Crystal structure of catena-DI(2-thiobarbiturato-O,S)aqualead(II)

The crystal structure of catena-di(μ₂-2-thiobarbiturato-O,S)aqualead(II) C₈H₈N₄O₅S₂Pb (C₄H₄N₂O₂S is 2-thiobarbituric acid, H₂TBA) is determined. Crystallographic data for catena-[Pb(H₂O)(μ₂-HTBA-O,S)₂] are as follows: a = 6.5972(1) Å, b = 9.8917(2) Å, c = 10.0893(2) Å, α = 106.702(1)°, β = 93.395(2)°, γ = 107.48(1)°, V = 593.82(2) ų, space group $P\bar 1$ , Z = 2. The Pb²⁺ ion is linked with six monodentate HTBA^? ligands through two O atoms and four S atoms and also connected with a water molecule. Additionally, there is a shortened Pb-S contact (3.622 Å), given which the complex polyhedron represents a distorted square antiprism. Hydrogen bonds N-H…O and O-H…O form a branched three-dimensional network. The structure is also stabilized by the π-π interaction of heterocyclic HTBA^? ions.     

Crystal structure of (S,S)-diphenylethanediammonium (R,R)-tartrate

Summary The crystal structure of (–)-diphenylethanediammonium-(R,R)-tartrate was determined. From this structure determination, the (S,S) configuration was assigned to the (–)-diphenylethanediamine. The asymmetric unit of the crystal structure contains two units of the title compound plus one molecule of ethanol and one water molecule, which form an intricate network of 19 hydrogen bonds.

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Die Kristallstruktur von (S,S)-Diphenylethandiammonium-(R,R)-tartrat

Zusammenfassung Es wurde die Kristallstruktur von (–)-Diphenylethandiammonium-(R,R)-tartrat bestimmt. Aus dieser Strukturbestimmung ergab sich die Zuordnung der (S,S)-Konfiguration zum (–)-Diphenylethandiamin. Die asymmetrische Einheit der Kristallstruktur besteht aus zwei Formeleinheiten der Titelverbindung sowie einem Molekül Ethanol und einem Wassermolekül, welche ein komplexes Netzwerk von insgesamt 19 Wasserstoffbrücken bilden.

     

Crystal and molecular structure of Dicyanotetrasulfane S4(CN)2

S₄(CN)₂ crystallizes in the monoclinic space group P2₁/c with a = 885.7 pm, b = 794.2 pm, c = 1032.6 pm, β = 109.0° (at 173 K). The molecules occupy general sites but are of approximate C₂ symmetry. The conformation of the molecules is all-trans with torsional angles CSSS = 74.6° and 81.7° and SSSS = 84.8°. The central SS bond (201.7 pm) is much shorter than the terminal SS bonds (av. 206.8 pm). There are no stronger than van-der-Waals type intermolecular interactions.     

Crystal and electronic structure of Ni3Bi2S2 (parkerite)

The crystal structure of parkerite, Ni₃Bi₂S₂, was studied by single-crystal X-ray diffraction analysis and refined. The single crystal was prepared by the method of chemical transport reactions. The electronic structure of Ni₃Bi₂S₂ was calculated by the extended Hückel and DFT--LMTO--ASA methods. Substantial delocalization of electrons in the vicinity of the Fermi level and the presence of the strong Ni--S and Ni--Bi bonds were revealed. The Ni--Ni bonds are weak, which is in agreement with the X-ray diffraction data.     

Crystal structure of 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo [8.8.8]hexacosane (2S,3S)-tartrate

Crystal structure of (2S,3S)-tartrate of 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo-[8.8.8]hexacosane, [H₂(Crypt-222)]²⁺·(C₄H₄O₆)^2? (I) has been studied by single crystal X-ray diffraction. Triclinic structure of I (space group P1, a = 8.424 Å, b = 13.011 Å, c = 13.806 Å; α = 116.37°, β = 106.45°, γ = 91.81°; Z = 2) was solved by the direct method and refined in the full-matrix anisotropic approximation to R = 0.140 for 5850 measured independent reflections (automated diffractometer CAD-4, λMoK _α). In the structure of I, two independent dications of 2.2.2-cryptand (nitrogen atoms are protonated) are linked to the approximate inversion symmetry and have a rare conformation of exo-exo type, when two atoms sitting on N atoms are protruded out of their cavity. The centroids of two crystallographically unique (2S,3S)-tartrate dianions are bound with the same approximate inversion center. An extended system of hydrogen bonds is developed in the crystal of I.     

