Iminoacetylacetonat-Komplexe der Lanthanoide: Synthese, Eigenschaften und Struktur / Iminoacetylacetonate Complexes of Lanthanides: Synthesis, Properties and Structure

1993 ◽  
Vol 48 (12) ◽  
pp. 1753-1759 ◽  
Author(s):  
Karl-Heinz Thiele ◽  
Annett Scholz ◽  
Joachim Scholz ◽  
Uwe Böhme ◽  
Rhett Kempe ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Organic Solvents ◽  
Structure Analysis ◽  
Chelate Complexes ◽  
Space Group ◽  
X Ray ◽  
Synthesis Properties ◽  
Lanthanum Complex

The reactions of (η5-C5Me5)2Ln(μ-Cl)2ML2 (Ln = Y, La, Lu; M = Li, K; L = Et2O, dme) 3a-c with the sodium iminoacetylacetonates 2a-b yield monomeric metallocene chelate complexes , (Ln = Y, La, Lu; R = C6H5, C6H4-4-Me) 4a-d which have been characterized by IR, NMR and mass spectrometry. In the case of the lanthanum complex 4c, the chelating structure was confirmed by an X-ray structure analysis. 4c crystallizes monoclinically in space group P21/c with a = 10.232(3), b = 10.216(1), c = 29.047(7)Å, α = γ = 90.0°, β = 97.76(3)°, Ζ = 4, and R = Rw = 0.0378 for 4026 observed reflections. The new complexes are sensitive to oxygen and moisture and soluble in all common organic solvents.

Darstellung, Eigenschaften und Struktur des Cyclopentadienyl(1.3-diborolenyl)nickel-Sandwiehs [1] / Synthesis, Properties and Structure of the Cyclopentadienyl(1,3-diborolenyl)nickel Sandwich [1]

1978 ◽  
Vol 33 (12) ◽  
pp. 1410-1416 ◽  
Author(s):  
Walter Siebert ◽  
Manfred Bochmann ◽  
Joseph Edwin ◽  
Carl Krüger ◽  
Yi-Hung Tsay
Keyword(s):  
Structure Analysis ◽  
Title Compound ◽  
Sandwich Structure ◽  
Unit Cell ◽  
Space Group ◽  
X Ray ◽  
Nmr Data ◽  
Synthesis Properties

Abstract 1,3,4,5-Tetraethyl-2-methyl-1,3-diborolene (5) reacts with nickelocene and dimeric cyclopentadienylcarbonylnickel, yielding orange red 4 a, a diamagnetic nickelocene analogue. 1H and 11B NMR data indicate a sandwich structure, which is confirmed by X-ray structure analysis. The title compound crystallizes in the space group Pnma with a = 9.265(I), b = 15.1343(9), c = 12.777(2) Å and four molecules in the unit cell. All metal carbon distances are similar to those of the isoelectronic ferrocene.

Synthese und Kristallstrukturen von Tris(glykolato)molybdän(VI) und Tris(pinakolato)molybdän(VI) / Syntheses and Crystal Structures of Tris(glycolato)molybdenum(VI) and Tris(pinacolato)molybdenum(VI)

1992 ◽  
Vol 47 (5) ◽  
pp. 706-712 ◽  
Author(s):  
Silke Buth ◽  
Sigrid Wocadlo ◽  
Bernhard Neumüller ◽  
Frank Weller ◽  
Kurt Dehnicke
Keyword(s):  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Structure Analysis ◽  
Chelate Complexes ◽  
Space Group ◽  
X Ray ◽  
Distorted Octahedral ◽  
Sodium Phenolate ◽  
C Nmr ◽  
Oxygen Atoms

PPh4[MoN(OPh)4] has been prepared by reaction of PPh4[MoNCl4] with sodium phenolate, as an orange-red crystal powder. The reactions of glycole and pinacole, respectively, with MoN(O-t-Bu)3 and MoNCl3, the latter in the presence of a base, lead to the tris-chelate complexes Mo(OC2H4O)3 and Mo(OC2Me4O)3, respectively. The complexes were characterized by 1H and 13C NMR spectroscopy, the chelate complexes in addition by X-ray structure analysis.[Mo(OC2H4O)3]: Space group P21/c, Z = 4, 2177 observed unique reflections, R = 0.047. Lattice dimensions at –40 °C: a = 1168.3(2), b = 716.0(1), c = 1206.1(2) pm, β = 92.84(1)°. [Mo(OC,Me4O)3] • 2CH2Cl2: Space group P bcn, Z = 4, 1860 observed unique reflections, R = 0.049. Lattice dimensions at –80°C: a = 1772.3(1), b = 1023.8(1), c = 1600.0(2) pm.Both complexes form monomeric molecules, in which the molybdenum atoms are surrounded in a distorted octahedral fashion by the six oxygen atoms of the chelates.

