Synthesis and crystal structure of bis(di-n-butyldithiocarbamato)(1,10-phenanthroline)cadmium(II)

A new mixed-ligand complex, Cd(S₂CN(C₄H₉)₂)₂Phen, is synthesized and investigated by thermal, element, and IR analyses and by diffractometry of polycrystals (DRON-3M, CuK_α radiation, Ni filter). The crystal structure was determined on a CAD-4 Enraf-Nonius automatic diffractometer (MoK_α radiation, θ from 1.5 to 25?, 2325 nonzero independent reflections, 190 refined parameters, R = 0.036 for I > 2Σ(I)). Crystal data for C₃₀H₄₄CdN₄S₄ : a = 15.592(3), b = 22.724(5), c = 9.922(2) å, space group Pbcn, V = 3515.5(12) å₃, Z = 4, M = 701.33, d_calc = 1.325 g/cm³. The structure involves monomeric molecules in which the cadmium atom has a distorted octahedral environment.     

Tetrabutylammonium Salts of Ruthenium(II) Nitroso Complexes

The paper describes synthesis of (nBu₄N)₂[RuNOCl₅](I), (nBu₄N)₂[RuNOCl₄OH](II), (nBu₄N)₂×[RuNOCl₄OH]·6H₂O (III), and (nBu₄N)₂[RuNOCl₅]· 2(nBu₄N)₂[RuNOCl₄(H₂O)]·2H₂O (IV). The complexes were studied by IR spectroscopy and powder Xray and crystal Xray analyses. The structures are built up of [RuNOCl₅]^2- (I, IV), [RuNOCl₄OH]^2- (II, III), and [RuNOCl₄(H₂O)]^- (IV) complex anions, (nBu₄N)⁺ cations, and crystal water molecules (III, IV). The substances are moderately soluble in water; highly soluble in polar organic solvents, such as acetone, ethanol, chloroform, methylene chloride; and almost insoluble in carbon tetrachloride and toluene. Under storage in light, the compounds decompose from the surface; in darkness I and II are stable, whereas III and IV can lose part of the crystal water.     

Layer arrangement in the structure of octakis-(trimethylsiloxy)octasilsesquioxane and dodecakis-(trimethylsiloxy)cyclohexasiloxane

Layers of [(CH₃)₃SiO]₈(SiO_1.5)₈ and [(CH₃)₃SiO]₁₂(SiO)₆ organosilicon compounds obtained by chemical vapor deposition were investigated by X-ray diffraction (DRON-RM4, R = 192 mm, CuK radiation) and Raman spectroscopy (Triplemate, SPEX). The layers were found to be ideally oriented polycrystalline films. The octakis-(trimethylsiloxy)octasilsesquioxane polycrystals are oriented in one crystallographic direction — [001], while the dodecakis-(trimethylsiloxy)cyclohexa-siloxane polycrystals are oriented in the and directions. Crystal structure analysis in these directions yielded the type of the planar lattice followed by the molecules and their orientation relative to the support.Original Russian Text Copyright © 2004 by S. A. Gromilov, T. V. Basova, D. Yu. Emelyanov, A. V. Kuzmin, and S. A. ProkhorovaTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 497–501, May–June 2004.     

Volatile ZnPhen(S2CNEt2)2 and MnPhen(S2CNEt2)2 complexes and the MnZn2Phen3(S2CNEt2)6 phase: Thermal behavior and crystal and molecular structures of two modifications of ZnPhen(S2CNEt2)2

