lengths Re= N bonds.

Synthesis and crystal structure of Na3.5Cr1.5Co0.5(PO4)3 phosphate

2006 ◽  
Vol 21 (3) ◽  
pp. 210-213 ◽  
Author(s):  
Mohamed Chakir ◽  
Abdelaziz El Jazouli ◽  
Jean-Pierre Chaminade
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Hexagonal Unit Cell ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

A new Nasicon phosphates series [Na3+xCr2−xCox(PO4)3(0⩽x⩽1)] was synthesized by a coprecipitation method and structurally characterized by powder X-ray diffraction. The selected compound Na3.5Cr1.5Co0.5(PO4)3 (x=0.5) crystallizes in the R3c space group with the following hexagonal unit-cell dimensions: ah=8.7285(3) Å, ch=21.580(2) Å, V=1423.8(1) Å3, and Z=6. This three-dimensional framework is built of PO4 tetrahedra and Cr∕CoO6 octahedra sharing corners. Na atoms occupy totally M(1) sites and partially M(2) sites.

Oxotetrafluoro-vanadate(V): Die Kristallstruktur von [enH2] [VOF4(H2O)]2.

1976 ◽  
Vol 31 (5) ◽  
pp. 541-543 ◽  
Author(s):  
Helmut Rieskamp ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Space Group ◽  
X Ray ◽  
In Trans ◽  
Oxygen Atoms

The crystal structure of [enH2][VOF4(H2O)]2 has been determined from X-ray diffractometer data. Crystals are monoclinic, space group C2/c with Z = 4 in a unit cell of dimensions a = 16.576(13), b = 7.781(4), c = 10.338(8) Å, β = 120.0(1)°.The structure was refined by least-squares methods to R 0.053 for 1436 reflections. The structure contains monomeric [VOF4(H2O)]⁻-ions with the oxygen atoms in trans position. The bond distances are 1.577 Å (terminal oxygen) and 2.333 Å (H2O molecule), resp. The V–F distances vary between 1.769(2) and 1.858(2) Å for fluorine atoms involved in strong hydrogen bonds.

Synthese und Kristallstruktur des Imidokomplexes {TaCl4NC(Ph)[N(SiMe3)2]}2 · 2 CH2Cl2 / Synthesis and Crystal Structure of the Imido Complex {TaCl4NC(Ph)[N(SiMe3)2]}2 · 2 CH2Cl2

1989 ◽  
Vol 44 (9) ◽  
pp. 1003-1006 ◽  
Author(s):  
Kurt Merzweiler ◽  
Dieter Fenske ◽  
Eva Hartmann ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Title Compound ◽  
Bond Angle ◽  
Trans Position ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Bond Lengths ◽  
In Trans ◽  
Complex Forms

The title compound has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)benzamidine with tantalum pentachloride in CH2Cl2 suspension, forming amber-coloured, moisturesensitive crystals, which were characterized by an X-ray structure determination. Space group P 21/n, Z = 2, 4895 observed independent reflexions, R = 0.059. Lattice dimensions (-65°C): a = 1165.2(6), b = 1335.4(6), c = 1629.0(7) pm, β = 93.23(4)°. The complex forms centrosymmetric molecules dimerized via chloro bridges TaCl2Ta with TaCl bond lengths of 247.2(2) and 277.1(2) pm, the longer one being in trans-position to the imido group, which can be formulatedas [xxx] (bond lengths Ta=Ν = 183.5(8), C=N = 134(1) pm, bond angle TaNC = 162.7(7)°).

scholarly journals Synthese und Kristallstruktur des dreikernigen μ-Nitridokomplexes (PPh4)2[W3N2Cl14] · CCl4 · CH2Cl2/ Synthesis and Crystal Structure of the Trinuclear μ-Nitrido Complex (PPh4)2[W3N2Cl14] · CCl4 · CH2Cl2

1985 ◽  
Vol 40 (8) ◽  
pp. 1005-1009 ◽  
Author(s):  
Thomas Godemeyer ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Trans Position ◽  
X Ray Diffraction ◽  
Tungsten Atom ◽  
Synthesis And Crystal Structure ◽  
Mean Values ◽  
X Ray ◽  
Bond Lengths ◽  
Cell Dimensions ◽  
In Trans ◽  
Single Bonds

AbstractThe title compound results from a slow reaction between two m oles of PPh4[W2NCl10], dissolved in dichlorom ethane, upon addition of carbon tetrachloride. The red crystals are characterized by X-ray diffraction. (PPh4)2[W3N2Cl14] · CCl4 · CH2Cl2 crystallizes triclinically in the space group P1̄ with two formula units per unit cell. The cell dimensions at -100 °C are: a = 1430, b = 1462, c = 1655 pm , α = 74.6°, β = 79.0°, γ = 82.4° (10,908 independent, observed reflexions, R = 0.078). The structure consists of PPh4⊕ ions, trinuclear finitrido anions [W3N2Cl14]2⊝ and enclosed molecules of CCl4 and CH2Cl2. The tungsten atom s of the anion are linked by almost linear nitrido bridges (~176°) with different WN bond lengths (mean values 184 pm and 207 pm ), corresponding to double and single bonds. The equatorial WCl4 groups are in eclipsed conformation; the two chlorine atoms in trans-position to the nitrido groups have mean bond lengths of 240 pm which is 9 pm longer than the equatorial W -Cl bonds. The IR spectrum is reported.

