Übergangsmetall-substituierte Phosphane, Arsane und Stibane, XXVII [1] Wolfram-Komplexe mit Di(tert-butyl)arsino-, mono- oder dihapto-Di(tert-butyl)thioarsinyl-Liganden / Transition-Metal Substituted Phosphanes, Arsanes and Stibanes, XXVII [1] Tungsten Complexes with Di(tert-butyl)arsino, mono- or dihapto-Di(tert-butyl)thioarsinyl Ligands

1981 ◽  
Vol 36 (12) ◽  
pp. 1580-1587 ◽  
Author(s):  
Wolfgang Malisch ◽  
Michael Luksza ◽  
William S. Sheldrick
Keyword(s):  
Transition Metal ◽  
Spectroscopic Data ◽  
Elemental Sulfur ◽  
Dynamic Behaviour ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Space Group ◽  
X Ray ◽  
Tert Butyl ◽  
Tungsten Complexes

The reaction of But2AsCl with Na[W(CO)3Cp] in THF yields the metal arsine Cp(CO)3W−AsBut2 (1), which is oxidized with elemental sulfur to the arsine sulfide Cp(CO)3W−AsBut2(S) (2). 2 is converted in refluxing pentane with loss of CO into Cp(CO)2W(η2-AsBut2S) (3). The chiral complex contains the novel dihapto-But2As−S ligand and exhibits dynamic behaviour (⊿G≠286 = 15.4 kcal/mol). Side-on coordination of the But2As−S ligand is proved by spectroscopic data and X-ray analysis. 3 crystallizes in the monoclinic space group P21/n with a = 12.141(2), b = 15.179(2), c = 19.558(2) Å, β = 99.61(2)°. The structure was refined to R = 0.051 for 4087 independent reflections.

scholarly journals Übergangsmetall-Carben-Komplexe, CXXXIV [1]. Synthese neuer Mono- und Biscarben-Komplexe der VI. Nebengruppe; Röntgenstruktur des ersten Bis[amino(alkoxy)carben]-Komplexes / Transition Metal Carbene Complexes, CXXXIV [1]. Synthesis of New Mono- and Bis-Carbene Complexes of Group VIb Elements; Structure of the First Bis[amino(alkoxy)carbene]-Complex

1984 ◽  
Vol 39 (5) ◽  
pp. 668-674 ◽  
Author(s):  
Ernst Otto Fischer ◽  
Rudolf Reitmeier ◽  
Klaus Ackermann
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Spectroscopic Data ◽  
The Novel ◽  
Nucleophilic Agent ◽  
Reaction Conditions ◽  
Carbene Complexes ◽  
X Ray ◽  
X Ray Crystallography ◽  
New Compounds

The hexacarbonyl compounds of chromium, molybdenum and tungsten react with the highly nucleophilic agent Li NiPr2 and in a subsequent alkylation with (Et3O)BF4 to give the carbene complexes (CO)5M[C(N′Pr2)OEt] (1, 3, 4). In case of W(CO)6 and Mo(CO)6 the novel biscarbene complexes cis(CO)4M[C(NiPr2)OEt]2 (2, 5) are additionally obtained. Reaction conditions, properties and spectroscopic data of the new compounds are reported. The molecular structure of cis(CO)4W[C(NiPr2)OEt]2 (4) was determined by X-ray crystallography

Reaktion von [Co(But2PH)2I2] mit [Ru3(CO)12]: Synthese und Röntgenkristallstrukturanalyse von [Ru3(CO)6(μ-H)(μ-I)2(μ-PBut2)(But2PH)]/ Reaction of [Co(But2PH)2I2] with [Ru3(CO)12]: Synthesis and X-Ray Crystal Structure of [Ru3(CO)6(μ-H)(μ-I)2(μ-PBut2)(But2PH)]

1998 ◽  
Vol 53 (8) ◽  
pp. 865-870 ◽  
Author(s):  
Marion Graf ◽  
Kurt Merzweiler ◽  
Clemens Bruhn ◽  
Hans-Christian Böttcher
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Cluster Expansion ◽  
Metal Clusters ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Space Group ◽  
X Ray ◽  
Iodine Transfer

Abstract [Co(But2PH)2I2] (1) reacts with [Ru3(CO)12] in refluxing toluene to give a mixture of products including the novel metal clusters [Ru3(CO)6(μ-H)(μ-I)2(μ-PBut2)(But2PH)] (2) and [Ru3(CO)7(μ-H)(μ-I)(μ-PBut2)2] (3) besides the known complex [Ru3(CO)8(μ-H)2(μ3- PBut)(But2PH)] (4). No cluster expansion products could be observed. Thus the cobalt compound acts merely as a phosphine and iodine transfer reagent. The molecular structures of the metal complexes 1 and 2 were determined by single-crystal X-ray structure analyses. 1 crystallizes in the tetragonal space group P4̄21c with a = 13.230(3), b = 13.230(3), c = 14.788(3)Å, V = 2588.4(9)A . 2 crystallizes in the monoclinic space group P21/c with a = 18.161(2), b = 10.292(2), c = 18.381(2)Å, β = 108.73(10)°, V= 3253.7(8)Å3.

