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2013 year, number 6

1.
Description of spin-crossover in a heterogeneous chain of exchangE clusterS

V. A. Morozov
International Tomography Center, Siberian Division, Russian Academy of Sciences, Novosibirsk
Keywords: molecular magnetics, exchange cluster, spin-crossover, effective magnetic moment

Abstract >>
Spin transition theory is developed for periodic chains with two and more exchange clusters in a unit cell. A general expression is obtained for the effective magnetic moment of a unit cell μeff with several exchange clusters. For heterospin complexes Cu(hfac)2LR characterized by chains with the head-to-head motif a two-site approximation for the statistical sum of the Cu2+ Jahn – Teller paramagnetic center Cu2+ with spin 1/2 is proposed, within which a comparison with the available experimental data is performed. It is shown that the model developed describes both smooth and abrupt (cooperative) spin-crossover cases for the chains of three-spin exchange clusters.



2.
ELECTRONIC STRUCTURE AND RELATED PROPERTIES FOR QUASI-BINARY (GaP)1– x(ZnSe)x CRYSTALS

W. Kara Mohamed1, F. Mezrag2, M. Boucenna2, N. Bouarissa3,4
1University of Bordj-Bou-Arreridj, El-Anasser, Bordj-Bou-Arreridj, Algeria
2University of M'sila, M'sila, Algeria
3College of Science and Arts Najran University, Najran, Saudi Arabia
4Centre for Advanced Materials and Nano-Engineering (CAMNE) Najran University, Najran, Saudi Arabia
Keywords: electronic structure, optical properties, quasi-crystals, pseudopotentials

Abstract >>
The results of pseudopotential calculations of the band structure and related electronic and optical properties of quasi-binary (GaP)1– x(ZnSe)x crystals in the zinc blende structure are presented. Trends in bonding and ionicity are discussed in terms of electronic charge densities. Moreover, the composition dependence of the refractive index and dielectric constants are reported. The computed values are in reasonable agreement with experimental data. The results suggest that for a proper choice of the composition x , (GaP)1 x(ZnSe)x could provide more diverse opportunities to achieve the desired electronic and optical properties of the crystals which would improve the performances of devices fabricated on them.



3.
INSIGHT INTO THE CHEMICAL BONDING AND ELECTROSTATIC POTENTIAL: A CHARGE DENSITY STUDY ON A QUINAZOLINE DERIVATIVE

A. Tojiboev1, R. Wang2, F. Pan2, U. Englert2, K. Turgunov3, R. Okmanov3
1Namangan State University, Namangan, Uzbekistan
2Institute of Inorganic Chemistry, RWTH Aachen University, Landoltweg 1, Aachen, Germany
3S.Yunusov Institute of the Chemistry of Plant Substances, Academy of Sciences Uzbekistan, Tashkent, Uzbekistan
Keywords: quinazoline, electronic structure, high-resolution X-ray diffraction, charge density, topological analysis, dipole moment

Abstract >>
2,3-Trimethylene-3,4-dihydroquinazoline shares the heterocyclic core with natural compounds and synthetic drugs. The hydrochloride of the compound forms excellent dihydrate crystals which have allowed us to collect high-resolution X-ray diffraction data and obtain the experimental charge density. The solid may be understood as built up from pairs of heterocyclic cations and chloride anions; a direct hydrogen bond links the halide to the formally cationic pyrimidine NH group. The hydrate water molecules interact with the anions, forming an infinite chain along the crystallographic a axis between the stacks of the heterocyclic cations. Based on the experimental charge density, a dipole moment of 16.1 Debye is calculated for a pair of the hydrogen-bonded quinazolinium cation and the chloride anion in the extended crystal structure.