Crystal structure of N,N-disalicylidene-(R,S)(S,R)-1,2-ethanediamine

N,N-disalicylidene-(R,S)(S,R)-1,2-ethanediamine crystallizes in orthorhombic space group Pbca with a = 9.5634(6), b = 14.2917(9), c = 16.9181(8) Å and Z = 4. The crystal structure was solved by direct methods and refined by full-matrix least squares to final values R1 = 0.0 + 399 and wR2 = 0.1004 with 2755 reflections (I > 2σ(I)). The N,N-disalicylidene-(R,S)(S,R)-1,2-ethanediamine molecules exhibit intramolecular N-H...O and are connected by C-H...O and C-H...π interactions to form a 2D supramolecular network.     

Crystal structure of neptunium(IV) N,N-diethyl dithiocarbamate Np[S2CN(C2H5)2]4

Crystal structure of Np[S₂CN(C₂H₅)₂]₄ has been determined. The environment of the Np atom is formed by eight sulfur atoms. The coordination polyhedron of the Np atom is a dodecahedron. The Np-S bond lengths vary from 2.782(2) to 2.812(2) Å (average 2.795 Å). Two independent (H₅C₂)₂NCS ₂ ^? anions are characterized by different orientations of the diethylcarbamate fragments. A comparison of the geometric characteristics of the coordination polyhedra of the compounds An[S₂CN(C₂H₅)₂]₄ (An = Th, Np) and Np(S₂CN(C₂H₅)₂)₄][N(C₂H₅)₄ shows that the average Np-S bond lengths in the coordination polyhedra decrease by the same value on going from Th⁴⁺ to Np⁴⁺ and from Np³⁺ to Np⁴⁺.     

Synthesis of S,N-chelating heterocyclic thionates of palladium(II). Crystal structure of cis-[Pd(pym2S)(PPh3)2] (pym2S = pyrimidine-2-thionate)

The synthesis of mononuclear palladium(II) complexes containing chelating heterocyclic thionates is described. The new compounds of general formula cis-[Pd(RS-N)(L) _x ](ClO₄) [x = 2, L = PPh₃, RS-N = pyridine-2-thionate (py2S) (1), pyrimidine-2-thionate (pym2S) (2), imidazolidine-2-thionate (imzdS) (3), 1-methylimidazoline-2 thionate (mimzS) (4), 1,3-thiazoline-2-thionate (tzdS) (5); x = 1, L = dppe, RS-N = pyridine-2-thionate (py2S) (6), pyrimidine-2-thionate (pym2S) (7), imidazolidine-2-thionate (imzdS) (8), 1-methylimidazole-2 thionate (mimzS) (9) and 1,3-thiazoline-2-thionate (tzdS) (10)] were prepared by directly reacting the hydroxo-complexes [{Pd(PPh₃)₂(-OH) }₂](ClO₄)₂ and [ {Pd(dppe)(-OH) }₂](ClO₄)₂ with the corresponding heterocyclic thiones (RS-N)H. The complexes have been characterized by partial elemental analyses, conductance measurements and spectroscopic methods (I.r., FAB, ¹H- and ³¹P-n.m.r.). No evidence for monomer-dimer equilibrium was found in solution. The crystal structure of (2) has been determined by X-ray diffraction analysis.     

Crystal structure of thallium(I) 2-thiobarbiturate

The crystal and molecular structures of thallium(I) thiobarbiturate C₄H₃N₂O₂STl (C₄H₄N₂O₂S is 2-thiobarbituric acid, Н₂ТВА) have been determined. Crystallographic data for Tl(НТВА) are a = 11.2414(7) Å, b = 3.8444(3) Å, с = 14.8381(9) Å, β = 99.452(2)°, V = 649.00(7) ų, space group P2/с, Z = 4. Each of the two independent thallium ions is bonded to four oxygen and two sulfur atoms to form a distorted tetrahedron. N?H…O and C?H…S hydrogen bonds form a branched three-dimensional network. The structure is also stabilized by π?π interaction between heterocyclic НТВА^- ions. The IR spectra of Tl(НТВА) agree with X-ray powder diffraction data. The compound is also stable below 280°C, and Tl₂SO₄ is one of the thermolysis products in an oxidative medium in the region of 500?650°C.     