Die Röntgenstrukturanalyse von (CO)9Co3CΟΒΒr2Ν(C5)3. X-ray Structure Analysis of (CO)9Co3COBBr2N(C2H5)3

1976 ◽  
Vol 31 (3) ◽  
pp. 342-344 ◽  
Author(s):  
Volker Bätzel
Keyword(s):  
Least Squares ◽  
Structure Analysis ◽  
Reliability Index ◽  
Three Dimensional ◽  
Diagonal Matrix ◽  
Crystal Data ◽  
Block Diagonal Matrix ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray

Using three dimensional X-ray data collected on a four circle diffractometer, the structure of (CO)9Co3COBBr2N(C2H5)3 was solved by Patterson and Fourier methods. Least squares refinement with a block-diagonal matrix leads to a reliability index of R = 10.7%. Crystal data: α = 13.277(6) Å, b = 10.17(1) Å, c = 9.22(2) Å; α = 91.12(6)°, β = 87.61(4)°, γ = 98.79(2)°; space group P1̅; Z = 2; V = 1229,7 Å3; Dx = 1.97 gcm-3.

Zur Struktur und Dotierung von Selenosilikaten: die Kristallstruktur von Er2SeSiO4 und Er3,75Ca0,25Se2,75Cl0,25Si2O7 Structure and Doping of Seleno Silicates: the Crystal Structures of Er2SeSiO4 and Er3,75Ca0,25Se2,75Cl0,25Si2O7

1994 ◽  
Vol 49 (6) ◽  
pp. 733-740 ◽  
Author(s):  
Klaus Stöwe
Keyword(s):  
Crystal Structures ◽  
Structure Analysis ◽  
Rare Earths ◽  
Structure Determination ◽  
Lattice Parameters ◽  
Energy Dispersive ◽  
Space Group ◽  
X Ray ◽  
By Products

Well-shaped brown and pink isometric crystals were obtained as by-products of the synthesis of erbium selenides from the elements in evacuated and sealed silica ampoules with graphite inlets. They could be identified as erbium seleno mono- and disilicates by energy dispersive X-ray fluorescence and X-ray structure determination. The monosilicate Er2SeSiO4 crystallizes isotypically to Nd2SeSiO4 in the space group Pbcm with the lattice parameters a = 600.2(2), b = 688.0(2), c = 1075.2(2) pm and represents the second known seleno inosilicate of the rare earths. From X-ray structure analysis an isotypic relation between the disilicate Er3,75Ca0,25Se2,75Cl0,25Si2O7 and the compound Sm4S3Si2O7 was found, the former crystallizing in the space group I41/amd with the lattice parameters a - 1177.7(2) and c = 1376.5(2) pm. The doping o f the sorosilicate with the elements Ca and Cl originated from contam inations in the graphit inlets used in the procedure

Titan(IV)-Fulvalenkomplexe. Darstellung und Struktur von [CpTiPh2l2(C10H8) / Titanium(IV) Fulvalene Complexes. Preparation and Structure of [CpTiPh2]2(C10H8)

1993 ◽  
Vol 48 (5) ◽  
pp. 603-607 ◽  
Author(s):  
Ulf Thewalt ◽  
Thomas Wöhrle
Keyword(s):  
Structure Analysis ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

The green insoluble TiIV compound which is obtained by treating titanocene with HC1 reacts with PhLi to yield the fulvalene-bridged compound [CpTiPh2]2(C10Hg) 3(Ph). An X-ray structure analysis of 3(Ph) shows, that the Ti atoms are in a trans arrangement with respect to the fulvalene group. Crystal data for 3(Ph) are as follows: C44H38Ti2, orthorhombic, space group P212,1 21, with a = 11,385(2), b = 14,510(2), c = 19,489(4) Å, Z = 4. The crystals exhibit enantiomorphism.

Thiocarbonyl Complexes of Rhenium. Part I.

