Nickel(II) complex with 4,4,4-trifluoro-1-(2-thienyl)butane-1,3-dione and dimethyl sulfoxide: Crystal and molecular structures

A nickel(II) complex with 4,4,4-trifluoro-1-(2-thienyl)butane-1,3-dione and dimethyl sulfoxide, [Ni(C₈H₄F₃O₂S)₂(C₂H₆OS)₂], was obtained and examined by X-ray diffraction. The crystals are monoclinic: a = 7.557(2) Å, b = 17.854(3) Å, c = 10.470(2) Å, β = 106.412(3)°, V = 1355.1(4) ų, ρ_calcd = 1.611 g/cm³, Z = 2, space group P2₁, R = 0.032. The coordination polyhedron of the nickel atom is a distorted octahedron consisting of four equatorial O atoms of two β-diketonate ligands and two axial O atoms of DMSO. The average Ni-O_ax and Ni-O_eq distances are 2.083(2) and 2.019(2)Å, respectively. The crystal structure is built from the discrete mononuclear complexes [Ni(C₈H₄F₃O₂S)₂(C₂H₆OS)₂] linked only by van der Waals contacts.     

Molecular and crystal structures of the complex of 18-dehydroglycyrrhetic acid with dimethyl sulfoxide

The crystal structure of the complex of 18-dehydroglycyrrhetic acid (GLD) with DMSO (C₃₀H₄₁O₄·C₂H₆OS) has been determined by x-ray structural analysis. Syntex P21 diffractometer, CuK radiation, 1309 reflections, R = 0.080. A conformational analysis has been made of the GLD molecule in comparison with that of glycyrrhetic acid. The conformations of rings A and B in the GLD molecule do not differ from the conformations of the corresponding rings of glycyrrhetic acid. Differences arise in ringsC,D, andE because of the presence of the double bond between the C18 and C19 atoms.Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 362–366, May-June, 1996. Original article submitted Novemher 11, 1995.     

Copper(II) complex with thienyltrifluoroacetylacetone and dimethyl sulfoxide: Synthesis and crystal structure

A new copper(II) complex with thienyltrifluoroacetone (Tfa) and dimethyl sulfoxide (DMSO), Cu(Tfa)₂DMSO, was synthesized, and its X-ray diffraction analysis was carried out. The crystals were triclinic: a = 9.4496(5), b = 10.5075(6), c = 11.9160(6) Å, α = 82.600(1)°, β = 84.116(1)°, γ = 77.904(1)°, V = 1143.8(1) ų, space group P $ \bar 1 $ , Z = 2, ρ_calcd = 1.696 mg/m³, R = 0.0700. The environment of the copper atom was formed by four oxygen atoms of two thienyltrifluoroacetylacetone molecules and one oxygen atom of DMSO.     

Synthesis and crystal structures of two lead(II) complexes of 4,4,4-trifluoro-1-naphthyl-1,3-butanedione ligand,subtle interplay of weak intermolecular interactions

[Pb₂(tfnb)₄ (µ-CH₃OH)] _n (1) and [Pb₂(dmp)₂(tfnb)₄] (2) (tfnb and dmp are the abbreviations for 4,4,4-trifluoro-1-naphthyl-1,3-butanedionate and 2,9-dimethyl-1,10-phenanthroline) have been synthesized and characterized by elemental analysis, IR, ¹H NMR spectroscopy, and thermal analysis. The single-crystal structure of 1 shows that the complex forms two 1-D polymeric networks containing four types of Pb²⁺ with coordination numbers seven for Pb(1) and Pb(3), five for Pb(2), and six for Pb(4). The single-crystal structure of 2 shows that the complex forms a dinuclear complex with eight-coordinate Pb(II). The supramolecular features in this complex are guided by lone-pair activity and the control of weak directional intermolecular interactions and aromatic π–π stacking interactions.     

二甲亚砜-二[4,4,4-三氟-1-(2-噻吩基)-1,3-丁二酮]合铜(II)的晶体结构

制备了标题化合物单晶,确定了它的分子和晶体结构,结果表明Cu(II)与五个氧原子配位,其中之一来自沿轴向(CH3)2SO.形成略为变形的四方锥结构.在配体上的噻吩基取顺式围绕差Cu(II)原子,这可以共轭效应来解释.     

Molecular and crystal structure of 4,4,4-trifluoro-3,3-dihydroxy-1-thiophene-2-yl-butane-1-one

An X-ray diffraction analysis and quantum chemical calculations of hydrated 2-thenoyltrifluoroacetone show that the planar diketone, form of TTA found in its metal complexes, does not occur in the free ligand. Hydrated TTA with two geminal hydroxo groups has a non-planar structure stabilized by an intramolecular hydrogen bond.     

Synthesis and unusual crystal structure of the Eu(III) complex with 1-(1,5-dimethyl-1H-pyrazol-4-yl)-4,4,4-trifluorobutane-1,3-dione

The reaction of Eu(NO₃)₃ · 6H₂O with 1-(1,5-dimethyl-1H-pyrazol-4-yl)-4,4,4-trifluorobutane-1,3-dione (HL) in the presence of NaOH in aqueous ethanol gave neutral complex [EuL₃(H₂O)] (I). The unstable adduct [EuL₃(H₂O)] · 1.3MeCN (Ia) was obtained from an acetonitrile solution and studied by X-ray diffraction. The crystals of Ia at 100 K are monoclinic, a = 17.551(3) Å, b = 11.532(2) Å, c = 20.371(3) Å, β = 110.886(3)°, V = 3852(1) ų, space group P2₁/c, Z = 4, R = 0.0505. The molecules are connected into chains by strong interactions between the europium atom of one molecule and the pyrazole N(2) atom of another molecule and additionally stabilized by strong hydrogen bonds O(1w)-H(1w1)…N(4)*. The chains are combined into layers by the hydrogen bonds (1w)-H(2w1)…N(2)*.     

