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.

Donor-Akzeptor-Komplexe von WCl3(N3S2) und WBr3(N3S2). Die Kristallstruktur von WCl3(N3S2) ·THF/ Donor Acceptor Complexes of WCl3(N3S2) and WBr3 (N3S2).The Crystal Structure of WCl3(N3S2)·THF

1987 ◽  
Vol 42 (8) ◽  
pp. 943-946 ◽  
Author(s):  
Abderraouf Khabou ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Dihedral Angle ◽  
Trans Position ◽  
X Ray Diffraction ◽  
Tungsten Atom ◽  
X Ray ◽  
Cell Dimensions ◽  
Donor Acceptor ◽  
In Trans

AbstractThe donor acceptor complexes WC13(N 3S2)-L (L = TH F, pyridine), and [WCl3(N3S2)]2 · dipy are prepared from WCl3(N3S2) and the corresponding donor molecules. WBr3(N3S2) ­ THF is formed by the reaction of WCl3(N3S2) THF with BrSiMe3. The complexes have been characterized by their IR spectra. The crystal structure of WCl3(N3S2) THF was determ ined by X-ray diffraction. It crystallizes monoclinically in the space group P21/c with four formula units per unit cell (1903 observed, independent reflexions, R = 0.031); the cell dimensions are a = 1072.0. b = 1007.2, c = 1128.9 pm; β = 94.84°. The tungsten atom is a member of a nearly planar WN3S2 ring with WN bond distances of 180 and 184 pm, which correspond to double bonds. The sixfold coordination of the W atom is completed by three chlorine atoms and the O atom of the tetrahydrofuran ligand, which is coordinated in trans-position to one of the N atoms; the THF molecules forms a dihedral angle of 40.1° with the WN3S2 ring.

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.

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)°).

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.

Pentamethylcyclopentadienyl-Vanadium Complexes Containing Halogeno- and Oxo-Ligands

1987 ◽  
Vol 42 (12) ◽  
pp. 1520-1526 ◽  
Author(s):  
Max Herberhold ◽  
Walter Kremnitz ◽  
Markus Kuhnlein ◽  
Manfred L. Ziegler ◽  
Karl Brunn
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
High Yield ◽  
Vanadium Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Oxygen Bond ◽  
Single Bonds ◽  
Oxo Ligands

AbstractA simple and high-yield preparation of the pentamethylcyclopentadienyl vanadium(IV) trihalides Cp*VX3 (X = CL, Br, I) from Cp*V(CO)4 as well as their conversion into the oxo-vanadium(V) compounds Cp*VOX2 (X = CL, Br) and [Cp*VOX]2(μ-O) (X = CL, Br, I) are described. The equilibrium between the two fluoride species Cp*VOF2 and [Cp*VOF]2(μ-O) has also been investigated. The complexes are characterized by their NMR (51V, l3C, 1H), IR, and mass spectra. The crystal structure of the binuclear chloro-oxo complex [Cp*VOCl]2(μ-O) has been determined by X-ray diffraction. The molecules contain two [Cp*VOCl] units combined via a bent oxo bridge (V-O-V angle of 142.2(2)°). The vanadium-oxygen bond lengths are 157.6(8) and 179.4(1) pm for the terminal and the bridging oxo ligands, respectively, corresponding to double and single bonds.

Synthese, Schwingungs- und Massenspektren von Et2Sn(O2PR2)2 (R = Me, Ph); Kristallstruktur von Et2Sn(O2PPh2)2 / Synthesis, Vibrational Spectra and Mass Spectra of Et2Sn(O2PR2)2 (R = Me, Ph); Crystal Structure of Et2Sn(O2PPh2)2

1996 ◽  
Vol 51 (8) ◽  
pp. 1111-1116 ◽  
Author(s):  
Abdel-Fattah Shihada ◽  
Frank Weller
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectra ◽  
Mass Spectra ◽  
Structure Refinement ◽  
Base Peak ◽  
Trans Position ◽  
X Ray Diffraction ◽  
X Ray ◽  
Octahedral Environment ◽  
In Trans

Et2Sn(O2PPh2)2 has been synthesized by the reaction of (Et2ClSn)2O with Ph2POCl in toluene and by the treatment of (Et2ClSn)2O or Et2SnCl2 with HO2PPh2 in methanol. The reaction of Et2SnO with HO2PMe2 in toluene was used to prepare Et2Sn(O2PMe2)2. An X-ray diffraction study of Et2Sn(O2PPh2)2 (space group P1̅, Z = 1, a = 559,9( 1), b = 983,7(1), c = 1262,4(l)pm, α = 81,85( 1 )°, β = 79,79( 1)°, γ = 75,00(1)°; structure refinement with 2662 independent reflections, R = 0.055) shows that the structure is polymeric and the O2PPh2 ligands function as double bridges between the tin atoms leading to the formation of centrosymmetric Sn2O4P2 eight-membered rings. The ethyl groups are in trans-position in the resulting octahedral environment around tin. The I. R. and Raman spectra of Et2Sn(O2PR2)2 (R = Ph, Me) have been discussed and assigned. The mass spectra of Et2Sn(O2PR2)2 show Sn(O2PR2)+ as the base peak.

Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur / Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure

1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
The Other ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Lattice Constants ◽  
Bond Lengths

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides

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.

Structural Characterization of Bis[N-(o-Hydroxybenzyl-(S)-Leucinato)]cobaltate(III) Anion. Tyrosine-Like Model Complex with Structurally Inequivalent Chelate Rings

1996 ◽  
Vol 61 (12) ◽  
pp. 1754-1766
Author(s):  
Svetlana Pakhomova ◽  
Jan Ondráček ◽  
František Jursík
Keyword(s):  
Structural Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Model Complex ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Average Bond ◽  
C Nmr

[Co(NH3)4(H2O)2]OH . [Co(ohb-(S)-Leu)2] . 2 H2O (ohb, o-hydroxybenzyl) was characterized by single-crystal X-ray diffraction which shows that both ligands in the [Co(ohb-(S)-Leu)2]- anion assume facial coordination mode with all donor atoms trans to each other, proposed on the basis of UV-VIS and 13C NMR spectroscopy, with R,S configuration of secondary N atoms. Compound crystallizes in the tetragonal space group I41 with unit cell dimensions a = 22.173(7), c = 13.270(2) Å, V = 6 524 Å3, Z = 4. Structural data show that both ligands are not equivalent. Bond angles and bond lengths depend on whether secondary N atoms adopt R or S configuration. The average bond lengths are shorter when the ohb-(S)-Leu ligand coordinates with (N)R configuration.

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