4.
THEORETICAL STUDY OF HYDROPHOBICITY AND HYDROPHILICITY OF INDOLE, SKATOLE, AND ETHANOLE

G. N. Ten1, A. A. Yakovleva1, V. I. Baranov2
1N. G. Chernyshevsky Saratov State University, Saratov
2V. I. Vernadsky Institute of Geochemistry and Analytical Chemistry, Russian Academy of Sciences, Moscow
Keywords: indole, skatole, ethanole, complexes with water, hydrophobicity, geometric parameters of the hydrogen bridge, stretching vibrational frequencies

Abstract >>
The structures of indole, skatole, and ethanole complexes with water molecules are calculated by the DFT method. Radial and angular dependences of hydrogen bridge parameters on the number of water molecules are analyzed. Two models are determined which enable the study of the reason for the hydrophobicity of indole and skatole. Frequencies and intensities of absorption bands corresponding to stretching vibrations of the NH bond of indole, skatole, and ethanol in complexes with water are compared. It is shown that the main reason for the domination of the hydrophobic component over the hydrophilic one is the taking into account of the interaction of water molecules with the aromatic system of indole and skatole, finally resulting in a substantial decrease in the HB strength.



5.
Intramolecular hydrogen BOND –ͷN in 1,1'-divinyl-2,2'-diimidazolyl According to the data of b initio calculations and QTAIM analysis

A. V. Vashchenko, A. V. Afonin
A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Division, Russian Academy of Sciences, Irkutsk
Keywords: intramolecular hydrogen bonds іHN, ab initio calculation, QTAIM, RDG analysis

Abstract >>
By non-empirical ab initio quantum chemical calculation the spatial structure of 1,1'-divinyl-2,2'-diimidazolyl is determined and the formation of intramolecular hydrogen bonds of the –H·N type in it is established. It is evidenced by energy preference for the conformation in which there is a short contact between the α-proton of the vinyl group and the endocyclic nitrogen atom (2.28 Å), creating favorable conditions for the formation of a six-membered chelate cycle. An analysis of the topological characteristics of the electron density and the reduced electron density gradient also give evidence in favor of the formation of a weak intramolecular hydrogen bond CHN. The estimation of the hydrogen bond energy by the Espinosa method results in a value below 3 kcal/mol.



6.
Synthesis of mesoporous bimetallic PtSn catalytic coatings from polynuclear precursors for fine organic synthesis processes

L. B. Okhlopkova1, E. V. Matus1, I. Z. Ismagilov1, M. A. Kerzhentsev1, I. P. Prosvirin1, Z. R. Ismagilov2
1G. K. Boreskov Institute of Catalysis, Siberian Division, Russian Academy of Sciences, Novosibirsk
2Institute of Coal Chemistry and Chemical Materials Science, Siberian Division, Russian Academy of Sciences, Kemerovo
Keywords: capillary microreactors, nanostructured catalysts, mesoporous titanium oxide, sol-gel synthesis, bimetallic clusters, citral hydrogenation

Abstract >>
A new method is developed to obtain nanosized catalytic Pt–Sn/TiO2 coatings on the inner surface of a capillary microreactor during adsorption of polynuclear carbonyl PtSn complexes on mesoporous TiO2. Titanium oxide sol prepared in the presence of template (Pluronic F127 surfactant) is supported in dynamic mode. PtSn bimetallic catalysts with an average particle size of 1.5-2 nm are synthesized by adsorption of the bimetallic [Pt3(CO)3(SnCl3)2(SnCl2×H2O)]n2n¯ complex followed by thermal treatment. Physicochemical properties of samples (thickness, structure and morphology, chemical composition of the material, electronic state, specific surface area, pore volume and size distribution) are characterized by a set of methods (HR TEM, SEM, powder XRD, XRF, XPS, low-temperature nitrogen adsorption). Conditions to prepare the uniform non-peelable PtSn/TiO2 coating on the inner surface of a silica capillary with good adhesion are determined. To increase the TiO2 thickness, multilayered TiO2 films are synthesized by layer-by layer deposition. The coating thickness is found to increase with an increase in the capillary diameter. The coating of a capillary with a diameter of 0.55 mm after 14-fold deposition is characterized by a thickness of 2 mm and an average pore size of 5.4 nm. The solvent effect on the adsorption of PtSn carbonyl complexes into the TiO2 support is studied. The amount of the adsorbed complex increases in the following order: ethanol < acetone ~ tetrahydrofuran. The physicochemical properties of the active component (surface concentration, dispersion, and composition) can be fine-tuned by varying the deposition method, precursor concentration in the initial solution, and temperature conditions of activation treatment. The catalyst activity in citral hydrogenation was 0.06-0.54 min1, with the selectivity with respect to unsaturated alcohols reaching 90% at citral conversion above 95%.