Reactions of Transition-Metal Sigma-Acetylides. V. Synthesis and X-Ray Structure of Co2(µ-η2-PhC2Fe(Co)2(η-C5h5))(Co)6

1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Diffraction Study ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.

S4N4 und seine Derivate: α-FeCl3 · S4N4, ein Übergangsmetallkomplex mit dem S4N4-Ligand / S4N4 and its Derivatives: α-FeCl3 · S4N4, a Transition Metal Complex with the S4N4 Ligand

1980 ◽  
Vol 35 (7) ◽  
pp. 855-859 ◽  
Author(s):  
Ulf Thewalt
Keyword(s):  
Transition Metal ◽  
Metal Complex ◽  
Iron Atom ◽  
Transition Metal Complex ◽  
Lattice Parameters ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The adduct α-FeCl3 · S4N4 has been prepared from FeCl3 and S4N4 in CCl4. The new compound crystallizes in the monoclinic space group P 21/c with Z = 4 and lattice parameters a = 6.360(2), b = 13.066(4), c = 12.686(5) Å, and β = 99.43(3)°. An X-ray analysis shows that the S4N4 ring is bonded via one of its nitrogen atoms to the iron atom of the FeCl3 group and that the four ligand atoms around the iron atom form a tetrahedron. The structure of the complex is similar to the known structure of BF3 · S4N4

scholarly journals Darstellung und Charakterisierung der μ3-Oxo-Cluster [Cp3Mo3(CO)4µ-Cl)(µ3-O)] und [Cp3Mo3(µ-CO)3(CO)3(µ3-O)]+ / Synthesis and Characterization of the µ3-Oxo Clusters [Cp3Mo3(CO)4μ-Cl)(μ3-O)] and [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+

1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler
Keyword(s):  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.

Reaktionen N-silylierter Endiamine, I Übergangsmetallkomplexe von 1,3-Diaza-2-sila-4-cyclopentenen / Reactions of N-Silated Endiamines, I Transition Metal Complexes of 1,3-Diaza-2-sila-4-cyclopentenes

1986 ◽  
Vol 41 (10) ◽  
pp. 1230-1238 ◽  
Author(s):  
Michael Zettlitzer ◽  
Heindirk tom Dieck ◽  
Lutz Stamp
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Structural Data ◽  
Spectroscopic Properties ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Poorly Soluble

Abstract1,3-Di̲aza-2-s̱ila-4-c̱yclopentenes 1 (DISC), which are electron-rich and easily oxidizable ole­ fins, form strongly coloured, but poorly soluble 1:1 adducts with cuprous halides, while silver trifluoromethylsulfonate oxidizes 1. Much more soluble and again strongly coloured complexes of stoichiometry LPdX2, (L)1.5PdX2 and L 2PdX2 are formed from 1 and palladium halides. The well-crystallizing adduct (PdCl2 · L)2 3a was chosen for an X-ray structure analysis (monoclinic, space group P2/c; a = 10.215(3), b = 14.681(3), c =23.642(5) Å , β = 101.31(2)°; Z = 8 ; R = 0.054), which revealed an almost planar DISC ligand in an oblique η2(C=C)-coordination relative to the π-plane. Structural data and rather peculiar spectroscopic properties encourage a comparison of 3a with complexes, in which an electron-rich olefin is split to give a bis(carbene) ligand system. The electronic reasons for the splitting of electron-rich olefins at d8 metals are discussed under symmetry considerations.

