Y. Yahsi1, E. Gungor1, C. Kazak2, H. Kara1,3 1Balikesir University, Faculty of Art and Science, Balikesir, Turkey 2Ondokuz Mayis University, Faculty of Art and Science, Samsun, Turkey 3Mugla Sitki Kocman University, Mugla, Turkey
Keywords: synthesis, Schiff-base ligands, iron (III) complexes, X-ray crystal structure analysis, oxo bridged structure
A dimeric [{Fe(5-ClL1)}2(m-O)], [H2-5-ClL1 = N,N¢-bis(5-Chloro-2-hydroxybenzylidene)- 2-methylpropane-1,2-diamine] tetradentate Schiff-base complex, 1, has been synthesized and its crystal structure has been determined by single crystal X-ray diffraction analysis. Structural analysis of complex 1 shows that the complex is a centrosymmetric dimer. Each of the Fe(III) ions has a five-coordinate geometry and one oxygen atom bridges two Fe(III) ions to form a m-oxo structure. The geometry around iron atom can be described as a square based pyramid with the FeN2O2 coordination plane and oxo ligand.
E. S. Vikulova1, S. I. Dorovskikh1, A. D. Shushanyan2, N. V. Kuratieva2, P. A. Stabnikov1, L. N. Zelenina2, N. B. Morozova2 1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia 2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: синтез, β-иминокетонаты меди(II), рентгеноструктурный анализ, термогравиометрия, дифференциально-сканирующая калориметрия, synthesis, copper(II) β-iminoketonates, single crystal X-ray diffraction analysis, thermogravimetry, differential scanning calorimetry
The single crystal X-ray diffraction (XRD) method was used to determine the structure of the [Cu(mi-tfac)2] (mi-tfac = MeC(O)CHC(NMe)CF3) complex at the temperature of 150 K. The crystallographic data are as follows: space group Pnna , a = 11.8798(16) Å, b = 12.0315(16) Å, c = 10.6259(14) Å, V = 1518.8(4) Å3, Z = 4, R = 0.0288. The structure is molecular, the coordination environment of copper in the molecule adopts a distorted tetrahedral geometry. The Cu-O and Cu-N distances are 1.9182(13) Å and 1.9610(16) Å respectively, the OCuN chelate angle is 94.18(5)°. The thermal properties of the compounds [Cu(mi-tfac)2] and [Cu(RC(O)CHC(NMe)R)2] (R = Me, t Bu) in the condensed phase have been studied by the methods of thermogravimetry and differential scanning calorimetry. The thermodynamic characteristics of the melting processes have been determined.
M. Ben Nasr1, E. Aubert1, V. Ferretti2, E. Espinosa1, P.S.P. Silva3, L.C.J. Pereira4, M.R. Silva3 1Vandoeuvre les Nancy, Nancy, France 2Center for Structural Diffractometry, Ferrara, Italy 3University of Coimbra, Coimbra, Portugal 4Instituto Superior Técnico, UTL, Bobadela LRS, Portugal
Keywords: coordination compounds, copper(II) complex, crystal structure, magnetism, IR spectroscopy, cryomagnetic
A new Cu (II) complex with bidentate o-phenanthroline (phen) ligand, ([Cu(phen)]2(H2PO4)2××HPO4)2(H3PO4)4, has been synthesized and characterized by single crystal X-ray diffraction, IR spectroscopy and magnetic data. The crystal structural analysis shows that the title compound contains two phosphate-bridged dimeric units ([Cu(phen)]2(H2PO4)HPO4), which are crystallographically independent. In these units, each copper atom is five coordinated and the geometry around the Cu(II) can be described as slightly distorted square-based pyramidal, with parameter varying between 0.001 and 0.04. The crystal structure is stabilized by O-H…O and C-H…O hydrogen bonds between the dimeric units and the phosphoric acid molecules. In addition, the organic ligands are associated by π-π stacking interactions between neighboring non-nitrogen aromatic rings. The infrared spectrum recorded at room temperature was interpreted on the basis of data published in the literature. The magnetic susceptibilities data show a weak intra-dimer ferromagnetic interaction with J = 31.8 K.
