Crystal and molecular structure of bis(2-isotropyliminomethinylphenyl) telluride

Scientific-Research Institute of Physical and Organic Chemistry, Rostov State University. A. N. Nesmeyanov Institute of Heteroorganic Compounds, Academy of Sciences of the USSR. Translated from Zhurnal Strukturnoi Khimii, Vol. 32, No. 3, pp. 104–106, May–June, 1991.     

Crystal and molecular structure of the ethanol solvate of 2-[bis(diphenylphosphoryl)methyl]phenol

Crystal and molecular structure of the ethanol solvate of 2-[bis(diphenylphosphoryl)methyl]phenol, C₃₁H₂₆O₃P₂·3/4 C₂H₅OH (I), was determined by X-ray diffraction analysis. Crystals I are monoclinic: a=11.896(3), b=17.207(3), c=28.421(6) Å, β=90.75(2)°, Z=8, space group P2₁/c. The structure of I was solved by direct methods and refined anisotropically by large-block least-squares analysis to R=0.066 (CAD-4 automatic diffractometer, λMoK_α radiation, 3650 independent reflections with I≥3σ). The crystal structure of I contains two independent molecules, Ia and Ib, of the basic substance and two independent solvate molecules of ethanol. The P atoms in molecules Ia and Ib have distorted tetrahedral environments; the average bond lengths are: P=O 1.476(3), P-C(sp³)=1.833(4) and P-C(Ar)=1.809(4) Å. Molecule Ia has an approximate symmetry plane C_s. The conformation of molecule Ib differs from that of Ia in rotation of one diphenylphosphoryl substituent around the P-C(sp³) bond by an angle of ≈34°. In molecule Ia, the O=P-C-P=O fragment has the form of a chela with two nearly parallel P=O bonds. In the crystal structure of I there are O-H...O=P intermolecular H-bonds; in molecules Ia and Ib there is an intramolecular H-bond of C-H...OH type.     

Crystal structure, spectroscopic, magnetic and theoretical studies of [bis(hippurato)bis(benzimidazole)copper(II)] propanol 1/4hydrate

The novel ternary complex [Cu(hipp)₂(bim)₂]·PrOH·0.25H₂O (1) has been prepared and fully characterised by single crystal X-ray structure determination. The central copper(II) is coordinated by two O-donor atoms of the hippurate ions and by two N-atoms of the benzimidazole ligand with a tetrahedrally distorted square-planar geometry. The complex molecules, connected by hydrogen bonds into a 2D network, form a supramolecular structure. A theoretical DFT calculation performed by the UB3LYP method combined with the LanL2DZ basis set shows that all metal-ligand bonds are of the L → M type. The results of the spectroscopic, EPR and NIR–Vis–UV, as well as magnetic study are consistent with the structural data.     

Pyrimidine-containing poly[bis(itaconimides)]

Heat-resistant pyrimidine-containing poly[bis(itaconimides)] with a glass transition temperature of 240–250°C were synthesized via the polyaddition reaction. The film materials based on a pyrimidine-containing poly[bis(itaconimide)] and an aromatic polybenzimidazole acquired good electric and mechanical characteristics after doping with phosphoric acid.     

Crystal and molecular structure of two monoclinic forms of tricarbonyldiiodo[bis(dimethylphosphine)ethane]-tungsten(II)

There are two monoclinic crystal forms of the title compound. In the first, a 11.701(6), b 15.680(9), c 9.316(5) Å, β 95.36(5)°, Z 4, with 1 molecule in the asymmetric unit, spacegroup P2₁/n. In the second, a 25.772(14), b 15.514(13), c 17.432(14) Å, β 91.59(8)°, Z 16, with 4 molecules in the asymmetric unit, spacegroup P2₁/a. In this latter form crystals were twinned with hk0 common. Both structures were solved by Patterson and Fourier methods from diffractometer data and refined by least squares methods to R 0.072 for 2226 independent reflections and to R 0.063 for 3250 independent reflections respectively. The five independent molecules are seven-coordinate monomers with similar geometries, all are distorted capped octahedra with a carbonyl group in the capping position, two carbonyl groups and a phosphorus atom in the capped face and two iodine atoms and a phosphorus atom in the uncapped face. Bond lengths are compatible with values found in similar structures. In all molecules, the two WP bond lengths differ by about 0.06 Å, the longer bond being to the phosphorus atom in the uncapped face which is trans to a carbonyl group.     

The crystal and molecular structure of oxo-bis[tribenzylsilicon(IV)]

Crystals of oxo-bis[tribenzylsilicon(IV)], O[(PhCH₂)₃Si]₂, are triclinic, space group P$\text{1}$, with a = 9.780(7), b = 9.938(9), c = 10.283(6) Å, α = 93.35(1), β = overall symmetry close to $\text{3}$: the SiOSi skeleton is strictly linear with SiO = 1.613(4) Å. The conformations of molecules and ions isoelectronic with O[(PhCH₂)₃Si]₂ are compared and discussed.     

The crystal and molecular structure of oxo-bis[tribenzylgermanium(IV)]

Crystals of oxo-bis[tribenzylgermanium(IV)], O[(PhCH₂)₃Ge]₂, are rhombohedral, space group R$\text{3}$, having a = 9.621(2) Å, α = 85.48(3)°. The structure was solved by Patterson methods using diffractometer data and refined by full-matrix least squares to R = 0.0876. The structure consists of molecules lying along the 3-fold axis of the unit cell, in which the GeOGe fragments are strictly linear and centrosymmetric. The GeO distance is 1.730(1) Å and the GeC distance is 1.980(5) Å.