Kenneth J Takeuchi

A hydrogen-bonded dichloromethane-perchlorate-water channel in the crystal structure ofcis-[Ru(bpy)2{PPh-(o-tolyl)2}Cl+][ClO4−]·CH2Cl2·H2O

The complexcis-[Ru(bpy)2{PPh(o-tolyl)2}Cl+][ClO4−] crystallized from a solution in dichloromethane as the dichloromethane-water solvate. The structure was refined toR=4.5% for those 2433 reflections with |Fo|>6σ(|Fo|). The octahedral Ru(II) cation is associated with metal-ligand distances as follows: Ru−Cl=2.434(3)Å, Ru-PPh(o-tol)2=2.382(2)Å, and Ru−N=2.037(7)–2.088(7)Å. The structure is stabilized by a hydrogen-bonded CH2Cl2...ClO4−...H2O channel which incorporates adventitious water of crystallization.

Crystal structure ofmer,trans-[Ru(NO2)(trpy)(PPr3) 2 + ][ClO 4 − ], a species with disordered PPr3 and NO2 ligands

The complexmer,trans-[Ru(NO2)(trpy)(PPr3)2+][ClO4−]crystallizes in the centrosymmetric orthorhombic space group Pnma withZ=4. Both the ruthenium(II) cation and the perchlorate ligand lie about crystallographic mirror planes. The nitro ligand is not coplanar with the Ru(trpy) moiety and suffers from two fold disorder about its Ru−N bond such that the two sets of oxygen atoms have symmetry-related sites above or below the crystallographic mirror plane. The n-propyl groups within the PPr3 ligands suffer from disorder of their C(α) and C(β) atoms but share common C(γ) sites. Ruthenium-ligand distances are: Ru−PPr3=2.398(2)Å, Ru−NO2=2.053(7) Å, Ru−N(trpy, outer)=2.078(6) and 2.092(6) Å and Ru−N(trpy, central) =1.965(6) Å.

Crystal structure ofmer,trans-[Ru(NO2)(trpy) (PPh3) 2 + ][PF 6 − ]: a “problem structure”

The complexmer,trans-[Ru(NO2)(trpy)(PPh3)2+][PF6−] crystallizes in the centrosymmetric monoclinic space groupP21/n withZ=4; the ruthenium atom lies close toy=1/4 and all data withh+l=2n+1 are systematically weak. The trpy ligand is not strictly planar, but has a “dish-like” geometry. The nitro ligand is rotated from the plane of the Ru(trpy) moiety, the N3Ru/NO2 interplanar angle being 32.5o. Ruthenium-ligand distances are: Ru−PPh3=2.418(4) Å and 2.429(4) Å, Ru−NO2=2.063(12) Å, Ru−N(trpy, outer)=2.100(12) Å and 2.116(12) Å and Ru−N(trpy, central)=2.004(11) Å.

Crystal structure ofcis-[Ru(bpy)2{PPh2(o-tol)}Cl][ClO4]·1.5(CH2Cl2), a structure containing both ordered and disordered dichloromethane molecules of crystallization

The complexcis-[Ru(bpy)2 {PPh2(o-tol)}Cl][ClO4] crystallizes from dichloromethane as the sesqui-dichloromethane solvate. The complex crystallizes in the monoclinic space group P21/n with Z=4. The structure was refined toR=5.50% for those 2552 independent reflections with |F0|>6σ(|F0|) The octahedral Ru(II) cation is associated with the following bond lengths: Ru-PPh2(o-tol)=2.360(3)Å. Ru−Cl=2.433(2)Å and Ru−N(bpy)=2.041(8)–2.095(8)Å. Both the perchlorate anion and the dichloromethane molecules of solvation exhibit large amplitudes of vibration. One dichloromethane molecule lies in a general position, the other lies about an inversion center and suffers from disorder.

Synthesis ofcis-[Ru{4,4′-(t-Bu)2bpy}2(PPh3)Cl+][ClO 4 − ] and the crystal structure of its disordered hemiacetonitrile, hemitoluene solvate

AbstractThe complexcis-[Ru{4,4′-(t-Bu)2bpy}2(PPh3)Cl+][ClO4−·0.5(toluene)·0.5(MeCN), where 4,4′-(t-Bu)2bpy=4,4′-di(t-butyl)-2,2′-bipyridyl crystallizes with an ordered racemic mixture of the chiral cations in the centrosymmetric triclinic space group

X-ray diffraction studies oncis-[Ru(bpy)2(PMe3)Cl+][ClO4 −] andcis-[Ru(bpy)2{PMe2(o-tol)}Cl+][ClO4 −]; two ordered structures in thecis-bis(bipyridyl)chloro(phosphine)-ruthenium(II) series

P\bar 1

Crystal and molecular structure of di(1-pyrazolyl)methane, CH2(C3N2H3)2

(No. 2). The structure was refined toR=4.42% for those 6426 reflections with 20=5–50o and |Fo|>6σ(F). Ruthenium ligand distances are Ru−Cl=2.423(2)Å, Ru−PPh3=2.346(2)Å and Ru−N=2.056(4)–2.098(4)Å. Both the Ru(II)-containing cation and the perchlorate anion are ordered, but the toluene and acetonitrile exhibit an interesting type of scrambled disorder about the inversion center atx=1,y=1/2,z=0.

Heat-Treatment of Synthetic Graphite under Argon and Effect on Li-Ion Electrochemistry

AbstractThe complexcis-[Ru(bpy)2(PPh3)Cl+][ClO4−] (where bpy=2,2′-bipyridyl) crystallizes from a solution in toluene/dichloromethane as the toluene-hemi(dichloromethane) solvate in the centrosymmetric space group