Molecular structure and bonding properties of bis(1-methylimidazole)bis(perchlorato)bis(pyridineN-oxide)copper(II)

Summary The crystal and molecular structure of bis(1-methylimidazole)bis(perchlorato)bis(pyridineN-oxide)copper(II) have been determined using three-dimensional x-ray diffraction data. The complex crystallizes in space group P2₁/c with Z=2. The cell dimensions area=9.355(3),b=14.363(4),c=9.698(4) Å, and =106.40(3)^o. Least-squares refinement of the structure has yielded a final R value of 0.049 for 1235 independent reflections. The centrosymmetric structure consists oftrans pairs of 1-methylimidazole and pyridineN-oxide figands forming a square planar geometry with Cu–N and Cu–O bond lengths of 1.963(4) Å and 1.948(4) Å, respectively. The two perchlorate ions are located above and below the square plane with Cu–O distances of 2.590(5) Å. The uv-vis and i.r. spectra and bonding properties of the title compound are discussed with reference to the structure.     

Hexafluorosilicates of bis(carboxypyridinium) and bis(2-carboxyquinolinium)

The preparation and characterization of three isomeric carboxypyridinium and carboxyquinolinium hexafluorosilicate salts is described. The salts of the general formulas (LH)₂[SiF₆] (I-III, L = 2-carboxypyridine, 3-carboxypyridine, 4-carboxypyridine) and (LH)₂[SiF₆]·2H₂O (IV, L = 2-carboxyquinoline) were prepared from the protonation reaction of the corresponding pyridine carbonic acid by the fluorosilicic acid. The compounds were characterized by IR, mass-spectrometry, thermogravimetric analysis, solubility data, and in the case of III by X-ray crystallography. The relationship between the salts solubility and the H-bonding system was analysed.     

Synthesis and characterization of sodium bis(trimethylstannyl) amide and bis(trimethylsilyl) bis(trimethylstannyl) -phospha-tetrazene

Sodium bis(trimethylstannyl)amide NaN(SnMe₃)₂, isolated by the reaction of trimethylstannyldiethylamine with sodium amide, reacts with tris(trimethylsilyl)hydrazino—dichloro-phosphine to form bis(trimethylsilyl)bis(trimethylstannyl)-2-phospha-2-tetrazene, (Me₃Si)₂N-N=P-N(SnMe₃)₂. Both the molecules have been isolated and characterized.     

Preparation and characterization of bis(acetonitrile)bis(acetylacetonato)technetium(III)

A new chemical species of bis(acetonitrile)bis(acetylacetonato)technetium(III), [Tc(acac)₂(CH₃CN)₂]⁺, has been prepared by the reaction of tris(acetylacetonato)technetium(III) with acetonitrile in the presence of a strong acid, perchloric or hydrochloric acid. The reaction kinetics were followed by observing spectral change of Tc(acac)₃ in the UV-visible region. The complex has been characterized by combination of elemental analyses, IR and UV-visible spectrophotometry, ion-exchange chromatography, and paper electrophoresis. Applicability of this substance to synthesize mixed-ligand technetium(III) complexes was discussed based on the solubility of this complex and the ease of substitution of the acetonitrile ligand.     

The polysulfonylamines bis(methylsulfonamido) sulfone and bis(trifluoromethylsulfonamido) sulfone

Bis­(methyl­sulfon­amido) sulfone, C₂H₈N₂O₆S₃ or SO₂(NHSO₂CH₃)₂, was synthesized from imidobis­(sulfonyl ­chloride), HN(SO₂Cl)₂, and bis­(tri­methyl­silyl)­methane, CH₂[Si(CH₃)₃]₂, in ­chlorotri­methyl­silane solution. In the solid state, there are two independent mol­ecules linked by two N—H⋯O hydrogen bridges into infinite chains parallel to the b axis. The central S atoms of the independent molecules each lie on a twofold axis. Bis­(tri­fluoro­methyl­sulf­onamido) sulfone, C₂H₂F₆N₂O₆S₃ or SO₂(NHSO₂CF₃)₂, was formed by the reaction of tri­chloro­phosphazosulfuryl tri­fluoro­methane, Cl₃PNSO₂CF₃, with fluoro­sulfonic acid, FSO₃H. The mol­ecules are connected by bifurcated N—H⋯O bridges into infinite layers parallel to the [001] plane. The central S atom lies on a twofold axis.     

Darstellung,struktur und eigenschaften on bis(cyclopentadienyl)oxalatotitan(IV) und bis(cyclopentadienyl)bis(hydrogenmaleinato)titan(IV)

The reaction of (π-C₅H₅)₂TiCl₂ with oxalic acid or maleic acid in aqueous solution yields dicyclopentadienyloxalatotitanium(IV) or dicyclopentadienylbis(hydrogenmaleato)titanium(IV), respectively. X-ray analyses show that both compounds are monomeric. The oxalate group acts as bidentate chelating ligand and each of the hydrogenmaleate groups is bonded via one oxygen atom to the titanium atom.     

Synthesis and characterization of bis(cyclopentadienyl)bis(hexafluoroantimonato) titanium(IV)

Reaction of titanocene dichloride with two equivalents of silver hexafluoroantimonate in sulphur dioxide quantitatively yields Cp₂Ti(SbF₆)₂ (Cp = η⁵-C₅H₅) and AgCl. The titanocene bishexafluoroantimonate was recrystallized from SO₂ and characterized by chemical analysis, ¹H NMR, IR and mass spectroscopy.