Crystal structure of EuH(SeO4)2

Institute of Chemical Reagents. Translated from Zhurnal Strukturnoi Khimii, Vol. 32, No. 3, pp. 30–33, May–June, 1991.     

Crystal structure of RbNbO(SO4)2

Journal of Structural Chemistry -     

Crystal structure of catena-(2-thiobarbiturato) dithallium(I)

By powder X-ray diffraction the crystal structure of catena-(2-thiobarbiturato)dithallium(I) C₄H₂N₂O₂STl₂ (C₄H₄N₂O₂S is 2-thiobarbituric acid, H₂TBA), Tl₂TBA, is determined. Crystallographic data for Tl₂TBA are as follows: a = 15.1039(3) Å, b = 12.0818(2) Å, c = 3.86455(6) Å, β = 97.203(1)°, V = 741.34(2) ų, space group P2₁/n, Z = 4. There are two non-equivalent thallium atoms in the structure. The Tl1 polyhedron is a distorted trigonal prism due to the shortened Tl-S contact (3.634 Å), and the Tl2 polyhedron is a distorted square antiprism.     

Crystal structure of diacetato-bis(2-methyl-2-propylamine)zinc(II)

The diacetato-bis(2-methyl-2-propylamine)zinc(II) compound crystallizes in the triclinic system, space group P-1 with unit cell parameters a = 10.0144(10)Å, b = 10.2687(10)Å, c = 10.5149(10)Å. α = 115.184(2)°, β = 97.489(2)°, γ = 114.066(2)°, ν = 830.85(14)ų. The obtained solid state structure of (^tBuNH₂)₂Zn(OOCCH₃)₂ shows both inter- and intramolecular NH—O hydrogen bond interactions which are analyzed.     

Crystal structure of tris(2-pyridylthio-2-pyridinium)pentaisothiocyanato-dioxouranate(VI)

Summary The crystal structure of [DPSH] ₃ ⁺ [UO₂[NCS)₅]^3– (DPSH = 2 pyridylthio-2-pyridinium) has been determined by standard methods using diffractometer data. Crystals are monoclinic, space groupP2₁/a, witha=33.16 (3),b=16.68(2),c=7.85(1) Å, and=97.3(1); D_c=1.65 g · cm^–3 for Z=4. The structure has been refined to R=5.8% by least squares methods. Five thiocyanate groups are equatorially bonded to the linear uranyl group. The mean of the five U-N, N-C, and C-S bond distances are 2.45, 1.17, and 1.59 Å respectively. The protonated DPS molecules have the N,N-inside conformations.     

Crystal structure of thiogermanic acid H(4)Ge(4)S(10)

X-ray diffraction analysis reveals the thiogermanic acid H(4)Ge(4)S(10) possesses discrete adamantane-like Ge(4)S(10)(4)(-) complex anions. Each thioanion is composed of four corner shared GeS(2.5)(-) tetrahedral units. Crystals were grown from anhydrous liquid hydrogen sulfide reactions with glassy germanium sulfide at room temperature. The crystal structure was solved and refined from single crystal diffractometer data (Mo Kalpha radiation) obtained at 173 K. H(4)Ge(4)S(10) is triclinic, centrosymmetric space group Ponemacr;, with a = 8.621(4) A, b = 9.899(4) A, c = 10.009(4) A, alpha = 85.963(7) degrees, beta = 64.714(7) degrees, gamma = 89.501(8) degrees, and Z = 2. Average bridging and terminal d(Ge-S) distances are 2.229 and 2.206 A, respectively. Vibrational mode assignments are reported from Raman scattering and IR absorption spectra of polycrystalline samples. The nu(s)(Ge-S-Ge) and nu(s)(Ge-S(-)) stretching modes are observed at 354 and 405 cm(-)(1), respectively.