Band 234, Heft 10

The Ga/In phase width ( y ) and the distribution of the two triels within the polyanions of known binary ( x  = 1, 2) and new ternary ‘intermediate’ ( x  = 1–2) alkali trielides A x (Ga 1− y In y ) 3 ( A  = K, Rb, Cs) was investigated in a synthetic (slow cooling of the melts of the three elements), crystallographic (X-ray single crystal) and bond theoretical (FP-LAPW DFT bandstructure calculation) study. The Cs 2 In 3 -type structure ( x  = 2, series A , tetragonal, I  4/ mmm ) exhibits layers of four-connected closo octahedra [ M 6 ] 4− . Ternary K compounds of this type were yielded within a large range ( y  = 0–0.87), whereas isotypic Rb/Cs trielides exist only at higher In contents (>52/69%). Geometric criteria determine not only the Ga/In stability ranges but also the occurrence of a commensurate superstructure at approx. 33% In (K 2 Ga 2.17 In 0.83 : P  4 2 / ncm , a  = 879.83(4), c  = 1557.66(10) pm, R  1 = 0.0887), in which the octahedra are slightly tilted against the layers. Cesium compounds of the RbGa 3 -type structure ( x  = 1, C , tetragonal, I  4̅ m 2), which exhibits a 3D network of all- exo bonded closo dodecahedra [ M 8 ] 2− and four-bonded M − anions, are stable throughout the whole substitutional range CsGa 3 –CsIn 3 . The maximum possible In content increases with increasing size of A + (Cs: 100%, Rb: 30%, K: 8% In). The similarities between these two tetragonal structures are consistent with the occurrence of two new structure types of ‘intermediate’ compounds A 7 M 15 ( x  = 1.4, 1 B / 2 B ), which differ in the stacking sequences of double layers of novel six-fold exo -bonded pentagonal bipyramidal closo clusters [ M 7 ] 3− connected via four-bonded M − (e.g. 1 B : Cs 7 Ga 8.4 In 6.6 , P  4̅ m 2, a  = 656.23(3), c  = 1616.0(1) pm, R  1 = 0.0742; 2 B : Rb 7 Ga 8.1 In 6.9 , P  4 2 / nmc , a  = 665.64(2), c  = 3140.9(2) pm, R  1 = 0.0720). The Rb/Cs compounds of these types are only stable in a limited Ga/In region and with a distinct Ga/In distribution within the [ M 7 ] clusters. According to the close relation between the structures A , B and C , the structure family is characterised by the occurrence of stacking faults and diffuse scattering, indicating the existence of further members of this series. The new compound Cs 5 Ga 3.1 In 5.9 ( x  = 1.667, P  4̅ m 2, a  = 654.62(2), c  = 3281.5(2) pm, R  1 = 0.1005) is a reasonably periodically ordered stacking variant containing layers A and double layers B in parallel.

Nickel oxide thin films have been prepared by sol-gel dip-coating technique on glass substrate. It is shown that nickel oxide thin films have poly crystalline nature. Nickel oxide thin films exhibit high transmission (39–85%) in the wavelength range of 400–900 nm, strong absorption between 300 and 400 nm wavelengths and decrease of band gap values are in the range 3.69–3.27 eV with increase of withdrawal speed. High band gap at low withdrawal speed is because of the small average crystallite size, which decreases with increase in withdrawal speed. The SEM micrograph shows cubic crystallites and surface of thin films become dense, smooth and homogeneous with an increase in withdrawal speed. Assessment of nickel oxide deposition conditions provides gateway for effective and cheap solar cells.

A dihydropyrimidine (DHPM) derivative was synthesized, characterized by X-ray diffraction and searched in silico for its inhibitory activities against AccD5 enzyme, the CT domain of a Mycobacterium tuberculosis ACCase. Its molecular structure was compared to another DHPM derivative (DHPM II ). The results have shown that the (±)2,6-methano-4-thioxo-3,4,5,6-tetrahydro-2H-[1,3,5] benzoxadiazocines (DHPM I) and (±)2,6-methano-4-oxo-3,4,5,6-tetrahydro-2H-[1,3,5] benzoxadiazocines (DHPM II) belong to the monoclinic and triclinic systems, respectively, and their crystal structures are stabilized by N–H⋯O, O–H⋯O and N–H⋯S interactions. The DHPM derivatives established hydrogen bond interactions with the oxyanion-stabilizing residues (Gly-434/Ala-435) beyond the Thr-217, Phe-394 and Ile-216 in the biotin pocket. The predicted MoB of the DHPM derivatives (21R, 24S, 22R) configuration showed that its phenyl moiety was positioned on the interface between the biotin and propionyl-CoA pockets, suggesting a possible blockade of both subsites. Additionally, the hydrogen bonds involving the O-bridged phenyl ring of the DHPM derivatives (21S, 24R, 22S) configuration with Gly434 in the oxyanion-stabilizing region placed its phenyl moiety in the bottom of the biotin pocket establishing hydrophobic interactions with Leu164, Tyr167, Val459 and Ala155. These results indicate the DHPM derivatives as potential AccD5 inhibitors and promising starting points for future optimizations. Although the overlap of DHPM I and DHPM II did not present significant differences, the exchange of a sulfur atom for an oxygen atom increased the predicted biological potential.

Androsta-1,4-dien-17β-ol-3-one, also known as boldenone, is an anabolic-androgenic steroid derived from testosterone. The crystal structures of boldenone base, boldenone acetate, boldenone propionate, boldenone cypionate and a boldenone acetate polymorph obtained by high throughput screening were investigated. Hirshfeld surfaces and fingerprint plots breakdown revealed that the molecular packing in the crystals are driven by dominant H⋯H intermolecular contacts, followed by O⋯H/H⋯O contacts and to a lesser degree C⋯H/H⋯C contacts. The steroid skeleton rings, for all the reported compounds, adopt the following conformation: planar in A, chair in B and C, whereas C(13) envelope conformations are found for the five-membered D rings. The total lattice energies were calculated as a sum of four terms (Coulombic, polarization, dispersion, repulsion).

Three chlorinated theinyl chalcone derivatives, namely ( E )-1-(5-chlorothiophen-2-yl)-3-(4-(methylthio)phenyl)prop-2-en-1-one ( I ), ( E )-1-(5-chlorothiophen-2-yl)-3-(4-(dimethylamino)phenyl)prop-2-en-1-one ( II ) and ( E )-1-(5-chlorothiophen-2-yl)-3-(2,3-dihydrobenzofuran-5-yl)prop-2-en-1-one ( III ), were synthesized and their crystal structures were determined by single-crystal X-ray diffraction analysis. Compounds I , II and III crystallize in the monoclinic space groups P  2 1 / c (centrosymmetric), P  2 1 / n (centrosymmetric) and Pc (non-centrosymmetric), respectively. In all three compounds, the molecules are in a relatively planar conformation and adopt a trans configuration with respect to the C=C double bond. The crystal packings are stabilized by weak hydrogen-bonds, π · · · π, C–H · · · π and C–Cl · · · π interactions. The intermolecular contacts and lattice energies were further analyzed by Hirshfeld surface analysis. The third-order nonlinear optical properties of these chalcone derivatives were investigated using the single beam Z-scan technique with a 5 mW continuous wave diode laser operating at 635 nm, where compound I showed the highest potential for optical application with its exclusive nonlinear refractive index and nonlinear susceptibility.