7.
DFT, FT-RAMAN, AND FT-IR INVESTIGATIONS OF 1-CYCLOPROPYLPIPERAZINE

G. Keşan1, O. Alver2, M. Bilge3, C. Parlak4
1University of South Bohemia, Česk Budĕjovice, Czech Republic
2Anadolu University, Eskişehir, Turkey
3Ege University, İzmir, Turkey
4Dumlupınar University, Ktahya, Turkey
Keywords: 1-cyclopropylpiperazine, vibrational spectra, PED, DFT, B3LYP

Abstract >>
FT-IR and FT-Raman spectra of 1-cyclopropylpiperazine (1cppp) are experimentally examined in the range 4000—200 cm–1. The optimized geometric parameters, conformational equilibria, normal mode frequencies and corresponding vibrational assignments of 1cppp C7H14N2 are theoretically examined by means of B3LYP hybrid density functional theory (DFT) with the 6-31++G(d,p) basis set. Based on the potential energy distribution (PED) reliable vibrational assignments are made and the thermodynamics functions, highest occupied and lowest unoccupied molecular orbitals (HOMO and LUMO) of 1cppp are predicted. Calculations are performed for four different conformations in two point groups of 1cppp in the gas phase. A comparison between the experimental and theoretical results indicates that the B3LYP method is able to provide satisfactory results for the prediction of vibrational frequencies, structural parameters, and assignments. Furthermore, the C s (equatorial-equatorial) point group is found as the most stable conformer of 1cppp.



8.
EXPERIMENTAL AND THEORETICAL CHARACTERIZATION OF N,N'-BIS(2,4-DIHYDROXYBENZYLIDENE)-1,2-DIAMINOBENZENE SCHIFF BASE AND ITS Cu(II) COMPLEX

S.A. Beyramabadi1, H. Eshtiagh-Hosseini2, M.R. Housaindokht2, S. Shirzadi2, A. Morsali1, M.A. Naseri3
1Mashhad branch, Islamic Azad University, Mashhad, Iran
2Ferdowsi University of Mashhad, Mashhad, Iran
3Department Birjand University, Birjand, Iran
Keywords: Schiff base, copper, IR assignment, NMR, DFT, resorcinol

Abstract >>
A new Schiff base ligand N,N'-bis(2,4-dihydroxybenzylidene)-1,2-diaminobenzene [=H2L] and its Cu(II) complex [Cu(L)] are synthesized and characterized by IR, UV-Vis, NMR, mass spectrometry and elemental analysis. Also, the computational prediction of optimized geometries, IR spectra and NMR chemical shifts is performed using the density functional theory (DFT) method. The DFT optimized geometry of the ligand is not planar, so the three benzene rings are located in separate planes. The phenolic protons are engaged in the intramolecular hydrogen-bonding interactions. In the optimized geometry of the square comlex, dianionic L2– acts as a tetradentate ligand, which occupies four coordination positions in the N, N, O, O manner. The consistency between the calculated and experimental results confirms the validity of the optimized structures for the H2L ligand and its Cu complex.



9.
3,3'-DIHYDROXY-4,4'-[1,2-CYCLOHEXANEDIYL BIS(NITRILOMETHYLIDYNE)]-BIS-PHENOL SCHIFF-BASE AND ITS Mn(II) COMPLEX: SYNTHESIS, EXPERIMENTAL AND THEORETICAL CHARACTERIZATION

H. Eshtiagh-Hosseini1, S.A. Beyramabadi2, M. Mirzaei1, A. Morsali2, A.R. Salimi1, M.A. Naseri3
1Ferdowsi University of Mashhad, Mashhad, Iran
2Mashhad branch, Islamic Azad University, Mashhad, Iran
3Birjand University, Birjand, Iran
Keywords: Schiff base, salen, Mn, DFT, IR assignment, NMR, cyclohexanediyl