Synthesis, characterization, and X-ray structural studies of octahedral transition metal complexes incorporating the novel anionic tridentate ligand, dimethyl(ethanolamino)(1-pyrazolyl)- gallate, [Me2Ga(OCH2CH2NH2)(N2C3H3)]−

1978 ◽  
Vol 56 (9) ◽  
pp. 1212-1221 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Tridentate Ligand ◽  
The Novel ◽  
Structural Studies ◽  
Space Group ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

Details of the synthesis and physical properties of octahedral transition metal complexes of the tridentate tris chelating ligand [Me2Ga(OCH2CH2NH2)(N2C3H3)]− are given. Crystals of sym-fac-bis[dimethyl(ethanolamino)(1-pyrazolyl)gallato(N(2),O,N]nickel(II) are monoclinic, a = 11.7908(6), b = 7.3158(6), c = 12.5797(8), β = 97.035(7)°, Z = 2, space group P21/n and crystals of the mer isomer are monoclinic, a = 18.6617(7), b = 8.7941(4), c = 13.5670(8), β = 91,766(4)°, Z = 4, space group P21/c. The structures were solved by Patterson and Fourier syntheses and were refined by full-matrix least-squares procedures to final R values of 0.048 and 0.052 for 1881 and 2573 reflections with I ≥ 3σ(I) for the fac and mer isomers respectively. The nickel atoms in both structures were found to have distorted octahedral coordination geometry. Bond lengths (corrected for libration) are: Ni—O, 2.090(3); Ni—N, 2.085(3) and 2.112(3); Ga—O, 1.908(3); Ga—N, 2.010(3); and Ga—C, 1.979(5) and 1.981(6) Å for the fac isomer, and Ni—O, 2.045(4) and 2.049(4); Ni—N, 2.091 (4)-2.156(5); Ga—O, 1.898(4) and 1.899(4); Ga—N, two at 1.991 (5); and Ga—C, 1.948(8)-1.971 (7) Å for the mer isomer.

Übergangsmetall-substituierte Phosphane, Arsane und Stibane, XLY. Einige Komplexe mit Dreiringstruktur: Aufbau aus Metallo-arsinsulfiden. Öffnung des Metallacyclus mit Phosphordonoren / Transition-Metal Substituted Phosphanes, Arsanes and Stibanes, XLV. Some Complexes with a Three Membered Ring Structure: Formation from Metallo-arsinesulfides. Opening of the Metallacycle with Phosphorus Donors

1984 ◽  
Vol 39 (8) ◽  
pp. 1123-1128 ◽  
Author(s):  
Michael Luksza ◽  
Wolfgang Malisch
Keyword(s):  
Transition Metal ◽  
Structure Formation ◽  
Spectroscopic Data ◽  
Elemental Sulfur ◽  
Dynamic Behaviour ◽  
Ring Structure ◽  
Membered Ring

AbstractThe interaction of the metallo-arsanes Cp(OC)2(L)W - AsR2(1a -c) with elemental sulfur or selenium leads to the formation of the metallo-arsinesulfides (selenides) Cp(OC)2(L)W -AsR2(S,Se) (2a-c), which are converted to the metallacyclic complexes (3a, b) with loss of CO on refluxing in pentane. While the of 3b is cleaved at the W -S bond by (MeO)3P to give Cp(OC)2[(MeO)3P]W -AsMe2(S), (4), with an A s-bonded η1-thioarsinyl ligand, Me3P preferentially cleaves the W -As bond in 3b, d to produce Cp(OC)2(Me3P)W -S -AsR2 (5a, b), in which the R2As-S-unit is S-coordinated. The spectroscopic data of the new complexes are reported and discussed with respect to the dynamic behaviour of the compounds.

Cyclische Diazastannylene, III1 Die Kristall-und Molekülstruktur der monoklinen Phase von 1.3-Di-tert-butyl-2.2-dimethyl-1.3.2.4λ2 -diazasilastannetidin / The Crystal and Molecular Structure of the Monoclinic Phase of 1,3-Di-feri-butyl-2,2-dimethyl-1,3,2,4λ2 -diazasilastannetidine

1978 ◽  
Vol 33 (1) ◽  
pp. 7-13 ◽  
Author(s):  
M. Veith
Keyword(s):  
Molecular Structure ◽  
Monoclinic Phase ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Site Symmetry ◽  
Space Group ◽  
X Ray ◽  
Tert Butyl ◽  
Cell Dimensions

Abstract The crystal and molecular structure of the monoclinic phase of 1,3-di-tert-butyl-2,2-dimethyl-1,3,2,4λ2 -diazasilastannetidine has been determined from three-dimensional X-ray data collected on a two-circle diffractometer at -120 °C (MoKa radiation, 2623 reflexions, R - 0,050). The crystals are monoclinic, space group C2/c, with cell dimensions a = 10.655(5), b = 25.75(1), c = 17.33(1) Å, β = 106.8(1)° and Z = 12. Four monomeric (crystal site symmetry 2 (C2)) and four dimeric units (crystal site symmetry 1̄ (Ci)) are present in the structure interacting over tin-tin (3.68 Å). Remarkable are the very short Sn-N bond (2.09 Å) in the monomer and the donation bond Sn-N (2.39 Å) in the dimer. The coordination of the tin atoms in the different units is discussed in detail.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

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