A. Aguirrechu-Comerón1, J. Pasán1, J. González-Platas1, J. Ferrando-Soria2, R. Hernández-Molina3 1Universidad de La Laguna, Tenerife, Spain 2Texas A&M University, Texas 77842, USA 3Instituto Universitario de Quimica Bioorganica, La Laguna, Tenerife, Spain
Keywords: copper, structures, halides, magnetism
The preparation of four new copper(II) complexes with different N-donor ligands [CuBr2×(2-benzylpyridine)2] (1), [CuBr2(2-benzylpyridine)(2,2'-bipyridine)]×H2O (2), [CuBr2(3-methyl-2-phenylpiridine)2] (3), [Cu(picolinate)2]×KI (4) from copper(I) halides as starting material is described. During the preparation of compound 4 a ligand oxidation reaction took place to give the picolinate ligand starting from 2-(2-methylaminoethyl)pyridine. The complexes were characterized by elemental analyses, IR spectroscopy and crystallographic studies. Single crystal X-ray diffraction analysis of the complexes reveals their monomeric penta- and tetracoordinated nature. For all compounds, the copper(II) present a common square planar coordination except for compound 2 which is five coordinated in a quasi-square pyramidal configuration with t of 0.29. The Cu-N distances for these compounds are in the range of 1.959(4)-2.041(3) Å, Cu-O distance was 1.961(3) Å and Cu-Br distances were in the range of 2.4052(4)-2.4381(6) Å for the square base configuration while for apical distance it was 2.6745(7) Å. Magnetic properties have been investigated for all compounds in the temperature range 2-300 K. Compound 1 shows weak antiferromagnetic intermolecular interaction.
W.-L. Hou1, G.-Y. Dong2, X.-X. Wang2, K. Van Hecke3 1Hebei Normal University of Science and Technology, Qinhuangdao, Hebei, P. R. China 2Hebei United University, Tangshan, Hebei, P. R. China 3Ghent University, Ghent, Belgium
Keywords: bis(benzimidazole) ligand, crystal structure, fluorescence, zinc(II) complex
A new Zn(II) coordination polymer, {[Zn(npht)(L)0.5(H2O)]×H2O} n (L = 1,4-bis(2-methylbenzimidazol-1-ylmethyl)benzene, H2npht = 3-nitrophthalic acid) has been hydrothermally synthesized and characterized by elemental analysis, IR, XRPD, and single-crystal X-ray diffraction. The Zinc(II) coordination compound exhibits a 1D linear chain, which is further assembled into a 2D supramolecular layer via two modes of classial hydrogen bonding interactions. The fluorescence properties and thermal stability of the complex have been investigated in the solid state.
H.H. Li, Y.Q. Zhao, G.Y. Li, G.H. Cui
Hebei United University, Tangshan, Hebei Province, P. R. China
Keywords: bis(benzimidazole), Cd(II) complex, crystal structure, fluorescence
A new coordination polymer, {[Cd(bbmb)(bdc)]} n (bbmb = 1,1¢-(1,4-butanediyl)bis-(2-methylbenzimidazole), H2bdc = 1,3-benzenedicarboxylic acid) was synthesized under hydrothermal conditions. The complex was structurally characterized by single crystal X-ray diffraction analyses, infrared spectroscopy (IR), elemental analyses. The compound crystallizes in the monoclinic system, space group P 21/ c with a = 10.860(6) Å, b = 13.115(7) Å, c = 21.009(9) Å, b = 120.94(2)°, V = 2567(2) Å3, Z = 4, C28H26CdN4O4, Mr = 594.93, Dc = 1.540 g/cm3, m = = 0.893 mm-1. Each cadmium center is six coordinated with four O atoms from two bdc2- anions, and two N atoms of two bbmb ligands. The complex features a 4-connected 2D (4, 4) sheet with a point symbol {42.62}. Fluorescence properties of the title complex were investigated.