1993 ◽  
Vol 48 (6) ◽  
pp. 771-777 ◽  
Author(s):  
Ulrich Abram ◽  
Bernd Lorenz
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
Monomeric Complex ◽  
Structure Solution ◽  
R Value

Novel rhenium complexes with terminal thiocarbonyl groups have been synthesized from ReCl3(Me2PhP)3 and sodium diethyldithiocarbamate. mer-(Diethyldithiocarbamato)tris-(dimethylphenylphosphine)(thiocarbonyl)rhenium(I), mer-[Re(CS)(Me2PhP)3(Et2dtc)], and tris(diethyldithiocarbamato)(thiocarbonyl)rhenium(III), [Re(CS)(Et2dtc)3] have been studied by infrared and NMR spectroscopy, mass spectrometry and X-ray diffraction.mer-[Re(CS)(Me2PhP)3(Et2dtc)] crystallizes orthorhombic in the space group Pna21 with a = 1516.1(2), b = 2189.8(2) and c = 1035.6(1) pm. Structure solution and refinement converged at R = 0.042. The coordination geometry is a distorted octahedron. The Re—C bond length is found to be 184(2) pm.[Re(CS)(Et2dtc)3] crystallizes monoclinic in the space group P21/c with a = 962.2(6), b = 1744.0(2), c = 1537.4(6) pm and β = 96.21(1)°. The final R value is 0.028. In the monomeric complex the rhenium atom is seven-coordinate with an approximate pentagonal-bipyramidal coordination sphere and a rhenium-carbon distance of 181(1) pm.

Zur Darstellung und Struktur des 1.3-Dichloro-5-N.N-dimethylamino-1.3-dithia-2.4.6-triazins / Synthesis and Structure of 1,3-Dichloro-5-N,N-dimethylamino-1,3-dithia-2,4,6-triazine

1983 ◽  
Vol 38 (3) ◽  
pp. 347-349 ◽  
Author(s):  
Herbert W. Roesky ◽  
Pierre Schäfer ◽  
Mathias Noltemeyer ◽  
George M. Sheldrick
Keyword(s):  
Structure Analysis ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cl Atoms ◽  
C Nmr

Abstract The six membered ring of composition (CH3)2NCN3S2Cl2 3 a was prepared from N,N-dimethylguanidinhydrochloride and trithiadiazindichloride. 3 a was characterized on the basis of mass, 1H, 13C NMR spectra and X-ray structure analysis. Crystals of 3 a are monoclinic, space group P21/c, with a = 660.3(6), b = 834.5(7), c = 1774.7(15) pm, β = 112.83(6)° and Z = 4. The C2N unit lies approximately in the plane of the [-CNSNSN-] ring, with both Cl atoms on the same side of the ring.

scholarly journals Reaction of Cresyl Saligenin Phosphate, the Organophosphorus Agent Implicated in Aerotoxic Syndrome, with Human Cholinesterases: Mechanistic Studies Employing Kinetics, Mass Spectrometry, and X-ray Structure Analysis

2011 ◽  
Vol 24 (6) ◽  
pp. 797-808 ◽  
Author(s):  
Eugénie Carletti ◽  
Lawrence M. Schopfer ◽  
Jacques-Philippe Colletier ◽  
Marie-Thérèse Froment ◽  
Florian Nachon ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Structure Analysis ◽  
Mechanistic Studies ◽  
X Ray

Darstellung und Röntgenstrukturanalyse von (DichIoro)-(1,3,5,7-tetramethyI-2,4,6,8,9,10-hexathiaadamantan)palladium(II), PdCl2(CH3)4C4S6 Preparation and X-Ray Structure Analysis of (D ichloro)-(l,3,5,7-tetram ethyl-2,4,6,8,9,10-hexathiaadam antane)palladium (II), PdCl2(CH3)4C4S6

1986 ◽  
Vol 41 (4) ◽  
pp. 409-412 ◽  
Author(s):  
Joachim Pickardt ◽  
Norbert Rautenberg
Keyword(s):  
Structure Analysis ◽  
Palladium Complex ◽  
Bond Angle ◽  
Free Ligand ◽  
Lattice Parameters ◽  
Space Group ◽  
X Ray ◽  
Chelating Ligand ◽  
Square Planar

By reaction of PdCl2(C6H5CN) 2 with 1,3,5,7-tetram ethyl-2,4,6,8,9,10-hexathiaadam antane, (CH3)4C4S6, (“TMTA”), the complex PdCl2-TMTA could be obtained. X-ray structure analyses were performed for the free ligand TMTA as well as for the adduct. Both com pounds crystallize monoclinically, space group P21/n, lattice parameters for TMTA are a= 845.9(5), b= 1225.8(7), c= 1314.8(8) pm, ß= 93.28(5)°; for PdCl2-TMTA a= 1262.3(3), b= 1376.3(4), c= 939.1(3) pm, and ß= 92.86(5)°. In the palladium complex TMTA acts as a bidentate chelating ligand. The coordination about the Pd atom is approximately square planar, but the bond angle S -Pd -S is only 76.2°

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