Chloridobis[2-(diphenylphosphanyl)ethanamine-κ(2)P,N](triphenylphosphane-κP)ruthenium(II) chloride toluene monosolvate.

The aminophosphane ligand 1-amino-2-(diphenylphosphanyl)ethane [Ph2P(CH2)2NH2] reacts with dichloridotris(triphenylphosphane)ruthenium(II), [RuCl2(PPh3)3], to form chloridobis[2-(diphenylphosphanyl)ethanamine-κ(2)P,N](triphenylphosphane-κP)ruthenium(II) chloride toluene monosolvate, [RuCl(C18H15P)(C14H16NP)2]Cl·C7H8 or [RuCl(PPh3){Ph2P(CH2)2NH2}2]Cl·C7H8. The asymmetric unit of the monoclinic unit cell contains two molecules of the Ru(II) cation, two chloride anions and two toluene molecules. The Ru(II) cation is octahedrally coordinated by two chelating Ph2P(CH2)2NH2 ligands, a triphenylphosphane (PPh3) ligand and a chloride ligand. The three P atoms are meridionally coordinated, with the Ph2P- groups from the ligands being trans. The two -NH2 groups are cis, as are the chloride and PPh3 ligands. This chiral stereochemistry of the [RuCl(PPh3){Ph2P(CH2)2NH2}2](+) cation is unique in ruthenium-aminophosphane chemistry.

Bromidobis[3-(1H-pyrazol-1-yl-κN(2))propionamide-κO]copper(II) bromide methanol monosolvate.

The title copper(II) N-pyrazolylpropanamide (PPA) complex, [CuBr(PPA)(2)]Br, was obtained in 78% yield by treatment of CuBr(2) with an excess of the ligand in methanol. Crystallization from the mother liquid afforded the title compound, i.e. the methanol solvate [CuBr(C(6)H(9)N(3)O)(2)]Br·CH(3)OH or [CuBr(PPA)(2)]Br·MeOH, as bright green crystals. In the solid state, the title salt comprises isolated [CuBr(PPA)(2)](+) cations, separated bromide ions and methanol of crystallization. In the cation, the central Cu(II) ion is coordinated by two N,O-chelating PPA ligands and one Br(-) ion. The coordination geometry around the Cu(II) ion is distorted trigonal-bipyramidal with the bromide ligand and the amide O atoms occupying the equatorial positions [Cu-Br = 2.4443 (4) Å; Cu-O = 2.035 (2) and 2.179 (2) Å], while the pyrazole N atoms coordinate in the axial positions [Cu-N = 1.975 (2) and 1.976 (2) Å]. In the crystal, the three constituents are linked by N-H⋯Br, O-H⋯Br, and N-H⋯O hydrogen bonds, forming a three-dimensional network.

Synthesis and crystal structures of three new benzotriazolylpropanamides.

The base-catalyzed Michael addition of 2-methyl-acryl-amide to benzotriazole afforded 3-(1H-benzotriazol-1-yl)-2-methyl-propanamide, C10H12N4O (1), in 32% yield in addition to small amounts of isomeric 3-(2H-benzotriazol-2-yl)-2-methyl-propanamide, C10H12N4O (2). In a similar manner, 3-(1H-benzotriazol-1-yl)-N,N-di-methyl-propanamide, C11H14N4O (3), was prepared from benzotriazole and N,N-di-methyl-acryl-amide. All three products have been structurally characterized by single-crystal X-ray diffraction. The crystal structures of 1 and 2 comprise infinite arrays formed by N-H⋯O and N-H⋯N bridges, as well as π-π inter-actions, while the mol-ecules of 3 are aggregated to simple π-dimers in the crystal.