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Methyl 5-chloro-2-hydr-oxy-3-(4-methoxyphenyl)-4,6-dimethylbenzoate

2009, Adeel, M., Ali, I., Langer, P., Villinger, A.

In the title compound, C17H17ClO4, the dihedral angle between the mean planes of the two benzene rings is 65.92 (5)°. The methyl ester group lies within the ring plane [deviations of O atoms from the plane = -0.051 (2) and 0.151 (2) Å] due to an intra-molecular O - H⋯O hydrogen bond. In the crystal, molecules are held together by rather weak non-classical inter-molecular C - H⋯O hydrogen bonds, resulting in dimeric units about inversion centers, forming eight- and ten-membered ring systems as R22(8) and R2 2(10) motifs. © Adeel et al. 2009.

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P-[N-(Diphenyl-phospho-rothio-yl)iso-propyl-amino]-N-isopropyl-P-phenyl- thio-phosphinic amide

2009, Peulecke, N., Aluri, B.R., Wöhl, A., Spannenberg, A., Al-Hazmi, M.H.

The title compound, C24H30N2P2S2, was obtained by the reaction of Ph2PN(iPr)P(Ph)N(iPr)H with elemental sulfur in tetra-hydro-furan. In the solid state, intra-molecular N - H⋯S hydrogen bonding influences the mol-ecular conformation; a P - N - P - N torsion angle of 2.28 (9)° is observed. The two phenyl rings attached to one P atom form a dihedral angle of 74.02 (4)°.

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Diacetonitrile[N,N′-bis(2,6-diisopropyl-phenyl)ethane-1,2-diimine] dichloridochromium(II) acetonitrile solvate

2009, Peitz, S., Peulecke, N., Müller, B.H., Spannenberg, A., Rosenthal, U.

The title compound, [CrCl2(CH3CN)2(C 26H36N2)]·CH3CN, was synthesized by the reaction of CrCl2(THF)2 with N,N′-bis-(2,6- diisopropyl-phen-yl)ethane-1,2-diimine in dichloro-methane/acetonitrile. The chromium center is coordinated by two N atoms of the chelating diimine ligand, two chloride ions in a trans configuration with respect to each other, and by two N atoms of two acetonitrile mol-ecules in a distorted octa-hedral geometry.

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Crystal structure of (2S,4S,7S)-7,7-dichloro-4-(1-chloro-1-methylethyl)-1- (2,2,2-trichloroethyl)bicyclo[4.1.0]heptane, C12H16Cl 6

2009, Boualy, B., el Firdoussi, L., Ali, M.A., Karim, A., Spannenberg, A.

C12H16Cl6, orthorhombic, P2 12121 (no. 19), a = 6.0742(3) Å, b = 9.7189(6) Å, c = 26.700(1) Å, V = 1576.2 Å3, Z = 4, Rgt(F) = 0.019, wRref(F2) = 0.045, T= 200 K. © by Oldenbourg Wissenschaftsverlag.

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[1-Dimethylsilyl-2-phenyl-3-(η5-tetramethylcyclopentadienyl) prop-1-en-1-ylκC1](n5-pentamethylcyclopentadienyl)- titanium(III)

2009, Lamač, M., Spannenberg, A., Arndt, P., Rosenthal, U.

The title compound, [Ti(C10H15)(C20H 26Si)], was obtained from the reaction of [Ti{5: 1-C5Me4(CH2)}(5-C 5Me5)] with the alkynylsilane PhC2SiMe 2H. The complex crystallizes with two independent mol-ecules in the asymmetric unit, which differ in the conformation of the propenyl unit, resulting in their having opposite helicity. No inter-molecular inter-actions or inter-actions involving the Si- H bond are present. The observed geometrical parameters are unexceptional compared to known structures of the same type.

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Bis[N,N′-bis-(2,6-diisopropylphenyl)ethane-1,2-diimine] -1κ2 N,N′;2κ2 N,N′-tri - Trichlorido-1:2κ6 Cl:Clchlorido-1Cltetrahydrofuran- 2Odichromium(II) dichloromethane 4.5-solvate

2009, Peitz, S., Peulecke, N., Müller, B.H., Spannenberg, A., Rosenthal, U.

