The present research work reports the study on crystal structure, vibrational spectroscopy and thermal analysis of organic-inorganic hybrid compound (C6H5(CH2)2NH3)2CdCl4. Single crystals of bis(phenethylammonium)tetrachlorocadmate (C6H5(CH2)2NH3)2CdCl4 (PEA-Cd) were obtained by diffusion at room temperature. This compound crystallizes in the orthorhombic space group C 2 cb with unit cell parameters a = 7.4444(2) Å, b = 38.8965(3) Å, c = 7.3737(2) Å and Z = 4. Single crystal structure has been solved and refined to R = 0.036 and wR = 0.092. The structure consists of an extended [CdCl4]2- network and two [C6H5(CH2)2NH3]+ cations to form a two-dimensional perovskite system. The infrared (IR) spectrum of the title compound was recorded at room temperature. Differential scanning calorimetry (DSC) was used to investigate the phase transition; this compound exhibits a reversible single solid-solid phase transition.
B. Liu1, Z.-H. Zhang2, L. Xu1,2, H. Jiao2 1Shaanxi University of Sciences and Technology, Xi'an, Shaanxi, P. R. China 2Shaanxi Normal University, Xi'an, Shaanxi, P. R. China
Keywords: crystal structure, fluorescence, 2-carboxyethyl(phenyl)phosphinic acid, TGA, topology
Hydrothermal syntheses of 2-carboxyethyl(phenyl)phosphinic acid (H2CEPPA) with Bi(NO3)3 and Cd(NO3)2 produce two layered complexes [Bi2(μ3-O)(CEPPA)2] n (1) and [Cd(HCEPPA)2] n (2). Compound 1 is comprised of [Bi4(m3-O)2(POO)4(COO)4] SBUs which grow into a double wave-like 2D layer with -CH2CH2- spacers. Compound 2 crystallizes in the orthorhombic noncentrosymmetric space group Pca 21, exhibiting a double lattice-like layer. Through edge-to-face d ⋯π stacking, a 3D supramolecular framework is formed based on 2D lattices. Topological analyses indicate that 1 and 2 have sql (or Shubnikov tetragonal plane net) and kgd (or Shubnikov (3.6.3.6) plane net) topological networks respectively. 1 and 2 are isolated as single crystal pure phases, which is confirmed by powder XRD. TGA shows high thermal stabilities with decomposition temperatures of 1 and 2 being 373 and 303 °C respectively. The fluorescent spectra exhibit fluorescence quenching in 1 and sharp emission at 292 nm in 2, which is assigned to intraligand emission.
E.E. Netreba1, E.A. Sarnit1, S.V. Shabanov1, A.A. Velikozhon1, N.V. Somov2 1Taurida Academy of Vernadsky Crimean Federal University, Simferopol, Russia 2Lobachevsky State University, Nizhny Novgorod, Russia
Keywords: бициклические бисмочевины, мебикар, европий(III), структура, десятивершинник, ИК, РСА, bicyclic bisureas, mebicar, europium(III), structure, 10-vertex polyhedron, IR, single crystal XRD
A centrosymmetric binuclear complex of europium(III) nitrate with bicyclic bisurea (2,4,6,8-tetramethyl-2,4,6,8-tetraazabicyclo(3.3.0)octane-3,7-dione, or mebicar, Mk) [Eu(C8H14N4O2)(H2O)2(NO3)3]2 (I) is synthesized and its atomic structure (CIF file CCDC No. 1451437) is determined. The crystals of I are triclinic: space group P , a = 9.8343(4) Å , b = 10.2544(4) Å, c = 10.9411(4) Å, a= 74.366(3)°, = 67.734(4)°, b= 67.673(4)°, V = 934.32(7) Å3, ρ(calc.) = 2.03398 g/cm3, Z = 1. The europium atom is coordinated by two oxygen atoms of two Mk molecules connected by a symmetry operation, three bidentate nitrate anions, and two water molecules. The coordination polyhedron of the europium atom is a 10-vertex polyhedron, the Eu…Eu distance is 9.7433(6) .
Z. G. Aliev, I. N. Zyuzin, S. M. Aldoshin
Institute of Problems of Chemical Physics, Russian Academy of Sciences, Chernogolovka, Russia
Keywords: алкокси-NNO-азоксисоединения, алкил-ONN-азокси-оксисоединения, 1,2-бис(метил-ONN-азокси-окси)этан, кристаллическая структура, гош-конформация, alkoxy-NNO-azoxy compounds, alkyl-ONN-azoxy-oxy compounds, 1,2-bis(methyl-ONN-azoxy-oxy) ethane, crystal structure, gauche conformation
The molecular and crystal structure of 1,2-bis(methyl-ONN-azoxy-oxy)ethane is studied. Its molecule has a gauche conformation with respect to the С-С bond with a torsion angle of 71.4°.