Abstract >>
In this work, a 3,3'-dihydroxy-4,4'-[1,2-cyclohexanediyl bis (nitrilomethylidyne)]-bis-phenol [=H2L] Schiff-base ligand and its Mn(II) complex [Mn(L)(H2O)2] are newly synthesized and characterized by elemental analysis, IR and NMR spectroscopies. Also the geometry optimizations, assignment of the IR bands and NMR chemical shifts are computed using the density functional theory (DFT) method. The DFT optimized geometry of the ligand is not planar; each of the cyclohexane and two benzene rings are located in separate planes. The phenolic protons are engaged in the intramolecular-hydrogen-bonding interactions with azomethine nitrogen atoms. In the optimized geometry of the octahedral Mn2+ complex, the dianionic L2– acts as a tetradentate ligand in the N, N, O, O manner, where the coordinating atoms occupy the four equatorial positions. The two axial positions are occupied by two H2O ligands. The theoretical and experimental results are in good agreement, confirming the validity of the optimized geometries for the H2L ligand and its Mn complex.



10.
STRUCTURE-DETERMINING ROLE OF Tl+ IN NATURAL AND SYNTHETIC SULFIDES

S. V. Borisov, S. A. Magarill, N. V. Pervukhina
A. V. Nikolaev Institute of Inorganic Chemistry, Siberian Division, Russian Academy of Sciences, Novosibirsk
borisov@niic.nsc.ru
Keywords: thallium sulfides, crystallographic analysis, cationic and anionic sublattices, thallium in the anionic sublattice

Abstract >>
A crystallographic analysis is performed for the structures of TlCu2S2, TlCu7S4, TlTaS3, TlIn3S5, TlIn5S8, and TlCr2V3S8. In them the Tl+ cation is included in anion sublattices and stabilizes their regularity. The cation sublattices are substantially distorted and have additional conjugation to the anionic positions of the thallium cations. The monoclinic structures (the last three) have geometrically similar anionic and cationic “forced skeletons,” while in tetragonal (the first two) and orthorhombic symmetries they are modified by symmetry restrictions.



11.
[(NH3)5Cl]WO4 ( = Cr,Rh): SYNTHESIS, CRYSTAL STRUCTURE, THERMAL PROPERTIES

S. A. Gromilov1,2, S. P. Khranenko1, P. E. Plyusnin1,2, P. Yu. Vanina1,2, N. V. Kuratieva1,2
1A. V. Nikolaev Institute of Inorganic Chemistry, Siberian Division, Russian Academy of Sciences, Novosibirsk
2Novosibirsk State University
Keywords: tungsten, rhodium, chrome, complex salt, crystal chemistry, single crystal X‑ray diffraction study, thermal properties

Abstract >>
By single crystal X‑ray diffraction the crystal structure of a series of [ (NH3)5Cl]WO4 ( = Cr, Rh) complex salts is determined. The features of thermal expansion of the single crystal of [Cr(NH 3) 5Cl]WO 4 are studied by low- and high-temperature X‑ray diffractometry in the temperature range from –173°C to +127C. It is shown that with an increase in the temperature, WO distances and ∠OWO bond angles equalize and the average WO distances decrease by 0.012 Å. The thermal properties of the salts in different gaseous atmospheres are examined and the phase composition of the obtained products is studied.



12.
PROPERTIES AND STRUCTURE OF NEW VOLATILE PHENYL-CONTAINING β-DIKETONATES OF TRIMETHYLPLATINUM(IV): (CH3)3Pt(btfa)H2O, (CH3)3Pt(bac)Py, AND INITIAL COMPLEX [(CH3)3PtI]4

G. I. Zharkova, I. A. Baidina, A. I. Smolentsev, I. K. Igumenov
A. V. Nikolaev Institute of Inorganic Chemistry, Siberian Division, Russian Academy of Sciences, Novosibirsk
Keywords: β-diketonates of trimethylplatinum(IV), synthesis, structure, volatility, thermal properties

Abstract >>
By interaction of trimethylplatinum(IV) iodide with phenyl-containing β-diketonates, the volatile monomeric complexes of trimethylplatinum(IV) based on benzoyltrifluoroacetone (Hbtfa) and benzoylacetone (Hbac) of the composition (CH3)3Pt(btfa)H2O (I) and (CH3)3Pt(bac)Py (II) are obtained. Synthesis of the complexes is described; data of elemental analysis and IR spectra are reported; thermal characteristics are studied by thermogravimetry. For the first time, a single crystal X-ray diffraction study of complexes (I), (II), and the initial tetrameric complex [(CH3)3PtI]4 (III) is performed.