In the mol-ecular structure of the title compound, [Cr2Cl4(C 26H36N2)2(C4H8O)] ·4.5CH2Cl2, the two CrII centers are bridged by three Cl atoms, forming a dinuclear complex. Each CrII center is coordinated by one chelating bis-(2,6-diisopropyl-phen-yl)ethane-1,2-diimine ligand via both N atoms. An additional chloride ion binds to one chromium center, whereas an additional tetra-hydro-furan mol-ecule coordinates to the second CrII center. The coordination geometry at each CrII center can be best described as distorted octa-hedral.

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[N,N-Bis(diphenyl­phosphino)isopropyl­amine]dibromidonickel(II)

2009, Hapke, M., Wöhl, A., Peitz, S., Müller, B.H., Spannenberg, A., Rosenthal, U.

The title compound, [NiBr2(C27H27NP2)], was synthesized by the reaction of NiBr2(dme) (dme is 1,2-dimethoxy-ethane) with N,N-bis-(diphenyl-phosphino)isopropyl-amine in methanol/tetra-hydro-furan. The nickel(II) center is coordinated by two P atoms of the chelating PNP ligand, PH2PN(iPr)PPH2, and two bromide ions in a distorted square-planar geometry.

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Redetermination of EuScO3

2009, Kahlenberg, V., Maier, D., Veličkov, B.

Single crystals of europium(III) scandate(III), with ideal formula EuScO3, were grown from the melt using the micro-pulling-down method. The title compound crystallizes in an ortho-rhom-bic distorted perovskite-type structure, where Eu occupies the eightfold coordinated A sites (site symmetry m) and Sc resides on the centres of corner-sharing [ScO6] octa-hedra (B sites with site symmetry ). The structure of EuScO3 has been reported previously based on powder diffraction data [Liferovich & Mitchell (2004). J. Solid State Chem. 177, 2188-2197]. The results of the current redetermination based on single-crystal diffraction data shows an improvement in the precision of the structral and geometric parameters and reveals a defect-type structure. Site-occupancy refinements indicate an Eu deficiency on the A site coupled with O defects on one of the two O-atom positions. The crystallochemical formula of the investigated sample may thus be written as A(0.032Eu0.968)BScO2.952.

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1,1,2,2-Tetra-phenyl-15-diphosphane 1-sulfide

2009, Aluri, B.R., Peitz, S., Wöhl, A., Peulecke, N., Müller, B.H., Spannenberg, A., Rosenthal, U.

In the title mol-ecule, C24H20P2S, the P - P bond length is 2.2263 (5) Å. The two phenyl rings attached to the three- and five-coordinated P atoms, respectively, form dihedral angles of 56.22 (5) and 71.74 (5)°.

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Trans-Di-μ-acetato-[μ-N,N-bis-(diphenyl-phosphino)aniline] bis-[chlorido-molybdenum(II)](Mo - Mo)-dichloro-methane-tetra-hydro-furan (1/0.3/1.7)

2009, Hapke, M., Wöhl, A., Peitz, S., Spannenberg, A., Rosenthal, U.

The mol-ecular structure of the title compound, [Mo2(CH 3COO)2Cl2(C30H25NP 2)]·0.3CH2Cl2·1.7C 4H8O, features an Mo - Mo dumbbell bridged by two acetate groups which are trans to each other. Perpendicular to the plane spanned by the acetate groups, the Ph2PN(Ph)PPh2 ligand bridges both Mo atoms, having a P - N - P angle of 114.09 (19)°. In a trans position to the PNP ligand are two Cl atoms, one on each molybdenum centre. The Mo - Mo bond distance is 2.1161 (9) Å, within the range known for Mo - Mo quadruple bonds. The Mo complex is located on a crystallographic twofold rotation axis which runs through the N - C bond of the ligand. The site occupation factors of the disordered solvent molecules were fixed to 0.15 for dichloromethane and 0.85 for tetrahydrofuran. © 2009.