Two crystal modifications, I and II, of the ZnPhen(S₂CNEt₂)₂ complex have been isolated. According to XRD data, the single crystals of I are triclinic with a=9.745(2), b=10.252(2), c=14.331(3) Å, α=99.18(2), β=91.01(2), γ=113.28(2)°, V=1293.2(4) ų, space group P1, Z=2, d_calc=1.401 g/cm³. The crystals of II are monoclinic with a=7.220(6), b=18.095(2), c=19.050(4) Å, β=95.85(2)°, V=2475.8(7) ų, space group C2/c, Z=4, d_calc=1.461 g/cm³. In both modifications, the structure is formed by monomer molecules with a distorted octahedral environment of the zinc atom. All atoms in I are in the general position; in II, the atoms are linked by the twofold rotation axis. It is shown by X-ray phase analysis (XRPA) that the MnPhen(S₂CNEt₂)₂ complexes (III) are isostructural to modification I of the ZnPhen(S₂CNEt₂)₂ complex, which underlies the synthesis of a solid solution of these complexes, MnZn₂Phen₃(S₂CNEt₂)₆ (phase IV). It is found that MPhen(S₂CNEt₂)₂ (M=Zn²⁺, Mn²⁺) and phase IV quantitatively sublime when heated in vacuum. Thermolysis of III in argon yields manganese(II) sulfide of cubic modification; the main product of thermolysis of phase IV is a solid solution of Zn_xMn_1?xS of hexagonal modification.     

Complex X-ray diffraction study of yttrium(III) dipivaloyl methanate

Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences. Translated fromZhurnal Strukturnoi Khimii, Vol. 34, No. 3, pp. 163–165, May–June 1993.     

Synthesis and structure of complex compound Rh(III) of (NH4)2[Rh(NO2)3(NH3)(µ-OH)]2 composition

The crystalline structure of a new compound Rh(III) of (NH₄)₂[Rh(NO₂)₃(NH₃)(μ-OH)]₂ composition has been determined. The crystallographic characteristics are H₁₆N₁₀O₁₄Rh₂: a = 6.3963(2) Å, b = 9.3701(4) Å, c = 13.6646(5) Å, β = 102.266(1)°, V = 800.28(5) ų, Z = 2, d _calc = 2.432 g/cm³. The distance Rh...Rh in the dimer is 3.200 Å. Original Russian Text Copyright ? 2006 by S. P. Khranenko, I. A. Baidina, and S. A. Gromilov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 2, pp. 380–384, March–April, 2006.     

Structural arrangement of layers in some octaorganylsilsesquioxanes

Thick (≈0.2–1 μm) layers of octaorganylsilsesquioxanes [RSiO_1.5]₈, where R is CH₃, C₂H₃, and C₂H₅, were obtained by vacuum deposition and studied by X-ray diffractometry (DRON-3M, R=192 mm, CuK_α radiation). Irrespective of the type of support, the layers are ideally oriented polycrystalline films with the [001] texture axis. Structural arrangement of the layers is analyzed on the basis of the crystal data. Orientation of the terminal atomic groups on the surface of the layer is established. It is shown that it is possible to adjust the scale of the layer pattern. Two-layer compositions— Cu(II) β-diketonates and phthalocyanines on octaorganylsilsesquioxane supports and vice versa — with preserved orientations of the films were obtained. Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences. Translated fromZhurnal Strukturnoi Khimii, Vol. 37, No. 5, pp. 923–928, September–October, 1996. Translated by L. Smolina     

Crystal structure of copper(II) bis-hexafluoroacetylacetonate

An X-ray diffraction investigation has performed for copper(II) bis-hexafluoroacetylacetonate (Bruker AXS P4 automatic diffractometer, MoK radiation, t = –25°C). Crystal data for C₁₀H₂CuF₁₂O₄: a = 5.530(1) Å, b = 6.038(1) Å, c = 11.266(2) Å, = 95.948(3)°, = 101.743(3)°, = 92.298(3)°, space group; P1, V = 365.6(1) ų, Z = 1, d _calc = 2.169 g/cm³. The square-planar environment of the copper atom (Cu-O_av 1.912 Å, O-Cu-O_av 93°) is completed to bipyramidal by two fluorine atoms of the neighboring molecules, Cu...F 2.71 Å and 2.75 Å.Original Russian Text Copyright © 2004 by S. A. Gromilov, I. A. Baidina, P. A. Stabnikov, and G. V. RomanenkoTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 502–507, May–June 2004.