Cobalt(II) silanethiolato complexes with dimethylpyridines: crystal structures and spectroscopic studies

Cobalt(II) tri-tert-butoxysilanethiolates with 2,5-dimethylpyridine, 3,4-dimethylpyridine and 3,5- dimethylpyridine co-ligands have been synthesized by reaction of bimetallic [Co{μ-SSi(O ^t Bu)₃}{SSi(O ^t Bu)₃}(NH₃)]₂ with the appropriate pyridines. The complexes were characterized by elemental analysis, single-crystal X-ray structure determination, IR and UV–Vis spectroscopy. These complexes are tetra- or penta-coordinated with CoN₂S₂ and CoNO₂S₂ cores, respectively.     

2-N-Tosylaminobenzaldehyde ferrocenoylhydrazone and its nickel(II) complex: Molecular and crystal structures

2-N-Tosylaminobenzaldehyde ferrocenoylhydrazone (H₂L) and the octahedral nickel(II) complex [Ni(HL)₂] · 2CH₃OH (I) are synthesized and structurally characterized (CIF files CCDC 981876 (H₂L) and 981877 (I)). The crystal structures of both compounds include two independent molecules with different mutual orientations of the tosyl and ferrocene fragments. In a single crystal of H₂L, the independent molecules are joined by intermolecular hydrogen bonds into infinite linear chains extended along the crystallographic axis x. The π-stacking interaction between the cyclopentadienyl rings is observed along with hydrogen bonds in a single crystal of complex I.     

Tris-(4,4,4-trifluoro-1-(-2-thienyl)-1,3-butandiono)-europium(III) als NMR-Verschiebungsreagens

The shift reagent behaviour of europium thenoyltrifluoroacetonate has been investigated for various substrates. Due to its good solubility this complex is superior to Eu(DPM)₃ for weak complexing substrates. Thus, it was possible to assign the C₉ and C₁₀ signals in the ¹³C–NMR spectra of D(+)-Camphor.     

Crystal Structure of Complex Tris(4,4,4-trifluoro-1-phenyl-1,3-butanedione)(1,10-phenanthroline) Europium(III)

IntroductionCertainlanthanideionspossessharpemissionlinesinthevisibleregions.Thepossibilityoftransferringenergyeffi cientlytotheseionsbywayofstronglyabsorbingtransitionscharacteristicoforganicligandshasspurredmanyworkerstoinvestigatelanthanidechelatesaspotentiallasermaterials .Amongthemtheternarycomplexesofeuropium(III)andter bium(III)withtris(β diketonates)andanneutralligandhaveespeciallyattractedmuchattentionfortheirstronglumi nescence.Itmakethemaextensiveapplicationsindevelop mentofnewl…     

Molecular and crystal structure of 4-trifluoro-2-[2-(4-fluorophenyl)hydrazine-1-ylidene]-1-(thiophen -2-yl)butane-1,3-dione

Single crystal X-ray diffraction is used to determine the crystal and molecular structure of 4-trifluoro-2-[2-(4-fluorophenyl)hydrazine-1-ylidene]-1-(thiophen-2-yl)butane-1,3-dione. Crystallographic data for C₁₄H₈F₄N₂O₂S are as follows: a = 8.2723(6) ?, b = 9.3009(7) ?, c = 9.9895(7) ?; α = 79.224(2)°, β = 75.851(2)°, γ = 72.337(2)°. Triclinic crystal system, P-1 space group, d _x = 1.622 g/cm³, V = 704.83(9) ?³, μ = 0.286 mm⁻¹, crystal size 0.30×0.20×0.20 mm, R1 = 0.0891, wR2 = 0.1989.     

Mixed-ligand chelate extraction of trivalent lanthanides with 4,4,4-trifluoro-1-phenyl-1,3-butanedione and neutral oxo-donors

Mixed-ligand chelate extraction of trivalent lanthanides such as Nd(III), Eu(III) and Lu(III) into benzene with mixtures of 4,4,4-trifluoro-1-phenyl-1,3-butanedione (HBFA) and bis-2-ethylhexyl sulphoxide (B2EHSO) or triphenylphosphine oxide (TPhPO) from thiocyanate solutions was investigated. The results demonstrate that these metal ions are extracted as Ln(BFA)(3) with HBFA alone and in the presence of a neutral oxo-donor, B2EHSO or TPhPO(S), as Ln(BFA)(3).S and Ln(BFA)(3).2S. The equilibrium constants of the above species increase monotonically with decreasing ionic radii of these metals ions. The addition of a neutral donor to the metal chelate system not only enhances the extraction efficiency but also improves the selectivity among these trivalent lanthanides. Hence this mixed-ligand system may be useful for the extraction and separation of individual lanthanides and also for the separation of lanthanides as a group from other metal ions.