13.
CRYSTAL AND ELECTRONIC STRUCTURE OF HETEROMOLECULAR COMPLEXES OF 3,6-BIS(3,5-DYMETHYLPYRAZOLE-1-YL)-1,2,4,5-TETRAZINE WITH AZOLES

P. A. Slepukhin1, E. S. Salmina1, V. A. Potemkin2, M. A. Grishina2
1I. Ya. Postovskii Institute of Organic Synthesis, Ural Division, Russian Academy of Sciences, Yekaterinburg, Russia
2Pharmacy Department, Chelyabinsk State Medical Academy, Chelyabinsk, Russia
Keywords: X-ray crystallography, molecular crystals, hydrogen bond, 3,6-bis(3,5-dimethylpyrazole-1-yl)-1,2,4,5-tetrazine, quantum topological analysis

Abstract >>
X-ray crystallography is used to investigate heteromolecular crystals of 3,6-bis(3,5-dimethylpyrazole-1-yl)-1,2,4,5-tetrazine with NH-donating azole derivatives. The effect is studied of the structure of azole on molecular packing in the crystal and the characteristics of covalent bonds in the molecule of 3,6-disubstituted tetrazine. The distribution of electron density critical points inside crystal cells is analyzed to identify and quantitatively describe the intermolecular interactions underlying the formation of lateral and stacking motifs.



14.
CRYSTAL AND MOLECULAR STRUCTURE OF THE ASYMMETRIC ETHYLENEDIAMINE-N,N-DI-3-PROPIONIC ACID MONOHYDRATE

O. N. Podmareva1, Z. A. Starikova2, N. V. Tsirul’nikova1
1Institute of Chemical Reagents and High-Purity Chemical Substances, Moscow, Russia
olga.podmareva-irea@rambler.ru
2A. N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Moscow, Russia
Keywords: N,N-ethylene-bis-β-alanine, ethylenediamine-N,N-di-3-propionic acid, EDDP, complexing agent, asymmetric structure, single-crystal X-ray diffraction

Abstract >>
A new complexing agent the “asymmetric” ethylenediamine-N,N-di-3-propionic acid (as.EDDP) is obtained. The crystal structure of the new compound is determined by single-crystal X-ray diffraction. 816N2O4×2 crystals are monoclinic; space group 21/c , = 12.7416(4) Å, b = 6.5470(2) Å, c = 12.1908(4) Å, β = 93.100(1)°, Z = 4, ρx = 1.454 mg/m3, and R1(I > 2.0σ( I )) = 0.0326. In the solid form, the as.EDDP molecule has a double betaine structure. The intramolecular hydrogen bonds with the betaine proton of the tertiary nitrogen atom are formed with the participation of one oxygen atom of the carboxyl group of each 3-propionic fragment, which forms two N(1)–H(1N)-bonded six-membered H-cycles. The intermolecular hydrogen bonds are formed between the three hydrogen atoms of the protonated primary nitrogen atom and the oxygen atoms of the 3-propionic fragments of three other as.EDDP molecules. The water molecule participates in the formation of intermolecular hydrogen bonds with the oxygen atom of one carboxyl group of the molecule.



