Molybdenum dinitrogen complexes facially coordinated by linear tridentate PEP ligands (E = N or P): impact of the central E donor in trans-position to N2

2016 ◽  
Vol 45 (37) ◽  
pp. 14801-14813 ◽  
Author(s):  
Svea Hinrichsen ◽  
Ann-Christin Schnoor ◽  
Katharina Grund ◽  
Benedikt Flöser ◽  
Alexander Schlimm ◽  
...  
Keyword(s):  
Trans Position ◽  
Dinitrogen Complexes ◽  
In Trans

The syntheses of new molybdenum dinitrogen complexes supported by the tridentate PEP ligands (E = N, P) prPP(Ph)P (2), prPPHP (3), PN(Ph)P (4) and prPN(Ph)P (5) are reported.

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.

Mononuclear ruthenium complexes containing two different phosphines in trans position: II. Catalytic hydrogenation of CC and CO bonds

2007 ◽  
Vol 692 (7) ◽  
pp. 1442-1450 ◽  
Author(s):  
Luca Salvi ◽  
Antonella Salvini ◽  
Francesca Micoli ◽  
Claudio Bianchini ◽  
Werner Oberhauser
Keyword(s):  
Catalytic Hydrogenation ◽  
Ruthenium Complexes ◽  
Trans Position ◽  
In Trans

Darstellung und Kristallstrukturen von Phenyliodoantimonaten(III). Strukturkorrelation für Halogenoantimonate(III) / Preparation and Crystal Structures of Phenyliodoantimonates(III). Structural Correlation for Haloantimonates(III)

1991 ◽  
Vol 46 (5) ◽  
pp. 639-646 ◽  
Author(s):  
W. S. Sheldrick ◽  
C. Martin
Keyword(s):  
Structural Analysis ◽  
Crystal Structures ◽  
Iodine Atom ◽  
Trans Position ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Structural Correlation ◽  
Bipyramidal Structure ◽  
In Trans

The phenyliodoantimonates(III) [Et4N][Ph2SbI2] (1), [Et4N]2[Ph2Sb2I6] (2) and [Hpy]3[Ph2Sb2I7] (3) have been prepared and their structures established by X-ray structural analysis. The anion [Ph2SbI2]⁻ displays a ψ-trigonal bipyramidal structure with axial Sb–I distances of 2.925(1) and 3.109(1) A. In the dimeric anions [Ph2Sb2I6]2- and [Ph2Sb2I7]3- the antimony atoms exhibit ψ-octahedral geometries. As observed for [Ph2SbI2]⁻, terminal Sb–I bonds in trans-position to one another display significantly different lengths. The anion [Ph2Sb2I7]3- displays Ci- symmetry with a bridging iodine atom at the crystallographic centre of symmetry. Long Sb—I distances of 3.404(1) A are observed to this atom. A structural correlation of opposite Sb–X distances (X = Cl, Br, I) in linear three centre X–Sb ··· X interactions is presented. The sum of the bond valences in iodoantimonates(III) is a minimum for symmetrical I–Sb–I three centre bonds, reflecting thereby the antibonding influence of the Sb 5 s-orbital. This influence is considerably smaller for bromoantimonates(III) and may be effectively neglected for chloroantimonates(III).

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.

Palladium Complexes with Bidentate P,N Ligands: Synthesis, Characterization and Application in Ethene Oligomerization

2002 ◽  
Vol 57 (7) ◽  
pp. 803-809 ◽  
Author(s):  
Gabi Müller ◽  
Martti Klinga ◽  
Peter Osswald ◽  
Markku Leskelä ◽  
Bernhard Rieger
Keyword(s):  
Single Crystal ◽  
Phosphorus Atom ◽  
Palladium Complexes ◽  
Metal Center ◽  
Coordination Geometry ◽  
Trans Position ◽  
Pyridine Ligand ◽  
X Ray ◽  
Square Planar ◽  
In Trans

Palladium complexes of two different P,N ligands (a phosphane-pyridine and a phosphane-imine ligand) were synthesized and characterized. Single crystal X-ray structure analyses of the palladium diiodide compounds revealed a square-planar coordination geometry at the metal center with a longer Pd-I bond in trans-position to the phosphorus atom. The chloro-methyl palladium species of the phosphane-pyridine ligand was applied for the oligomerization of ethene using a borate salt as cocatalyst.

