Darstellung und Struktur von [Cp2MoHLi(thf)]3 · Toluol

Synthesis and Crystal Structure of [Cp₂MoHLi(thf)]₃ · Toluene [Cp₂MoHLi]₄ reacts in THF/Toluene to the trimeric complex [Cp₂MoHLi(thf)]₃ · Toluene 1 . The structure of 1 was characterized by X-ray single crystal structure analysis. Space group P6₃, Z = 2, a = 1459.5(9) pm, c = 1182.3(8) pm. The central unit is represented by a Mo₃Li₃-hexagon. Each Mo-Atom is surrounded by two Cp-Ligands. One THF-Molecule is coordinated to each Li-atom. The Hydrogen-Ligand could not be located by the single crystal structure analysis.     

Zur Reaktion von 2,2′-Dilithiumbiphenyl mit SmBr3 Die Struktur von [(C24H16)SmBr(thf)2]2 · [C24H14]

On the Reaction of Dilithiumbiphenyl with SmBr₃. The Crystal Structure of [(C₂₄H₁₆)SmBr(thf)₂]₂ · [C₂₄H₁₄] In THF SmBr₃ forms with [(biph)Li₂] the dimeric complex [(quaph)SmBr(thf)₂]₂ · [C₂₄H₁₄]. The structure was characterized by X-ray single crystal structure analysis (space group P1 (No. 2), Z = 1, a = 943.3(6) pm, b = 1 350.3(1) pm, c = 1 599.9(9) pm, α = 64.99(5)°, β = 89.02(5)°, γ = 73.02(6)°). The Sm iones are bridged by two Br iones. Coordination by one quaph and THF ligands leads to distorded octahedra coordination of the Sm iones. Additionally crystallizes one molecule dibenzonaphthacene.     

Synthese und Struktur eines Molybdän–Gadolinium-Heterometall-Komplexes Die Struktur von [Li(thf)4]2[Cp2MoSGdBr4(thf)]2

Synthesis and structure of a Molybdenum–Gadolinium Heterometallic Complex. The Structure of [Li(thf)₄]₂[Cp₂MoSGdBr₄(thf)]₂ [Cp₂MoHLi] reacts in THF with S and GdBr₃ to yield the tetranuclear heterobimetallic complex [Li(thf)₄]₂[Cp₂MoSGdBr₄(thf)]₂. The bonding situation and the structure of this compound were characterized by X-ray structure analysis (space group P1 (No. 2), Z = 1, a = 10.845(2) Å, b = 12.166(2) Å, c = 15.881(2) Å, α = 101.74(2)°, β = 97.62(2)°, γ = 103.97(2)°). Each S atom of the central Mo₂S₂-ring is coordinated by a GdBr₄(thf) fragment. Additionally each Mo atom is connected to two Cp ligands. This leads to a tetrahedral coordination of the Mo atoms and a octahedral coordination of the Gd ions.     

Synthesis and Crystal Structure of [Fe(Cp)2]3(Bi2Cl9)·thf

Single crystals of [Fe(Cp)₂]₃(Bi₂Cl₉)·thf were obtained from a thf solution containing ferrocene and BiCl₃. The structure shows disorder at room temperature which disappears upon cooling, coupled with a decrease in symmetry. The title compound crystallizes in the orthorhombic space group P2₁2₁2₁ [a = 1698.64(2), b = 2318.69(3), c = 1085.66(2) pm] with three ferrocenium ions, one nonachlorodibismutate ion and one molecule of thf in the asymmetric unit.     

[(Ph3Sn)3VO4]·CH3CN und [(Ph3Sn)3VO4]·2 DMF,Triphenylzinnvanadate mit neuartigen Kettenstrukturen

[(Ph₃Sn)₃VO₄]·CH₃CN and [(Ph₃Sn)₃VO₄]·2 DMF, Triphenyltin Vanadates with Novel Chain Structures The reaction of Na₃VO₄ with Ph₃SnCl in a water/CH₂Cl₂ mixture leads to the formation of [(Ph₃Sn)₃VO₄] ( 1 ). Recrystallization of 1 from toluene/CH₃CN gives pale yellow crystals of [(Ph₃Sn)₃VO₄]·CH₃CN ( 2 ). 2 crystallizes as coordination polymer which consists of infinite chains composed of corner‐sharing VO₄ tetrahedra and Ph₃SnO₂ trigonal bipyramides. Additionally the VO₄ groups are connected to two terminal SnPh₃‐Groups containing tin atoms in a tetrahedral environment. [(Ph₃Sn)₃VO₄]·2 DMF ( 3 ) which is obtained from Na₃VO₄ and Ph₃SnCl in a water/DMF mixture contains a polymeric chain structure similar to 2 and additionally one of the terminal SnPh₃ groups is coordinated to a DMF solvent molecule.     