15.
CRYSTAL STRUCTURES OF METHYL AND BENZYL 5-FERROCENYL-3,5-DIMETHYL-2-PYRAZOLINE-1-DITHIOCARBOXYLATE

X. Zhu1,2, D.-S. Xiang1, W.-Y. Shi3
1Department of Chemical Engineering, Yancheng Textile Vocational Technology College, Yancheng, P. R. China
2School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing, P. R. China
3School of Chemical and Biological Engineering, Yancheng Institute of Technology, Yancheng, P. R. China
Keywords: pyrazoline, ferrocenyl, dithiocarboxylate, X-ray

Abstract >>
Reactions of E -4-ferrocenylpent-3-en-2-one with S -methyldithiocarbazate or S -benzyldithiocarbazate result in the formation of methyl 5-ferrocenyl-3,5-dimethyl-2-pyrazoline-1-dithiocarboxylate (1) or benzyl 5-ferrocenyl-3,5-dimethyl-2-pyrazoline-1-dithiocarboxylate (2). The single crystals of both products are obtained and their structures are identified by X-ray diffraction method with triclinic P -1 space groups. The cell parameters for compound 1 are as follows: a = 7.7029(8) Å, b = 10.1631(11) Å, c = 10.7305(12) Å, α = 101.3270(10), β  = 90.6740(10), γ = 94.8390(10), and V = 820.40(15) Å 3. For compound 2, the crystallographic data are: a = 7.953(3) Å, b = 10.970(5) Å, c = 12.534(3) Å, α = 84.718(5), β  = 81.651(3), γ = 76.274(4), and V = 1049.1(7) Å 3.



16.
CONFORMATIONAL VARIABILITY IN A NEW TERPENOID-LIKE BISCHALCONE: STRUCTURE AND THEORETICAL STUDIES

W.B. Fernandes1, L.A. Malaspina2, F.T. Martins, L.M. Lio, A.J. Camargo1, C. Lariucci2, C. Noda-Perez, H.B. Napolitano1
1Cincias Exatas e Tecnolgicas, Universidade Estadual de Gois, 75001-970 Anpolis, GO, Brazil
2Instituto de Fsica, Universidade Federal de Gois
Keywords: terpenoid-like bischalcone, X-ray diffraction, disorder modeling

Abstract >>
A new terpenoid-like bischalcone (1E,4E)-1-(4-nitrophenyl)-5-(2,6,6-trimethylcyclohex-1-enyl)-penta-1,4-dien-3-one was synthesized from a b-ionone and 4-nitrobenzaldehyde by ClaisenSchmidt condensation reaction and its structure was determined by single crystal X-ray diffraction analysis. Additionally, this compound was featured by powder X-ray diffraction, 1H, 13C NMR and IR spectroscopy techniques. The molecule in the asymmetric unit showed disordered occupancy sites over two positions for the trimethylcyclohexene atoms. These two conformations were related by a rotation of about 180 around the axis of the CC bond linking the six-membered ring and the olefin carbons. Single-molecule calculations using the DFT method have strengthened this structural finding, since our theoretical approaches also suggest two well-defined conformations of similar energies which resemble the molecular geometries determined by X-ray diffraction. Furthermore, the inspection of the crystal packing revealed that the hydrogen bonding patterns are different for each conformation of the compound reported here.



17.
CRYSTAL ARCHITECTURE AND THERMAL DECOMPOSITION OF TWO NEW ORGANICALLY TEMPLATED CADMIUM SULFATES

R. Jlassi1, W. Rekik1, H. Nali1, T. Mhiri1, T. Bataille2
1Laboratoire Physico-Chimique de l'tat Solide, Dpartement de Chimie, Facult des Sciences de Sfax, Universit de Sfax, Sfax, Tunisia
2Sciences Chimiques de Rennes (CNRS, UMR 6226), Universit de Rennes 1, Rennes Cedex, France
Keywords: hybrid material, slow evaporation, X-ray diffraction, crystal structure, thermal decomposition, supramolecular

