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  • Author: F. Ekkehardt Hahn x
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The reaction of lithiated catechol ligands with W (0)Cl4 produces LiCl as a side product. The lithium chloride from this reaction crystallizes as (THF)2Li(μ-Cl)-,Li(THF)2. The X -ray analysis shows lithium in the center of a distorted tetrahedron made up from two THF molecules and two bridging chlorides with d(Li-Cl) = 2.342(3) and 2.308(3)Å.

The title compound, 1, is obtained as colorless crystals by reaction of LuCl3, NaC5H5 and LiCH3 in the molar ratio 1:1:4 in diethylether in the presence of tmed. 1 crystallizes in the tetragonal space group P412121 a = 8.375(8) Å, c = 28.78(4) Å, V = 2018.6 Å3 and Z = 4. The molecular structure of 1 possesses crystallographically imposed C2-symmetry and consists of a (C5H5)2Lu-moiety joined to a Li(tmed)-unit by two methyl bridges. Principal dimensions are as follows: Lu-C(br) 2.461(12) Å, Li-C(br) 2.24(2) Å. Cp-Lu-Cp′ 131.9(3)°, C(br)-Lu-C′(br) 95.0(3)°.

The o-phenylenediamine ligand tris[3-(2,3-diaminophenoxy)propyl]amine, TRIPACEN (4) and bis[3-(2,3-diaminophenoxy)propyl]amine, DIPACEN (8) are obtained by Williamson coupling of the potassium salt of 2,3-dinitrophenole (1) to tris(3-chlorpropyl)amine (2) or benzylbis(3-chlorpropyl)amine (5), respectively, followed by reduction of the nitro functions with Sn/HCl or Pd(OH)2/H2.

The synthesis of diethylindiumdiphenylphosphinate and the crystal structures of dimethylgalliumdiphenylphosphinate and diethylindiumdiphenylphosphinate are reported. The two structures confirm the proposed dimeric nature of the title compounds with bridging diphenylphosphinate groups. [Ph2P(O)2Ga(CH3)]2 crystallizes triclinically, PĪ, with a = 9.483(6), b = 10.216(4), c = 8.780(9)Å, α = 101.66(5)°, β = 113.74(5)°, γ = 69.93(5)° and Ζ = 1 (dimer). [Ph2P(O)2In(C2H5)2]2 crystallizes monoclinically, C2/c, with a = 19.971(5), b = 8.590(2), c = 19.457(5)Å, β = 102.91(2)° and Ζ = 4 (dimers). Both structures contain tetrahedrally coordinated phosphorous and metal atoms.

The palladium(II) dicarbene complex trans-[PdBr2(L)2], 2 (L = 1,3-di-(2-propenyl)-benzimidazol- 2-ylidene) was synthesized from 1,3-di-(2-propenyl)-benzimidazolium bromide 1 and Pd(OAc)2 by in situ deprotonation. The X-ray structure analysis revealed a mononuclear complex with a palladium( II) center coordinated in a square-planar fashion by the two carbene functions and two bromo ligands.

The red title compound was synthesized by the metathesis reaction of [FeCl2(dppe)] (dppe = Ph2PCH2)2PPh2) and NaS-tBu in THF. The X-ray structure analysis revealed a dinuclear complex with two iron(II) centers coordinated in a distorted tetrahedral fashion by two bridging thiolates, one bridging dppe molecule and one terminal chloro ligand.

The reaction of the aliphatic unsymmetrical tripod [N(CH2CH2NH2)2(CH2CH2OH)], H5-1, with cobalt(II) chloride in THF yields after aerial oxidation the dinuclear complex [(H4-1)CoIII(μ-OH)CoIII(H4-1)](CoIICl4)Cl, [5](CoCl4)Cl. The trianion 53− contains two cobalt atoms triply bridged by two alkoxo groups of the singly deprotonated ligand (H4-1) and a hydroxo group. The new ligand [N(CH2CH2CH2NH2)(CH2CH2OH)2], H4-3, providing an N2O2 donor set reacts with cobalt(II) chloride to give after aerial oxidation the hexanuclear complex [CoIII 4(H2-3)4CoII 2(HOMe)2Cl2(μ-OH)4], [6]Cl2, containing an unprecedented mixed-valent CoIII 4CoII 2 core.

Abstract

The tetrakis(phenyl isocyanide)nickel(0) complexes [Ni(CNR)4](R = C6H5, 1; R= C6H3-2,6-Me2, 2; R = C6H4-2-NO2, 3) have been synthesized from [Ni(COD)2] and the corresponding phenyl isocyanides in toluene. Complexes 1 - 3 were characterized by X-ray diffraction. All three complexes contain a nickel atom which is coordinated in a slightly distorted tetrahedral fashion.

Abstract

The pale yellow palladium(II) dicarbene complex cis-[PdI2(L)], 2 (L = 1,3-bis-(3-neopentylbenzimidazol- 2-ylidene)-2,2-dimethylpropane) was synthesized by the reaction of PdI2 with an N1,N1’- 2,2’-dimethylpropane-bridged dibenzotetraazafulvalene 1 in tetrahydrofuran. The X-ray structure analysis revealed a mononuclear complex with a palladium(II) center coordinated in a slightly distorted square-planar fashion by the bidentate carbene ligand and two iodo ligands.

Abstract

The reaction of the dibenzotetraazafulvalene C6H4(NC2H5)2C=C(NC2H5)2C6H4, 1 = 1, with [(COD)Rh(μ-Cl)2Rh(COD)] proceeds via cleavage of the C=C double bond and yields the carbene complex [(COD)RhCl(1)], 2. The X-ray structure analysis shows 2 to be a mononuclear complex with a rhodium(I) center coordinated in a slightly distorted square-planar fashion.