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.     

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?.     

Synthese und Struktur eines Caesium-tetraimidophosphat-diamids,Cs5[P(NH)4](NH2)2 = Cs3[P(NH)4] · 2 CsNH2

Synthesis and Crystal Structure of a Cesium-tetraimidophosphate-diamide, Cs₅[P(NH)₄](NH₂)₂ = Cs₃[P(NH)₄] · 2 CsNH₂ Well crystallized Cesium-tetraimidophosphate-diamide is obtained by the reaction of CsNH₂ with P₃N₅ in autoclaves at 673 K within three days. X-ray single crystal investigations led to the following data

• Ccca, Z = 4, a = 8.192(5) Å, b = 20.472(5) Å,
• c = 8.252(3) Å
• Z(F) ≥3σ(F) = 916, Z(Var.) = 32, R/R_w=1 = 0.017/0.021

The compound contains the hitherto unknown anion [P(NH)₄]^3?.     

Kristallstrukturen des Sr(BrO3)2 · H2O,Ba(BrO3)2 · H2O,Ba(IO3)2 · H2O,Pb(CIO3)2 · H2O und Pb(BrO3)2 · H2O

Crystal Structure of Sr(BrO₃)₂ · H₂O, Ba(BrO₃)₂ · H₂O, Ba(IO₃)₂ · H₂O, Pb(ClO₃)₂ · H₂O, and Pb(BrO₃)₂ · H₂O The crystall structures of the isostructural halates Sr(BrO₃)₂ · H₂O, Ba(BrO₃)₂ · H₂O, Ba(IO₃)₂ · H₂O, Pb(ClO₃)₂ · H₂O, and Pb(BrO₃)₂ · H₂O were determined using X-ray single crystal data (monoclinic space group C2/c? C, Z = 4), The mean bond lengths and bond angles of the halate ions in the Ba(ClO₃)₂ · 1 H₂O-type compounds, which correspond to those of other halates, are Cl? O, 149.0, Br? O, 165.9, I? O, 180.2 pm, ClO₃^?, 106.4, BrO₃^?, 104.0, and IO₃^?, 99.6°. The structure data obtained are discussed in terms of possible orientational disorder of the water molecules, strengths of the hydrogen bonds, influence of the lead ions on the structure, and site group distortion of the halate ions.