Abstract >>
Two organic-inorganic hybrid compounds (C 5H 14N 2)[Cd(H 2O) 6](SO 4) 2 (I) and R-(C 5H 14N 2) [Cd(H 2O) 6](SO 4) 2 (II) are synthesized by the slow evaporation method and characterized by single crystal X-ray diffraction, thermogravimetry, temperature-dependent X-ray diffraction, and infrared spectroscopy. The first compound crystallizes in the centrosymmetric space group P 2 1/ n with the following unit cell parameters: a = 6.6208(2) Å, b = 10.6963(3) Å, c = 12.9318(4) Å, V = 893.05(6) Å 3, and Z = 2. Its structure is solved by direct methods and refined by the least-squares analysis [ R 1 = 0.0389 and wR 2 = 0.0821]. This compound shows a crystallographic disorder II destroys the inversion symmetry and leads to a fully ordered structure. Indeed, compound II crystallizes in the non-centrosymmetric space group P 2 1 with the following unit cell parameters: a = 6.6306(1) Å, b = 10.7059(2) Å, c = 12.9186(1) Å, V = 894.67(2) Å 3, and Z = 2. The crystal structure of both compounds is built from isolated anions, disordered 2-methylpiperazinediium, (C 5H 14N 2) 2+ in compound I or R-2-methylpiperazinediium R-(C 5H 14N 2) 2+ in compound II, and divalent metal cations surrounded by six water molecules. These different entities are connected together only by a 3D hydrogen bond network. The thermodiffractometry and the thermogravimetric analyses indicate that the decomposition of the supramolecular precursors proceeds through several stages leading to cadmuim oxide.



18.
CRYSTAL STRUCTURE OF [CoEn3]2(W724)⋅62

N. V. Kuratieva1,2, I. O. Tereshkin1,2, S. P. Khranenko1, S. A. Gromilov1,2
1A. V. Nikolaev Institute of Inorganic Chemistry, Russian Academy of Sciences, Siberian Division, Novosibirsk
2Novosibirsk State University, Novosibirsk
Keywords: tungsten, cobalt, complex salt, carbide, crystal chemistry, X-ray crystallography, thermal properties

Abstract >>
Crystal structure of a complex salt [CoEn3]2(W724)×62 is determined by X-ray crystallography. Powder X-ray diffraction is applied for the phase identification of the products of thermal decomposition of the salt in the helium atmosphere.



19.
CRYSTAL STRUCTURE OF DIETHYL-1-ISOBUTYL-9-HYDROXY-9-METHYL-7-PHENYL-1,4-DIAZASPIRO[4,5] DECANE-6,8-DICARBOXYLATE C25H38N2O5

A. M. Magerramov1, A. I. Ismiev1, N. A. Kadyrova1, K. . Gadzhieva1, R. K. Askerov1, K. A. Potekhin2
1Baku State University, Baku
2Vladimir State University, Vladimir
Keywords: oxocyclohexanedicarboxylates, N-isobutylethylenediamine, diazaspirocycles

Abstract >>
The reaction of diethyl-4-hydroxy-4-methyl-2-phenyl-6-oxocyclohexane-1,3-dicarboxylate with N-isobutylethylenediamine is performed and the crystal structure of this reaction product (diethyl-1-isobutyl-9-hydroxy-9-methyl-7-phenyl-1,4-diazaspiro[4,5]decane-6,8-dicarboxylate) is determined by X-ray crystallography.



20.
CONSTRUCTION OF CHLORIDO-BRIDGED DINUCLEAR COPPER(II) COMPLEXES WITH SIMILAR TRIDENTATE SCHIFF BASES

S.-S. Qian1, H.-H. Li2, Z.-L. You2, H.-L. Zhu1
1School of Life Sciences, Shandong University of Technology, ZiBo, P. R. China
2Department of Chemistry and Chemical Engineering, Liaoning Normal University, Dalian, P. R. China
Keywords: Schiff base, copper complex, dinuclear complex, crystal structure

Abstract >>
Two new chlorido-bridged dinuclear copper(II) complexes [Cu 2Cl 2(L 1) 2] (1) and [Cu 2Cl 2(L 2) 2] (2), where L 1 and L 2 are the deprotonated form of Schiff bases 2-[1-(2-morpholin-4-ylethylimino)ethyl]phenol (HL 1) and 2-[1-(2-piperidin-1-ylethylimino)ethyl]phenol respectively, are prepared and structurally characterized by elemental analysis, IR spectra, and single crystal X-ray crystallography. Complex 1 crystallizes in the monoclinic space group P 2 1/ c with unit cell dimensions a = 8.0816(2) Å, b = 19.1780(3) Å, c = 9.6757(3) Å, b = 106.465(2), V = 1438.13(6) Å 3, Z = 2, R 1 = 0.0409, and wR 2 = 0.1085. Complex 2 crystallizes in the monoclinic space group P 2 1/ c with unit cell dimensions a = 7.7640(10) Å, b = 19.930(3) Å, c = 9.628(2) Å, b = 103.890(3), V = 1446.2(4) Å 3, Z = 2, R 1 = 0.0634, and wR 2 = 0.1316. Each Cu atom in the complexes is coordinated by three donor atoms of the Schiff bases and by two bridging Cl atoms, forming square pyramidal geometry. The Cl anions are preferred bridging groups for the construction of dinuclear copper complexes with tridentate Schiff bases.