Zur Reaktion von Makrozyklen mit Lanthanoiden. II. Die Strukturen von [K(thf)3]2[(C22H28N4)2Sm2] · 4THF und [(C22H22N4)Co] · DME

On the Reaction of Macrocycles with Lanthanoids. II. The Crystal Structures of [K(thf)₃]₂[(C₂₂H₂₈N₄)₂Sm₂] · 4 THF and [(C₂₂H₂₂N₄)Co] · DME In a complicated redox reaction [(TMTAA)K₂] and [SmI₂(thf)₂] form the polynuclear metal complex [K(thf)₃]₂[(TMTAT)₂Sm₂]. This complex crystallizes with four molecules THF per formula unit and its structure was determined by single crystal X-ray investigation (spacegroup P2₁/c (No. 14), z = 4, a = 998.0(2) pm, = b = 2618.3(6) pm, c = 1619.4(3) pm, β = 96.52(2)°). In the dimeric unit [(TMTAT)₂Sm₂]^2? the Sm³⁺ ions are bonded to the four N atoms of the macrocyclic ligand and one C₆H₄ ring of the second ligand is attached η⁶ like to one metal ion. Additionally two [K(thf)₃]⁺ fragments are bonded to this central unit, and therefor coordination number seven results for the K⁺ ion. [TMTAA]^2? is not reduced by [Cp₂Co] in a similar reaction. The monomeric paramagnetic complex [(TMTAA)Co] (μ_eff = 2,76 μ_B) is formed instead. The structure reveils a square planar coordination of the Co atom by the four N atoms of the TMTAA ligand (spacegroup C2/c (No. 15), z = 4, a = 1945.1(4) pm, b = 1165.6(2) pm, c = 1144.7(2) pm, β = 116.38(1)°).     

The first observation of the [Cp3Mn]- anion; structures of hexagonal [(eta 2-Cp)3MnK.1.5thf] and ion-separated [(eta 2-Cp)3Mn]2[Mg(thf)6].2thf

Hexagonal [(eta 2-Cp)3MnK.1.5thf] 1 and ion-separated [(eta 2-Cp)3Mn]2[Mg(thf)6].2thf 2 are obtained from reactions of CpK and Cp2Mg, respectively, with manganocene, Cp2Mn; they are the first complexes to be structurally characterised containing the [Cp3Mn]- anion.     

Zur Struktur des Isopropylammonium-trichloro-Managanats (II) (CH3)2CHNH3MnCl3 · 2 H2O

On the Structure of Isopropylammonium Trichloro Manganate(II) (CH₃)₂CHNH₃MnCl₃ · 2 H₂O The crystal structure of (i-C₃H₇NH₃)MnCl₃ · 2 H₂O has been determined by X-ray diffraction and the parameters refined by leastsquares calculations. (i-C₃H₇NH₃)MnCl₃ · 2 H₂O is monoclinic, space group P2_1/c with a = 1410(3), b = 584(1) and c = 1299(2) pm, β = 110.5(1)°. There are four formula units per unit cell. The manganese is octahedrally coordinated by four chlorine atoms and two water molecules in “trans” position. The structure contains discrete dioctahedra Mn₂Cl₆(H₂O)₄^2?.     

Lithio-di-t-butylfluorsilylphenylphosphan; im Kristall ein (SiFLiP)2-Achtring

Di-t-butylfluorosilylphenylphosphane (I) reacts with CMe₃Li to give the lithium compound [(CMe₃)₂SiFLi(THF)₂PC₆H₅]₂ (II) and butane. The crystal structure of II has been determined. The SiP bond length (217.1 pm) in the eight-membered ring is extremely short. The SiP spin coupling constant (84.12 Hz) in II is remarkably large. LiF elimination from II leads to the formation of the four-membered (SiP) ring III. The bis(fluorosilyl)phosphane IV is formed in the reaction of II with Me₂SiF₂.