Bernard Marciniak

Crystal Structure of a Metastable Anthracene Modification, Grown from the Vapor Phase

The crystal structure of a new monoclinic metastable phase of anthracene formed during vapor growth has been determined from single crystal X-ray data (DARCH-1 automatic diffractometer, Mo K α radiation). This metastable anthracene phase crystallizes in the monoclinic space group P2 1 /n with a =8.553(2), b =6.021(1), c =22.334(4), Å and β=124.54(3)°, and four molecules per unit cell. All carbon and hydrogen atom positions have been determined and refined to R=0.044 for 330 unique reflections.

5-(N,N-Diethyl­amino)-4,6-diphenyl-1,2,3-triazine

In the title compound, C19H20N4, the dihedral angles formed by the planes of the triazine ring and the two phenyl substituents are 51.54 (1) and 49.27 (1)°. The phenyl rings form a dihedral angle of 80.81 (1)°. All bond lengths and angles are normal. The structure is stabilized by van der Waals interactions.

Novel multistage zone refiner for purification of organic materials

A novel, large scale, laboratory zone refiner for purification of organic materials is described. The device can operate in continuous mode and makes it easy to operate the temperature and the passing rate of the molten zones at wide-ranges. At the constant rate of molten zone it can be possible to purify of five different materials. High-purity naphthalene, acenaphthene and fluoranthene were obtained by using this zone refiner.

Morphology and x-ray characterization of acenaphthene, fluoranthene, and pyrene crystals grown by sublimation

The preparation of relatively large of acenaphthene, fluoranthene and pyrene crystals grown from vapor phase by plate sublimation method, is described. In order to characterize the intrinsic structure perfection of such grown crystals the X-ray examinations have been performed. The observed morphologies of these crystals have been compared with that predicted from PBC theory by Hartman-Perdok, model growth conditions (vacuum, temperature gradient) effect have been assessed.

Purity and zone refining of some coal-tar aromatic hydrocarbons

Impurities present in commercially available naphthalene, fluoranthene and anthracene have been concentrated by zone melting and further evaporation of their extracts in chloroform, and identified by gas chromatography performed on CGC-FID and CGC-MS apparatuses. Quantitative contents of fourteen, eight and twelve impurities detected in naphthalene, fluoranthene and anthracene, respectively, have also been determined.

Solubility and thermodynamical properties of some growth solutions of fluoranthene

The solubility of fluoranthene in some halogen derivative organic solvents has been determined experimentally. These results have been correlated by using the classical equation for solid-liquid solubility and the obtained experimental activity coefficients have been compared to the values predicted on the basis of the regular solution theory. The best solubility correlation has been obtained with the extended regular solution theory. Thermodynamical characterization of the considered solutions is also given.

Optimalization of growth solution volume for investigations of growth and nucleation processes

Influence of the growth solution volume on the values of the metastable zone width ((Delta) TMET), the induction period ((tau) ), and the shape of the crystals has been determined experimentally. The growth solution of naphthalene-1,2-dichloroethane (1,2- dCHLE) was chosen as the model one. The errors due to the evaporation of the solvent were eliminated as the special procedure of measurements was used.

6-(3-Iodo­propyl)­benzo­[f][1,7]­naphthyridin-6-ium iodide

In the title compound, C15H14IN2+·I−, the C15H14IN2+ cations and I− anions are joined together via strong C—H⋯I hydrogen bonds. In the [010] direction, these cations form positively charged columns, between which the I− anions are included.

Morphology of New (P2 1 /n) Metastable Anthracene Modification Crystals, Grown from the Vapor Phase

The morphology of the vapor-grown crystals of a new metastable anthracene modification (that crystallizes in the monoclinic space group P2 1 /n with a =8.553(2), b =6.021(1), c =22.334(4) Å, β=124.54(3)°, and four molecules per unit cell) was determined from the X-ray single crystal orientation data and optical reflection goniometry measurements. In the standard space group P2 1 /c, the crystals of this new phase possessed a rhomboidal tabular habit with two major {002} faces oriented in [001] direction, and twelve lateral faces of {11 \bar{3} }, {111}, {100}, and {102}. This morphology differs nearly fully from that observed for the crystals of a long-known parent anthracene phase (P2 1 /a) grown under the same conditions. The experimental morphologies of both crystal phases were compared with those predicted from the periodic band chain (PBC) theory of Hartman and Perdok. Moreover, the melting point for this new metastable anthracene phase, equal to 215.1°C, was determined with help of a differential scanning calorimeter.

Solvent effects on morphology and crystal structure of solution-grown organic crystals

Based on the measured solubility data of acenaphthene, fluoranthene and pyrene in six halogen derivative solvents, the solutes activity coefficients ((gamma) s) have been determined from Scatchard-Hildebrand solution theory and used as a measure of solute-solvent interactions for determination of observed solvent effect on growth morphology and intrinsic structure of solution grown crystals of these hydrocarbons. The growth morphologies of these crystals have been interpreted on the basis of PBC theory assumptions. Correlation between activity coefficients of the investigated solutes and morphology as well as structure of obtained crystals, are found.