21.
CHARACTERIZATION AND CRYSTAL STRUCTURES OF SOLVATED N'-(4-HYDROXY-3-NITROBENZYLIDENE)-3-METHYLBENZOHYDRAZIDE AND N'-(4-DIMETHYLAMINOBENZYLIDENE)-3-METHYLBENZOHYDRAZIDE

J.-J. Ma
Hebei Key Laboratory of Bioinorganic Chemistry, College of Sciences, Agricultural University of Hebei, Baoding 071001, P. R. China
Keywords: benzohydrazone, Schiff base, hydrogen bonding, π⋯π interaction

Abstract >>
Two new solvated benzohydrazone derivatives N'-(4-hydroxy-3-nitrobenzylidene)-3-methylbenzohydrazidemethanolwater (2/1/1) 2(C 15H 13N 3O 4)×CH 3OH×H 2O (1) and N'-(4-dimethylaminobenzylidene)-3-methylbenzohydrazide methanol monosolvate C 17H 19N 3O×CH 3OH (2) are prepared and characterized by elemental analysis, 1H and 13C NMR, and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group P2 1/ c with unit cell dimensions a = 17.084(2) Å, b = 12.706(1) Å, c = 15.412(1) Å, β = 113.207(1), V = 3074.1(4) Å 3, Z = 4, R 1 = 0.0567, and wR 2 = 0.1209. Compound 2 crystallizes in the monoclinic space group P2 1/ n with unit cell dimensions a = 15.058(1) Å, b = 6.658(1) Å, c = 17.211(2) Å, β = 94.189(2), V = 1720.8(3) Å 3, Z = 4, Rsub>1 = 0.0611, and wR 2 = 0.1594. X-ray diffraction indicates that the asymmetric unit of 1 contains two independent benzohydrazone molecules, one methanol and one water molecules. The asymmetric unit of 2 contains one benzohydrazone molecule and one methanol molecule. Benzohydrazone molecules of the compounds display trans configurations with respect to the C=N double bonds. The crystal structures of the compounds are stabilized by hydrogen bonds and weak π⋯π interactions.



22.
CRYSTAL STRUCTURES OF AROYLHYDRAZONES DERIVED FROM 5-METHOXYSALICYLALDEHYDE

Q.-S. Zong1,2, J.-Y. Wu1
1College of Biology and Chemical Engineering, Jiaxing University, Jiaxing Zhejiang, P. R. China
2School of Pharmaceutical Sciences, Zhejiang University, Hangzhou Zhejiang, P. R. China
Keywords: aroylhydrazone, Schiff base, synthesis, X-ray structure, hydrogen bonding

Abstract >>
Two new aroylhydrazones 3-bromo-N'-(2-hydroxy-5-methoxybenzylidene)benzohydrazide (1) and 4-hydroxy-3-methoxy-N'-(2-hydroxy-5-methoxybenzylidene)benzohydrazide (2), derived from 5-methoxysalicylaldehyde, are prepared and determined by means of infrared and 1H NMR spectroscopy and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group P2 1/ n with a = 5.9406(7) Å, b = 31.833(3) Å, c = 7.6460(8) Å, β = 94.522(4), V = 1441.4(3) Å 3, Z = 4. Compound 2 crystallizes in the monoclinic space group P2 1/ c with a = 14.3471(9) Å, b = 11.3893(7) Å, c = 9.6853(6) Å, β = 94.063(2), V = 1578.6(2) Å 3, Z = 4. Both molecules have very similar bond lengths and angles. The crystal structures of both compounds are stabilized by NH⋯O and OH⋯O hydrogen bonds as well as π⋯π interactions.