A two-dimensional (2D) coordination polymer, formulated as [Y4(m3-OH)4(hma)(cba)5] n × × n (Hcba) (1), is synthesized by the synergistic coordination of hemimellitate (H3hma) and 4-chlorobenzoate (Hcba) ligands with Y2O3 under hydrothermal conditions. It has been characterized by single-crystal X-ray diffraction, powder XRD, thermogravimetric analysis, elemental analysis and infrared spectroscopy. Single-crystal X-ray diffraction reveals that it crystallizes in the triclinic crystal system, P space group. Unit cell parameters: a = 11.0280(6) Å, b = 14.5791(10) Å, c = 18.9515(12) Å, a = 72.233(6)°, b = 82.641(5)°, g = 70.933(5)°, V = 2741.1(3) Å3, Z = 2. The asymmetric unit contains a [Y4(m3-OH)4]8+ core which is extended into an infinite {[Y4(m3-OH)4]8+} n chain along the direction of a axis. Every {[Y4(m3-OH)4]8+} n chain is further connected to two neighboring chains by hma3- ligands along the direction of b axis, forming a 2D yttrium-organic layer in the ab plane. Adjacent layers are further packed with each other via hydrophobic interactions to form a three-dimensional (3D) structure.
A. V. Gerasimenko, R. L. Davidovich, M. A. Pushilin, V. B. Logvinova
Institute of Chemistry, Far East Branch, Russian Academy of Sciences, Vladivostok, Russia
Keywords: синтез, кристаллическая структура, комплексный фторид, цирконий, гафний, полиморфная модификация, конформер, 4-амино-1,2,4-триазол, synthesis, crystal structure, complex fluoride, zirconium, hafnium, polymorph, conformer, 4-amino-1,2,4-triazole
New hybrid organic-inorganic complex zirconium and hafnium fluorides with the 4-amino-1,2,4-triazolium cation (C2H5N4)2MF6 (M = Zr, Hf, Zr x Hf1- x ), which crystallize in two polymorphs (monoclinic ( P 21/ n , Z = 4) and triclinic ( P , Z = 2)) are synthesized and structurally studied for the first time. The structures of both polymorphs are composed of hydrogen bonded (N-H⋯F and C-H⋯F) 4-amino-1,2,4-triazolium cations protonated via the nitrogen atom in site 1 and complex [M2F12]4- anions that are centrosymmetric dimers formed by edge-sharing pentagonal bipyramids MF7 (M = Zr, Hf, Zr x Hf1- x ). It is found that in the structures studied 4-amino-1,2,4-triazolium cation occur simultaneously as cis- and trans- conformers. The packing character of structural units in the unit cells of the studied crystals is discussed along with the structure of the neutral and protonated forms of 4-amino-1,2,4-triazole.
A novel inorganic-organic hybrid salt, hexanediammonium heptamolybdate (C6H18N2)2[H2Mo7O24]×7H2O has been synthesized and characterized by elemental analyses, IR, TGA, cyclic voltammetry, UV and X-ray single crystal diffraction. It crystallizes in triclinic space group P -1 with a = 10.0619(2) Å, b = 12.059(2) Å, c = 20.044(3) Å, a = 97.06(1)°, b = 91.56(1)°, g = 110.59(2)° and Z = 2. The crystal structure shows that seven MoO6 distorted octahedra share edges which have four ranges of Mo-O bond distances. The heptamolybdate anion of the crystal has approximate mm 2 point symmetry and its structure is similar to that observed in other heptamolybdates. The titled compound consists of the protonated hexanediamine cations and the inorganic [H2Mo7O24]4- oxomolybdate anions, linked by hydrogen-bonding interactions.
M. Gowri1, T. Srinivasan2, D. Velmurugan2 1Avinashilingam University for Women, Coimbatore - 641 043, Tamilnadu, India 2University of Madras, Guindy Campus, Chennai - 600 025, Tamilnadu, India
Keywords: Ru(II) complex, triphenyl arsine, pyridine, chloride, carbonyl complex, crystal structure
The title complex [Ru(Cl)2(CO)(py)2(AsPh3)], was synthesized and characterized. The molecular structure and crystal structures are determined by X-ray crystallography. The dihedral angle between the two cis -pyridine rings is 73.3(2)°, which shows that they are almost orthogonal to each other. The molecular structure is stabilized by inter-molecular and intra-molecular C-H…Cl interactions. The molecular structure is further stabilized by interactions between the aromatic rings.