Notizen: Die Kristallstruktur des Rhenium-Tolankomplexes [ReCl4(PhC ≡ CPhXOPCl3)] / The Crystal Structure of the Rhenium-tolane Complex [ReCl4(PhC ≡ CPh)(OPCl3)]

1993 ◽  
Vol 48 (7) ◽  
pp. 1019-1022 ◽  
Author(s):  
Gerlinde Frenzen ◽  
Dorothea Wolff von Gudenberg ◽  
Kurt Dehnicke
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Oxygen Atom ◽  
Bond Length ◽  
Trans Position ◽  
X Ray ◽  
Bond Lengths ◽  
In Trans ◽  
Ray Methods ◽  
Ligand Bond

The crystal structure of [ReCl4(PhC = CPh)(OPCl3)] was solved with X-ray methods. Space group P1̄, Z = 2, 2085 observed unique reflections, R = 0.029. Lattice dimensions at -70°C: a = 857.0(2), b = 937.9(2), c = 1249.6(2) pm, α = 87.43(3)°, β = 83.48(3)°, γ = 89.80(3)°. [ReCl4(PhC ≡ CPh)(OPCl3)] has a molecular structure with the alkyne ligand bonded side-on (bond lengths Re-C 198.9(8) and 198.6(7) 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 226.7(5) pm).

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)°).

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.

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, 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.

Crystal Structure of α-Zn2V2O7

1973 ◽  
Vol 51 (7) ◽  
pp. 1004-1009 ◽  
Author(s):  
Ramanathan Gopal ◽  
Crispin Calvo
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Bond Length ◽  
Fold Axis ◽  
Full Matrix ◽  
X Ray ◽  
R Value ◽  
The Individual ◽  
Zn Ions ◽  
Oxygen Atoms

α-Zn2V2O7 is monoclinic with lattice parameters a = 7.429(5), b = 8.340(3), c = 10.098(3) Å, β = 111.37(5)°, Z = 4 and space group C2/c. The structure was refined using a full matrix least-squares with 1034 reflections measured with a quarter-circle General Electric automatic X-ray diffractometer to a final R value of 0.066. The anion consists of a pair of VO4 tetrahedra sharing an oxygen atom which lies on a two-fold axis. The bridging V—O bond length is 1.775(4) Å while the three independent terminal ones are 1.728(4), 1.704(7), and 1.658(8) Å long. These bond lengths are consistent with the charge character around the individual oxygen atoms. The Zn ions are coordinated to five oxygen atoms with Zn—O bonds ranging from 1.973 to 2.088°Å. The structure is similar to that of α-CU2P2O7 and transforms to the thortvietite structure at about 615 °C.

scholarly journals Die Kristallstruktur von PPh3Me[NbOCl4(CH3CN)] / The Crystal Structure of PPh3Me[NbOCl4(CH3CN)]

1984 ◽  
Vol 39 (1) ◽  
pp. 107-110 ◽  
Author(s):  
W. Hiller ◽  
J. Strähle ◽  
H. Prinz ◽  
K. Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Nitrogen Atom ◽  
Bond Length ◽  
Unit Cell ◽  
Trans Position ◽  
Space Group ◽  
X Ray ◽  
Oxo Ligand ◽  
Solvate Molecule

The X-ray structure of PPh3Me[NbOCl4(CH3CN)] at 210 K was solved (space group P1̄, two formula units per unit cell, a = 1173.5(5), b = 1130.1(4), c = 946.8(3) pm, α = 97.70(4), β = 93.57(3), γ = 78.62(3)°, 3688 inde­pendent reflexions, R = 0.025). The material consists of cations [P(C6H5)3CH3]⊕ and anions [NbOCl4(CH3CN)]⊖. The nitrogen atom of the acetonitrile solvate molecule is coordinated to the niobium centre in the trans-position to the oxo ligand; the NbO bond length of 169 pm corresponds to a double bond.

Lewis-Säure/Base Addukte von TiCl4 und Methylpyridinen / Lewis Acid/Base Adducts of TiCl4 and Methylpyridines

2000 ◽  
Vol 55 (9) ◽  
pp. 877-881 ◽  
Author(s):  
Karl Hensen ◽  
Alexander Lemke ◽  
Michael Bolte
Keyword(s):  
Molecular Structure ◽  
Lewis Acid ◽  
Equatorial Position ◽  
Acid Base ◽  
Nitrogen Base ◽  
X Ray ◽  
Nitrogen Bases ◽  
Distorted Trigonal Bipyramid ◽  
In Trans ◽  
Ray Methods

By the reaction of 2-methyl- and 2,6-dimethylpyridine the first neutral TiCl4L complexes (L = single bonded ligand) could be synthesized. The structures have been determined by single crystal X-ray methods. The best description of the molecular structure is a distorted trigonal bipyramid with the nitrogen base occupying an equatorial position. With 2,4-dimethylpyridine, a 1:2 adduct is formed, where the nitrogen bases are in trans-positions of a TiCl4N2-octahedron, as also confirmed by an X-ray analysis

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.

Cis-2-telluro-1.3.2λ5.4λ3-diazadiphosphetidin - Kristallstruktur eines in Lösung fluktuierenden Redoxsystems / Cis-2-telhirium-1.3.2λ5.4λ3-diazadiphosphetidine - Crystal Structure of a Redox System Fluctuating in Solution

1978 ◽  
Vol 33 (6) ◽  
pp. 610-613 ◽  
Author(s):  
Siegfried Pohl
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Bond Length ◽  
Title Compound ◽  
Redox System ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Nitrogen Ring

Abstract The crystal structure of the title compound was determined from single crystal X-ray data. The compound crystallises in the orthorhombic space group Pnma. In contrast to the solution where fluctuating P-Te bonds have been established by NMR analyses the crystals contain isolated molecules with fixed P-Te bonds (bond length: 235.4 pm). The four-membered phosphorus nitrogen ring exhibits significant deviations from planarity. The P-N bond lengths were found to be 168.3 and 175.0 pm, respectively

Notizen: Synthesis and Crystal Structure of the Hydrogen Bonded Complex of Tri-paratoluidylphosphazenyl Oxide with Ethyl Alcohol

1976 ◽  
Vol 31 (9) ◽  
pp. 1295-1296 ◽  
Author(s):  
T. Stanley Cameron ◽  
M. Gerard Magee ◽  
Samuel Mclean
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Oxygen Atom ◽  
Ethyl Alcohol ◽  
Title Compound ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Bond Lengths ◽  
X Ray Crystallography ◽  
Phosphoryl Oxygen

The title compound was synthesised and its structure determined by X-ray crystallography. The structure contains a hydrogen bond between the OH group of the alcohol and the phosphoryl oxygen atom. The P–N bond lengths are significantly different and the differences can be attributed to varying ρπ—dπ interactions along the bonds.

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