X-ray structure studies have been carried out on single crystals of 4,4'-dichlorobenzophenone at temperatures from 164 to 295 K. The structure determined at 164 K is monoclinic I2/c. Crystal data: T = 164 K; a = 24.527 (6), b = 6.064 (1), c = 7.457 (4) Å; beta = 100.10 (2) degrees; V = 1091.9 (6) Å(3); Z = 4; d(c) = 1.528 g cm(-3); lambda(Mo Kalpha) = 0.71073 Å; µ = 0.565 mm(-1); F(000) = 512; R = 0.04. The temperature dependence of the unit-cell parameters and of the intensities of some symmetry-sensitive reflections has been measured over the range 164-293 K, both in warm-up and cool-down experiments. It has been established that the phase transformation between the C2/c and I2/c structures occurs as a sequence of two closely spaced first-order phase transitions. In between these phase transitions the crystal is in an intermediate state whose structure is different from both C2/c and I2/c. The experimental data give us ground to suppose that the intermediate state is disordered, having a primitive cell half as large as in the two ordered phases. Within the temperature interval where the said intermediate state exists the thermal expansivity along axis c is negative.
Intercalation of C 60 single crystals with helium was studied by powder x-ray diffractometry. It was established that the intercalation is a two-stage process, octahedral cavities are filled first and then tetrahedral ones, the chemical pressure being negative during both stages. For the first time low-temperature (5 K) photoluminescence spectra of helium-intercalated fullerite C 60 were studied. The presence of helium in lattice voids was shown to reduce that part of the luminescent intensity which is due to the emission of covalently bound pairs of C 60 molecules, the so-called «deep traps» with the 0-0 transition energy close to 1.69 eV. The mechanism of the effect of the intercalation with helium on the pair formation in fullerite C 60 is discussed.
A combination of single-crystal and powder X-ray diffractometry was used to study the structure of two polymorphs of 4-bromobenzophenone over the temperature range from 100 to 300 K. One of the polymorphs of the title compound was known previously and its structure has been determined at room temperature [Ebbinghaus et al. (1997). Z. Kristallogr. 212, 339-340]. Two crystal growth methods were employed, one of which (a modification of the Bridgman-Stockbarger technique) resulted in single crystals of a previously unknown structure. The basic physical properties of the stable polymorph are: growth method, from 2-propanol solutions or gradient sublimation; space group, monoclinic P2(1)/c; melting point, T(m) = 355.2 K; X-ray density (at 100 K), D(x) = 1.646 g cm(-3). The same properties of the metastable polymorph (triclinic P\overline 1 ) are: growth method, modified Bridgman-Stockbarger method; X-ray density (at 100 K), D(x) = 1.645 g cm(-3); T(m) = 354 K. Thermograms suggest that the melting of the metastable form is accompanied by at least a partial crystallization presumably into the monoclinic form; the transformation is therefore monotropic. Analysis of short distances in both polymorphs shows that numerous weak hydrogen bonds of the C-H...pi type ensure additional stabilization within the respective planes normal to the longest dimension of the molecules. The strong temperature dependence of the lattice constants and of the weak bond distances in the monoclinic form suggest that the weak bond interactions might be responsible for both the large thermal expansion within plane bc and the considerable thermal expansion anisotropy.
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