Synthese und Kristallstruktur von MoCl4(DME) · 15-Krone-5 und MoCl4(DME) (DME = 1,2-Dimethoxyethan) / Synthesis and Crystal Structure of MoCl4(DME) · 15-Crown-5 and MoCl4(DME) (DME = 1,2-Dimethoxyethane)

1991 ◽  
Vol 46 (3) ◽  
pp. 307-314 ◽  
Author(s):  
Evamarie Hey-Hawkins ◽  
Hans Georg von Schnering
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Work Up

NaSi reacts with MoCl5 and 15-crown-5 in toluene with reduction of Mo(V) to Mo(IV). Work-up in DME yields MoCl4(DME)· 15-crown-5 (1). MoCl4(DME) (2) is prepared more conveniently from MoCl5/DME. 1 and 2 were characterized spectroscopically and by X-ray structure determination. Crystal data: 1, space group P212121 (No. 19), Z = 4, 2765 observed independent reflexions, R = 0.026, cell dimensions (110 K): a = 16.292(4), b = 12.884(3), c = 10.452(2) Å. 2, space group I4̄2d (No. 122), Z = 8, 558 observed independent reflexions, R = 0.037, cell dimensions (292 K): a = b = 9.562(2), c = 23.777(6)Å. The MoCl4(DME) molecule of 1 and 2 forms a distorted octahedron. There are four non-coordinating 15-crown-5 molecules present in the unit cell of 1. The UV/VIS spectrum and the magnetic properties of 2 are discussed.

Phosphaniminatokomplexe von Molybdän(V). Die Kristallstruktur von [MoCl4(NPPh3)]2 / Phosphaneiminato Complexes of Molybdenum(V). The Crystal Structure of [MoCl4(NPPh3)]2

1987 ◽  
Vol 42 (12) ◽  
pp. 1563-1566 ◽  
Author(s):  
Klaus Hosier ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Bond Angle ◽  
Unit Cell ◽  
Formula Unit ◽  
Double Bonds ◽  
Centrosymmetric Dimer ◽  
Space Group ◽  
Bond Lengths ◽  
Cell Dimensions

Abstract[MoCl4(NPPh3)]2 is prepared by the reaction of Mo2Cl10 with Ph3PNSiMe3 in boiling CH2Cl2 as brown paramagnetic (μeff = 1.72 B.M. at 20 °C) crystals, which contain ~2 mol CH2Cl2 per formula unit. With PPh4Cl the yellow complex PPh4[MoCI3(NPPh3)] · CH2Cl2 is formed. The IR spectra are recorded and discussed. [MoCl4(NPPh3)]2 crystallizes monoclinically in the space group P21/n with two formula units per unit cell (3146 observed independent reflexions, R = 0.046). The cell dimensions are a = 981.6; b = 1401.7; c = 1743.1 pm; β = 101.15°. The complex is centrosymmetric dimer showing MoCl2Mo bridges with Mo-Cl bond lengths of 244 and 278 pm. respectively. The Mo=N = P axis is nearly linear (bond angle 168.5°) with bond lengths MoN = 172 pm and PN = 166 pm. which correspond to double bonds.

Notizen: 1,2-Dimethoxyethan-Komplexe von MoNCl3 und WNCl3. Die Kristallstruktur von [MoNCl3 · DME] / 1,2-Dimethoxyethane Complexes of MoNCl3 and WNCl3. The Crystal Structure of [MoNCl3 · DME]

1993 ◽  
Vol 48 (12) ◽  
pp. 1841-1844 ◽  
Author(s):  
Eva Rentschler ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Organic Solvents ◽  
Structure Determination ◽  
Triple Bond ◽  
Trans Position ◽  
Molybdenum Complex ◽  
Structure Solution ◽  
In Trans ◽  
Moisture Sensitive

The complexes [MoNCl3·DME] and [WNCl3·DME] (DME = 1,2-dimethoxyethane) have been prepared by the reaction of the nitride chlorides MNC13 with equimolar amounts of DME in CH2Cl2 suspensions. They form orangered, moisture sensitive crystals, which are soluble in organic solvents. The molybdenum complex has been characterized by a crystal structure determination. Space group Pbca, Z = 8, structure solution with 1781 observed unique reflections, R = 0.031. Lattice dimensions at –60°C: a = 738.6(1), b = 1182.2(1), c = 2314.1(1) pm. [MoNCl3·DME] forms monomeric complexes with chelating DME molecules and Mo–O bond lengths of 215.4(4) and 247.4(4) pm, the longer one being in trans-position of the nitrido ligand. The MoN bond length of 163.3(5) pm suggests a triple bond.

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