The reaction of 2,4-diacetyl-5-hydroxy-5-methyl-3-phenylcyclohexanone-1 with phenylhydrazine is conducted, and the crystal structures of its products, 1-(6-hydroxy-3,6-dimethyl)-2,4-diphenyl-4,5,6,7-tetrahydro-2H-indazol-5-yl)ethane-1-one and 1-(2-hydroxy-2-methyl-6-phenyl-4-(2-phenylhydrazono)-5-(1-(2-henylhydrazono)ethyl)cyclohexyl)ethane-1-one, are determined by single crystal XRD.
S.A. Poluyanov1, F.V. Tuzikov1, Yu.V. Larichev1,2, S.V. Tsybulya1,2 1Boreskov Institute of Catalysis, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia 2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: малоугловое рентгеновское рассеяние, обработка данных, минимизация, наноразмерные системы, small-angle X-ray scattering, data processing, minimization, nanosized systems
New approaches to the small-angle scattering data analysis for nanosized systems are presented. They are based on the application of optimization methods and a repeated solution of direct problems. Based on the new approaches the program is developed which makes it possible to simulate small-angle X-ray diffraction data, to introduce collimation corrections, and to analyze the disperse composition of samples. Results of the program performance are demonstrated for a series of typical nanosized systems (sols, catalysts) and the program is compared with the available programs for small-angle data processing.
T.V. Rybalova1,2, Yu.V. Gatilov1,2, Ya.V. Zonov1,2, V.M. Karpov1 1Vorozhtsov Institute of Organic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia 2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: 3-гидрокси-перфтор-3-алкилфталиды, рентгеноструктурный анализ, межмолекулярные взаимодействия, квантово-химические расчеты, супрамолекулярная архитектура, полиморфы, 3-hydroxyperfluoro-3-alkylphthalides, single crystal X-ray diffraction study, intermolecular interactions, quantum chemical calculations, supramolecular architecture, polymorphs
The molecular and crystal structures of perfluoro-3-alkylphthalides (3-hydroxyperfluoro-3-methylphthalide and its hydrate, two polymorps of 3-hydroxyperfluoro-3-ethylphthalide and 3-hydroxyperfluoro-3-isopropylphthalide) are determined by single crystal X-ray diffraction. In the crystals, the supramolecular O-Н…O=C synthon occurs leading, except for the crystallohydrate, to the formation of hydrogen bonded chains (6) (supramolecular 1D motifs). According to the DFT/M06-2X/TZV calculations, the interaction energy of hydrogen bonded molecular pairs increases in this series, which can be explained by the additional C=O…π, O…π and C-F…π interactions.
A new titanium complex [Ti(Me-Q)2(Cl)2] (1) is prepared by reacting titanium tetrachloride with 2-methyl-8-hydroxyquinoline in a fast and facile process. The complex is fully characterized based on its 1H and 13C NMR, IR, and UV spectra and elemental analysis. The prepared nanostructured compound is synthesized by the sonochemical method. This new nanostructure is characterized by scanning electron microscopy (SEM), powder X-ray diffraction (XRD), IR spectroscopy, and elemental analysis. Thermal stability of single crystalline and nanosize samples of the prepared compound is studied by thermal gravimetric (TG) and differential thermal analysis (DTA). The prepared complexes both bulk and nanosized are utilized as a precursor for the preparation of TiO2 nanoparticles by direct thermal decomposition at 600 °C in air. The morphology and size of TiO2 nanoparticles are determined by SEM, powder XRD, and IR spectroscopy and the results show that the TiO2 nanoparticle size depends on the initial particle size of 1. Photoluminescence (PL) properties of the nanostructured and crystalline bulk prepared complex and their TiO2 nanoparticle cores are investigated.
The structures of solid phases of water and IV(b) group elements of the periodic table (carbon, silicon, germanium, and tin) are compared. Both water and mentioned elements are characterized by high polymorphism. All mentioned elements and ice have a modification with a diamond structure. For all substances considered, except tin, modifications with the structure of a hexagonal analogue of diamond (lonsdaleite) have been known. The modification with the β-Sn structure has not been known only for ice and carbon. One of the germanium modifications is isostructural to ice III. Tin has a modification with the α-Fe structure. The same structure is observed for ices VII, VIII, and X. Both water and IVb group elements can form clathrate hydrates with cavities in the form of Allen's polyhedra. In water clathrates these cavities contain noble gas atoms (Ar, Kr, Xe) and various molecules. Clathrates of IVb group elements contain metal atoms as well as noble gas atoms.
V.V. Bannikov, I.R. Shein
Institute of Solid State Chemistry, Ural Branch, Russian Academy of Sciences, Ekaterinburg, Russia
Keywords: 1111 фазы, нестехиометрия, ab initio моделирование, 1111 phases, non-stoichiometry, ab initio simulation
Features of the electronic structure of layered LaZnAsO1- δ phases with the ZrCuSiAs structure type at δ = 0.11 and 0.44 are briefly discussed based on the results of ab initio calculations. It is shown that the effect of oxygen vacancies on the electronic structure of non-stoichiometric phases is equivalent to the effect of an electron dopant and the charge compensation occurs inside [La-O] structural blocks due to a change in the population of lanthanum atomic states.