Die Kristallstrukturen von [MoCl2(NO)2(OPEt3)]2, [MoCl3(NO)(OPPh3)2•MoCl4(OPPh3)2], [MoCl2(NO)(PPh3)2(CH3CN)] und [MoCl4(NPPh3)(OPPh3)] / The Crystal Structures of [MoCl2(NO)2(OPEt3)]2, [MoCl3(NO)(OPPh3)2 • MoCl4(OPPh3)2], [MoCl2(NO)(PPh3)2(CH3CN)], and [MoCl4(NPPh3)(OPPh3)]

1995 ◽  
Vol 50 (1) ◽  
pp. 1-10 ◽  
Author(s):  
Gunnar Philipp ◽  
Sigrid Wocadlo ◽  
Werner Massa ◽  
Kurt Dehnicke ◽  
Dieter Fenske ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Trans Position ◽  
Nitrosyl Complex ◽  
Centrosymmetric Dimer ◽  
Acetonitrile Molecule ◽  
Space Group ◽  
Structure Determinations ◽  
In Trans ◽  
Complex Forms

The title compounds have been prepared by reactions of MoCl2(NO)2 with PPh3, OPPh3, or Me3SiNPR3 (R = Et, Ph) in dichloromethane and acetonitrile suspension, respectively. All complexes were characterized by IR spectroscopy and by crystal structure determinations. [MoCl2(NO)2(OPEt3)]2: Space group C2/c, Z = 4, 2950 observed unique reflections, R = 0.029. Lattice dimensions at —70 °C: a = 2390.5(11), b = 875.5(5), c = 1399.1(6) pm, β = 113.18(2)°. The complex forms a centrosymmetric dimer with MoCl2Mo bridges, the nitrosyl groups being in a cis-arrangement. The OPEt3 ligand is coordinated in trans position to one of the nitrosyl ligands.[MoCl3(NO)(OPPh3)2 • MoCl4(OPPh3)2]: Space group P21/c, Z = 4, 10243 observed unique reflections, R = 0.060. Lattice dimensions at —60 °C: a = 1900.4(3), b = 1689.1(5), c = 2209.3(7) pm, β = 95.92(2)°. The structure consists of the two independent complexes [MoCl3(NO)(OPPh3)2] and [MoCl4(OPPh3)2]. In both complexes the OPPh3 groups are in a cis-arrangement at the octahedrally coordinated Mo atoms; in the nitrosyl complex one of the OPPh3 molecules is in trans-position to the nitrosyl ligand.[MoCl2(NO)(PPh3)2(CH3CN)]: Space group P21/n, Z = 4, 5107 observed unique reflections, R = 0.028. Lattice dimensions at 20 °C: a = 1006.5(2), b = 1527.2(2), c = 2342.3(2) pm, β = 90.97(1)°. The PPh3 molecules are in trans-positions to one another at the octahedrally coordinated Mo atom, whereas the acetonitrile molecule is in trans-position to the nitrosyl ligand.[MoCl4(NPPh3)(OPPhi)]: Space group P21, Z = 2, 3323 observed unique reflections, R = 0.057. Lattice dimensions at —70 °C: a = 985.7(8), b = 1471.2(9), c = 1215.9(11) pm, β = 100.50(3)°. The OPPh3 molecule coordinates in trans-position to the phosphorane iminato ligand at the octahedrally coordinated Mo atom.

Notizen: Gezielte Synthese von Sulfinato-O–und -S-Komplexen einiger Übergangsmetalle, XVIII1 Synthese eines Sulfinato-O-Komplexes und Ionisationsisomerie bei Palladium(II)2 / Directed Synthesis of Sulfinato-O and -S Complexes of Some Transition Metals, XVIII1. Synthesis of a Sulfinato-O Complex and Ionization Isomerism with Palladium(II)2

1977 ◽  
Vol 32 (2) ◽  
pp. 234-235 ◽  
Author(s):  
Ingo-Peter Lorenz ◽  
Ekkehard Lindner ◽  
Wolfgang Reuther
Keyword(s):  
Transition Metals ◽  
Structural Models ◽  
Ethylene Diamine ◽  
Trans Position ◽  
Ionic Compound ◽  
Directed Synthesis ◽  
In Trans ◽  
Ligand Addition

The sulfinato-O complex (p-CH3C6H4S(O)O)2Pd(en) (2a) and its ionization isomer, the ionic compound [Pd(en)2][p-CH3C6H4SO2]2 (2b), are obtained from 1 by ligand addition in dependence of the nature of the solvent. 2 a, b can be transformed into each other reversibly. For 2 a two structural models are discussed. The pseudooctahedral configuration with two bidentate ethylene diamine and two sulfinato-O ligands in trans position seems to be more likely.

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